CN111097748A - Multi-element composite cleaning method for polished large-size sapphire window - Google Patents

Multi-element composite cleaning method for polished large-size sapphire window Download PDF

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Publication number
CN111097748A
CN111097748A CN201911387268.4A CN201911387268A CN111097748A CN 111097748 A CN111097748 A CN 111097748A CN 201911387268 A CN201911387268 A CN 201911387268A CN 111097748 A CN111097748 A CN 111097748A
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cleaning
sapphire window
size
solution
size sapphire
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Inventor
梁志强
钟劲
王西彬
杨海成
苏瑛
周天丰
王银惠
焦黎
刘志兵
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Beijing Institute of Technology BIT
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Beijing Institute of Technology BIT
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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
    • B08B3/10—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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/37—Mixtures of compounds all of which are anionic
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble compounds
    • C11D7/06—Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble compounds
    • C11D7/08—Acids

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a multi-element composite cleaning method for a large-size sapphire window after polishing, wherein the large-size sapphire windowCleaning is sequentially carried out through the following steps: treating the surfactant solution in an ultrasonic environment to remove larger particles on the surface; h in megasonic environment2SO4And H2O2Removing organic pollutants from the mixed solution; NH in megasonic environments4OH，H2O2And H2O mixed solution and H3PO4，H2O2And H2Removing micro particles from the mixed solution of O; HCl, H in megasonic Environment2O2And H2And treating in the mixed solution of O to remove pollutants such as metal ions and the like. The multi-element composite cleaning method can effectively remove various pollutants on the surface of the large-size sapphire window, particularly the large-size sapphire window with the size of more than 6 inches, the pollutants are uniformly removed, the large-size sapphire window with extremely high integral cleanliness is obtained, the cleaning process is easy to master, the cleaning effect is stable, and the repeatability and the standardization degree are high.

