CN114653679A - Method for cleaning organic pollutants on surface of silicon carbide wafer - Google Patents
Method for cleaning organic pollutants on surface of silicon carbide wafer Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 63
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- 239000002957 persistent organic pollutant Substances 0.000 title claims abstract description 20
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- HHHBEVPEYINXHC-UHFFFAOYSA-N 3-butyl-1-methyl-1,2-dihydroimidazol-1-ium;dibutyl phosphate Chemical compound CCCCN1C[NH+](C)C=C1.CCCCOP([O-])(=O)OCCCC HHHBEVPEYINXHC-UHFFFAOYSA-N 0.000 claims description 4
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Images
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
- B08B13/00—Accessories or details of general applicability for machines or apparatus for cleaning
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
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- 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 cleaning organic pollutants on the surface of a silicon carbide wafer, which comprises the steps of putting the silicon carbide wafer into an ultrasonic cleaning tank filled with an activating solution for ultrasonic cleaning, then carrying out electrolytic treatment in an electrolytic bath, and adding ozone into a positive bath of the electrolytic bath; and taking out the silicon carbide wafer after the electrolysis is finished, cleaning by using pure water, drying and storing. The surface of the silicon carbide wafer is subjected to activation treatment, and then the strong oxidizing liquid generated by electrolysis is utilized to be matched with the action of an electric field, so that the surface of the silicon carbide wafer can be effectively cleaned, organic pollutants on the surface can be effectively removed, and particle pollutants on the surface can be thoroughly removed; the invention can not damage the surface of the wafer, thereby obtaining the most excellent cleaning effect.
Description
Technical Field
The invention relates to a method for cleaning organic pollutants on the surface of a silicon carbide wafer, belonging to the technical field of wafer cleaning.
Background
The third generation semiconductor material is mainly a wide bandgap semiconductor material represented by silicon carbide (SiC), gallium nitride (GaN), zinc oxide (ZnO), diamond, and aluminum nitride (AlN). The method has advantages in application scenes such as communication, automobiles, high-speed rails, satellite communication, aerospace and the like. Among them, the research and development of silicon carbide and gallium nitride are more mature.
At present, the common cleaning technology of the silicon carbide wafer is usually cleaned by a chemical method. Chemical cleaning is a process of utilizing various chemical reagents and organic solvents to perform chemical reaction or dissolution with impurities and oil stains adsorbed on the surface of a cleaned wafer, so that the impurities are desorbed from the surface of the cleaned wafer, and then washing the wafer with a large amount of high-purity hot and cold deionized water, thereby obtaining a clean surface. The chemical cleaning can be divided into wet chemical cleaning and dry chemical cleaning, wherein the wet chemical cleaning is still dominant in the semiconductor cleaning process.
In wet chemical cleaning, the following methods are classified:
1) solution soaking method
The solution immersion method is a method of immersing a wafer in a chemical solution to remove surface contamination. It is one of the most common methods used in wet chemical cleaning. Different solutions are selected to remove different types of pollution impurities on the surface of the wafer, such as organic solvents for removing organic pollutants and RCA solutions for removing organic, inorganic and metal ions and other impurities. Usually, this method cannot completely remove impurities on the wafer surface, so the soaking is usually assisted by physical measures such as heating, ultrasound, stirring, etc.
2) Mechanical scrubbing method
Mechanical scrubbing is commonly used to remove particles or organic residues from the wafer surface and can be generally divided into manual scrubbing and wafer scrubbing. The manual scrubbing is the simplest scrubbing method, a cotton ball soaked with organic solvents such as absolute ethyl alcohol is clamped by stainless steel tweezers, and the surface of a wafer is lightly scrubbed along the same direction to remove wax films, dust, residual gum or other solid particles. The wafer wiping machine adopts mechanical rotation, and the surface of the wafer is wiped by using a soft sheep brush or a brush roll, so that the scratch of the wafer is greatly reduced. The high-pressure wafer wiping machine has no mechanical friction, so that the wafer cannot be scratched, and the contamination in the groove mark can be removed.
3) Ultrasonic cleaning
Ultrasonic cleaning is a cleaning method widely applied in the semiconductor industry, and has the advantages that: the cleaning effect is good, the operation is simple, and complex devices and containers can be cleaned. The cleaning method is characterized in that under the action of strong ultrasonic waves, a sparse part and a dense part are generated in a liquid medium, the sparse part generates cavity bubbles which are nearly vacuum, and when the cavity bubbles disappear, strong local pressure is generated nearby, so that chemical bonds in molecules are broken, and impurities on the surface of a wafer are desorbed. The effect of ultrasonic cleaning is related to ultrasonic conditions (such as temperature, pressure, ultrasonic frequency, power, etc.), and is mostly used for removing bulk contamination and particles attached to the wafer surface.
4) Megasonic cleaning
Megasonic cleaning not only has the advantages of ultrasonic cleaning, but also overcomes the disadvantages thereof. Megasonic cleaning is the cleaning of wafers by the high energy (850kHz) frequency vibration effect combined with the chemical reaction of chemical cleaning agents. During cleaning, solution molecules are driven by megasonic waves to do accelerated motion (the maximum instantaneous speed can reach 30 cm/s), and the solution molecules continuously impact the surface of the wafer by high-speed fluid waves, so that pollutants and fine particles attached to the surface of the wafer are forcibly removed and enter the cleaning solution. The method can simultaneously play the roles of a mechanical wiping piece and a chemical cleaning method. Currently, megasonic cleaning has become an effective method for cleaning polishing pads.