Description

Multi-element composite cleaning method for polished large-size sapphire window
Technical Field
The invention relates to a multi-element composite cleaning method specially used for a large-size sapphire window, in particular to a multi-element composite cleaning method after polishing of the large-size sapphire window with the size of more than 6 inches.
Technical Field
Sapphire (single crystal alumina, α -Al)2O3) The material is widely applied to industries such as semiconductors, aerospace and the like; the Mohs hardness of the material is 9 times of that of diamond, the material has excellent electrical insulation performance, good optical transmittance and thermal conductivity, and stable physical and chemical properties at high temperature and high pressure, and is commonly used for manufacturing LED substrates, laser lenses, aircraft windows and the like.
With the increasing use demand of sapphire, higher requirements are made on the surface cleaning degree of sapphire. Especially in the field of precision instruments, the surface cleanliness of sapphire elements can significantly affect the service performance and service life of the sapphire elements. At present, the sapphire cleaning is mainly wet cleaning, mainly using solutions such as organic solvents, acids, alkalis, deionized water and the like, and adopting processes such as soaking, rinsing, washing and the like at a proper temperature to achieve the purpose of removing pollutants such as organic matters, metal ions, particles and the like attached to the surface of the sapphire.
In addition, the ultrasonic cleaning technology is also applied to the sapphire cleaning and purifying process, the bubble breaking effect generated in the cavitation process is utilized to reduce the adsorption force of the pollutants and the cleaning surface, so that the pollutants are easier to remove, and the ultrasonic vibration can impact the cleaned surface through the strong vibration of medium particles, so that the pollutants are separated from the cleaning surface.
With the improvement of the polishing process, the polishing solution containing a large amount of nano-particles is used in sapphire chemical mechanical polishing, although the polishing solution containing small-sized nano-particles can effectively improve the surface quality of sapphire, the polishing particles are very easy to attach to the surface of sapphire, so that the difficulty of cleaning a sapphire window is greatly increased, particularly, the cleaning difficulty of a large-size sapphire window with the cleanliness requirement higher than 6 inches is multiplied, the cleanliness of the sapphire window can be improved only in a limited range by using independent cleaning methods of solutions such as ultrasound, organic solvents, acid, alkali, deionized water and the like, the cleanliness requirement in an actual application environment is difficult to meet, and the multi-element composite cleaning of the large-size sapphire window by using various cleaning technologies is rarely researched in the prior art, so how to provide a special cleaning solution for the large-size sapphire window, Particularly, the method has very important practical significance for the high repeatability and standardized cleaning method after the polishing of the large-size sapphire window with the size of more than 6 inches.
Disclosure of Invention
Aiming at the problems that particles, organic matters, metal ions and other pollutants which are difficult to remove are attached to the surface of a large-size sapphire window, particularly a large-size sapphire window with the surface cleanliness being higher than 6 inches, and the pollutants are difficult to remove uniformly by a single cleaning means due to the large size of the sapphire window, strong adsorption force of micro pollutants and the like, the invention adopts a multi-step chemical cleaning method combining ultrasound and megasonic to perform multi-element composite cleaning on the large-size sapphire window, particularly aiming at the sapphire window with the surface cleanliness being higher than 6 inches, and can effectively remove various pollutants on the surface of the large-size sapphire window, thereby obtaining the large-size sapphire window with extremely high surface cleanliness.
The invention relates to a multi-element composite cleaning method for a polished large-size sapphire window, which is realized by the following steps:
(1) ultrasonically cleaning the polished large-size sapphire window in a compounded surfactant cleaning solution at the temperature of 60-80 ℃ for 10-50 min, and then ultrasonically cleaning in deionized water for 5-10 min;
(2) megasonically cleaning the large-size sapphire window cleaned in the step (1) in a cleaning solution A at the temperature of 60-80 ℃ for 10-30 min, and megasonically cleaning in deionized water for 5-10 min, wherein the cleaning solution A is H2SO4And H2O2The mixed solution of (A) and (B) in a ratio of H2SO4:H2O2＝3:1；
(3) Megasonically cleaning the large-size sapphire window cleaned in the step (2) in a cleaning solution B at the temperature of 60-80 ℃ for 10-30 min, and megasonically cleaning in deionized water for 5-10 min, wherein the cleaning solution B is NH4OH，H2O2And H2Mixed solution of O in NH ratio4OH:H2O2:H2O＝1:1:5；
(4) Megasonically cleaning the large-size sapphire window cleaned in the step (3) in a cleaning solution C at the temperature of 60-80 ℃ for 10-30 min, and megasonically cleaning in deionized water for 5-10 min, wherein the cleaning solution C is H3PO4，H2O2And H2Mixed solution of O in the proportion of H3PO4:H2O2:H2O＝1:2:10；
(5) Cleaning the large-size sapphire window cleaned in the step (4) at the temperature of 60-80 DEG CMegasonically cleaning in liquid D for 10-30 min, and megasonically cleaning in deionized water for 5-10 min, wherein the cleaning liquid D is HCl and H2O2And H2Mixed solution of O in the ratio of HCl to H2O2:H2And (5) drying the surface, and performing vacuum packaging.
The surfactant cleaning solution in the step (1) is a cleaning solution compounded by two anionic surfactants of dodecylbenzene sulfonic acid and sodium dodecylbenzene sulfonate in an alkaline environment, and the pH value of the solution can be adjusted by the alkaline solution, so that the solution reaches a specific environment.
The ultrasonic cleaning frequency used in the step (1) is 40-100 kHz, the ultrasonic power is 300W, and the ultrasonic cleaning frequency is matched with a surfactant cleaning solution to remove large particle pollutants on the surface of a large-size sapphire window.
The megasonic cleaning frequency used in the steps (2) to (4) of the invention is 1MHz, the megasonic power is 600W, and the megasonic cleaning device is used for removing micro particles with the size of less than 1 μm on the surface of a large-size sapphire window.
H in step (4) of the present invention3PO4，H2O2And H2The mixed solution of O can strip the sapphire at the edge of the pollutant from a large-size sapphire window by the corrosion effect on the surface of the sapphire, and the purpose of removing the sapphire is achieved by matching with megasonic cleaning environment.
In the step (5), a nitrogen gun is used for drying the surface of a large-size sapphire window, and the content of ultrapure nitrogen is 99.9999%; the containers for vacuum packaging also need to be cleaned and are vacuum packaged in two layers using a dust free bag or an aluminum foil bag.
The multi-step chemical cleaning method for the polished large-size sapphire window is a multi-step chemical cleaning method combining ultrasonic treatment and megasonic treatment, can effectively remove various pollutants on the surface of the large-size sapphire window, particularly the large-size sapphire window with the surface cleanliness higher than 6 inches, and obtains the large-size sapphire window with extremely high surface cleanliness, wherein the number of particles on the surface of the large-size sapphire window after being cleaned is less than or equal to 100 by taking the 6-inch large-size sapphire window as an example, and the cleaning process is easy to master, simple to operate, stable in cleaning effect, high in repeatability and standardization degree.
In addition, the invention also has the following advantages:
the cleaning solution compounded by two anionic surfactants, namely dodecyl benzene sulfonic acid and sodium dodecyl benzene sulfonate, is adopted in an alkaline environment, and compared with a common cleaning solution with an active agent, the cleaning solution has stronger removal capability on surface particles of a large-size sapphire window.
The cleaning method combining ultrasound and megasonic is adopted, the cavitation of the ultrasound is matched with the surfactant solution, the particle pollutants on the surface of the sapphire are effectively removed, the impact effect of the cleaning liquid in the megasonic environment on the surface of a large-size sapphire window is utilized, and the micro-corrosion effect of phosphoric acid in the cleaning liquid C on the sapphire is matched, so that the small particle pollutants on the surface of the sapphire are effectively removed.
The method has the advantages of high efficiency and avoidance of introduction of other pollutants compared with methods such as drying and air drying by blowing the ultra-pure nitrogen to dry the large-size sapphire window, and effectively ensures high cleanliness of the sapphire after cleaning before use by adopting two-layer vacuum packaging of a dust-free bag or an aluminum foil bag.
Drawings
FIG. 1 is a surface cleanliness detection image of a large-size sapphire window before and after cleaning, and a surface defect detector is used for detection; FIG. 2 is an AFM topography of a sapphire surface during cleaning; FIG. 3 is a schematic diagram of a specific cleaning step.
Detailed Description
The following describes a specific embodiment of the present invention through a multi-component cleaning test after polishing a large-size sapphire window:
(1) ultrasonically cleaning the polished large-size sapphire window in a compound surfactant cleaning solution at 60 ℃ for 20min, and then ultrasonically cleaning in deionized water for 5 min;
(2) megasonically cleaning the large-size sapphire window cleaned in the step (1) in a cleaning solution A at 60 ℃ for 20min, and megasonically cleaning in deionized water for 5min, wherein the cleaning solution A is H2SO4And H2O2The mixed solution of (A) and (B) in a ratio of H2SO4:H2O2＝3:1；
(3) Megasonically cleaning the large-size sapphire window cleaned in the step (2) in a cleaning solution B at 60 ℃ for 20min, and megasonically cleaning in deionized water for 5min, wherein the cleaning solution B is NH4OH，H2O2And H2Mixed solution of O in NH ratio4OH:H2O2:H2O＝1:1:5；
(4) Megasonically cleaning the large-size sapphire window cleaned in the step (3) in a cleaning solution C at 60 ℃ for 20min, and megasonically cleaning in deionized water for 5min, wherein the cleaning solution C is H3PO4，H2O2And H2Mixed solution of O in the proportion of H3PO4:H2O2:H2O＝1:2:10；
(5) Megasonically cleaning the large-size sapphire window cleaned in the step (4) in a cleaning solution D at 60 ℃ for 20min, and megasonically cleaning in deionized water for 5min, wherein the cleaning solution D is HCl and H2O2And H2Mixed solution of O in the ratio of HCl to H2O2:H2And (5) drying the surface and packaging.
The large-size sapphire window used in the test was a large-size sapphire window to be cleaned after polishing, and the size was 6 inches.
The surfactant cleaning solution used in the test step (1) is prepared from dodecylbenzene sulfonic acid and sodium dodecylbenzene sulfonate in deionized water (wherein the mass fractions of the dodecylbenzene sulfonic acid and the sodium dodecylbenzene sulfonate are both 1%), fully stirred, and then 10% is used-3Adjusting the pH value of the cleaning solution by using a KOH solution of mol/L to ensure that the pH value of the cleaning solution is 10. The chemicals used in this test were all commercially available.
The ultrasonic cleaning frequency used in the test is 40kHz, the ultrasonic power is 300W, the megasonic cleaning frequency is 1MHz, the megasonic power is 600W, the immersion cleaning method is adopted, and the temperature is set to be 60 ℃ during cleaning.
In the step (5) of the test, a nitrogen gun is used for drying the surface of a large-size sapphire window, and the content of ultrapure nitrogen is 99.9999%; the container for vacuum packaging needs to be cleaned and vacuum packaged by two layers of a dust-free bag or an aluminum foil bag.
The measurement results of the surface particles before and after cleaning of the large-size sapphire window are shown in fig. 1, the number of the surface particles before cleaning is large, 18534 particles exist, the number of the surface particles after cleaning is 87, and the surface particle number is obviously reduced compared with the surface particle number before and after cleaning. In addition, because the pollutant components adsorbed on the surface of the polished sapphire are complex, other detection methods are needed to represent the cleaning effect of the sapphire, and an AFM (atomic force microscope) topography of the surface of the sapphire in the cleaning process is shown in FIG. 2.
FIG. 2(a) is a topographic map after the cleaning in step (1), wherein larger particles on the surface are removed, but some tiny particles remain, the surface is still covered with a layer of organic contaminants, and the original surface of sapphire cannot be observed; FIG. 2(b) is a topographic map after the cleaning in step (2), the organic contaminants are removed, and the structure of the surface can be observed, but some micro particles remain; FIG. 2(c) is a graph of the post-cleaning topography of step (4) with substantial removal of particles by the cleaning fluid and megasonic treatment; and (d) in FIG. 2 is a topography after cleaning in step (5), and after complete cleaning, the surface structure is observed to be clearer, and various pollutants are basically and completely removed.
The tests show that the surface of the large-size sapphire window treated by the multi-element composite cleaning method after the polishing of the large-size sapphire window is extremely high in cleanliness, and the method is particularly suitable for the large-size sapphire window with the size of more than 6 inches, and the cleaning process is easy to operate, simple in cleaning equipment, stable in cleaning effect and high in repeatability and standardization.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention. The parts not involved in the present invention are the same as or can be implemented using the prior art.

Claims (5)

1. A multi-element composite cleaning method for a large-size sapphire window after polishing is characterized by being realized through the following processes:
(1) ultrasonically cleaning the polished large-size sapphire window in a compounded surfactant cleaning solution at the temperature of 60-80 ℃ for 10-50 min, and then ultrasonically cleaning in deionized water for 5-10 min;
(2) megasonically cleaning the large-size sapphire window cleaned in the step (1) in a cleaning solution A at the temperature of 60-80 ℃ for 10-30 min, and megasonically cleaning in deionized water for 5-10 min, wherein the cleaning solution A is H2SO4And H2O2The mixed solution of (A) and (B) in a ratio of H2SO4:H2O2＝3:1；
(3) Megasonically cleaning the large-size sapphire window cleaned in the step (2) in a cleaning solution B at the temperature of 60-80 ℃ for 10-30 min, and megasonically cleaning in deionized water for 5-10 min, wherein the cleaning solution B is NH4OH，H2O2And H2Mixed solution of O in NH ratio4OH:H2O2:H2O＝1:1:5；
(4) Megasonically cleaning the large-size sapphire window cleaned in the step (3) in a cleaning solution C at the temperature of 60-80 ℃ for 10-30 min, and megasonically cleaning in deionized water for 5-10 min, wherein the cleaning solution C is H3PO4，H2O2And H2Mixed solution of O in the proportion of H3PO4:H2O2:H2O＝1:2:10；
(5) Megasonically cleaning the large-size sapphire window cleaned in the step (4) in a cleaning solution D at the temperature of 60-80 ℃ for 10-30 min, and megasonically cleaning in deionized water for 5-10 min, wherein the cleaning solution D is HCl and H2O2And H2Mixed solution of O in the ratio of HCl to H2O2:H2And (5) drying the surface, and performing vacuum packaging.
2. The method of claim 1, wherein the large sapphire window has a size of 6 inches or more.
3. The method according to claim 1 or 2, wherein the particle size of the polishing liquid during the polishing process is 100 nm.
4. The method according to any one of claims 1 to 3, wherein the surfactant solution used in step (1) is a cleaning solution prepared by compounding two anionic surfactants, namely dodecylbenzene sulfonic acid and sodium dodecylbenzene sulfonate, in an alkaline environment.
5. The method according to any one of claims 1 to 4, wherein the ultrasonic cleaning is performed in step (1) at an ultrasonic frequency of 40kHz to 100kHz and at an ultrasonic power of 300W, and the megasonic cleaning is performed in the subsequent step at a megasonic frequency of 1MHz and at a megasonic power of 600W.
CN201911387268.4A 2019-12-27 2019-12-27 Multi-element composite cleaning method for polished large-size sapphire window Pending CN111097748A (en)

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CN104842225A (en) * 2015-04-22 2015-08-19 苏州爱彼光电材料有限公司 Wet processing method for large-dimension sapphire substrate surface
US20160370116A1 (en) * 2015-06-19 2016-12-22 Apple Inc. Process for heat treating a sapphire component
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