5) Rotary spraying method
The spin spray method is a method of removing impurities on the surface of a wafer by rotating the wafer at a high speed by a mechanical method and continuously spraying a liquid (high purity deionized water or other cleaning liquid) onto the surface of the wafer during the rotation. The method utilizes the dissolution of sprayed liquid or chemical reaction to dissolve the contamination on the surface of the wafer, and simultaneously utilizes the centrifugal effect of high-speed rotation to ensure that the liquid dissolved with impurities is separated from the surface of the wafer in time. The rotary spraying method has the advantages of chemical cleaning, hydromechanical cleaning and high-pressure scrubbing, and can be combined with a spin-drying process, wherein deionized water is used for spraying and cleaning for a period of time, water is stopped, inert gas is sprayed, and the surface of a wafer can be quickly dehydrated by increasing the rotation speed and centrifugal force.
Among the dry cleaning techniques that are commonly used today are:
1) plasma cleaning technique
The plasma cleaning has the advantages of simple process, convenient operation, no waste treatment, no environmental pollution and the like. It does not remove carbon and other non-volatile metal or metal oxide impurities. Plasma cleaning is commonly used in the photoresist removal process, a small amount of oxygen is introduced into a plasma reaction system, and under the action of a strong electric field, the oxygen generates plasma, so that the photoresist is rapidly oxidized into volatile gaseous substances to be pumped away. The cleaning technology has the advantages of convenient operation, high efficiency, clean surface, no scratch, contribution to ensuring the quality of products and the like in the photoresist removing process, and does not use acid, alkali, organic solvent and the like, thereby being more and more valued by people.
2) Vapor phase cleaning technique
Vapor phase cleaning is a cleaning method which utilizes the interaction of vapor phase equivalent of corresponding substances in a liquid process and contaminant substances on the surface of a wafer to achieve the aim of removing impurities. Wafer cleaning in CMOS processes such as in MMST engineering studies employs vapor phase HF and water vapor interaction to remove oxide. Typically, an aqueous HF process must be supplemented with a particle removal process, and a subsequent particle removal process is not required with vapor phase HF cleaning techniques. The most important advantages of aqueous HF processes are much less chemical consumption of HF and higher cleaning efficiency.
3) Beam cleaning technology
The beam cleaning technology is a cleaning technology which utilizes the interaction between high-energy beam-shaped material flow and the contamination impurities on the surface of a wafer to remove the impurities on the surface of the wafer. Common beam cleaning techniques include micro focused beam cleaning techniques, laser beam techniques, condensation spray techniques, and the like. The micro-focusing beam cleaning technology is a novel on-line wafer surface cleaning technology with the greatest development prospect at present, and the cleaning liquid sprayed from a capillary is applied to the surface of a wafer by adopting an electro-hydrodynamic spraying principle to remove particles and organic thin film stains on the surface of the wafer. The advantages are that: the consumption of the cleaning solution is low, only dozens of microliters of cleaning solution is needed for cleaning one silicon wafer, and the occurrence of secondary pollution is reduced.
Various existing wet chemical cleaning technologies have some defects, and the cleaning effect and the cleaning efficiency are low. Therefore, it is necessary to develop a new cleaning method.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for cleaning organic pollutants on the surface of a silicon carbide wafer, which has the following specific technical scheme:
a method for cleaning organic pollutants on the surface of a silicon carbide wafer comprises the following steps:
step one, surface treatment
Putting the silicon carbide wafer into an ultrasonic cleaning tank, pouring an activating solution into the ultrasonic cleaning tank, and soaking for 10-15 min; then carrying out ultrasonic cleaning in an ultrasonic cleaning tank, wherein the temperature in the tank is kept at 65-68 ℃, the ultrasonic frequency is 66-72 kHz, and the ultrasonic cleaning time is 15-20 min; after ultrasonic cleaning, sending the mixture into a constant-temperature oven for drying;
step two, deep cleaning
An ion exchange membrane is arranged in the middle of the electrolytic cell, the electrolytic cell is divided into a cathode cell and an anode cell by a semi-homogeneous ion exchange membrane, the cathode of the electrolytic cell is positioned in the cathode cell, and the anode of the electrolytic cell is positioned in the anode cell; pouring electrolyte between the cathode and the anode of the electrolytic cell, controlling the pH of the solution in the cathode to be more than 13 by using strong alkali solution, adding ozone into the anode cell, and electrolyzing for 3-5 min; and (3) putting the silicon carbide wafer subjected to surface treatment into an electrolytic bath, continuing to electrolyze for 3-5 min, taking out the silicon carbide wafer, cleaning with pure water, drying and storing.
According to the further optimization of the technical scheme, the activating solution is 1.3-1.7 mass percent of 1-butyl-3-methylimidazol dibutyl phosphate solution.
According to the further optimization of the technical scheme, the activating solution is 1.6 mass percent of 1-butyl-3-methylimidazolium dibutyl phosphate solution.
According to the further optimization of the technical scheme, the cathode of the electrolytic cell adopts low-carbon steel as an electrode, and the anode of the electrolytic cell adopts a catalytic coating titanium electrode; the catalytic coating titanium electrode is characterized in that a coating is formed on the surface of a titanium plate by using a powdery cerium dioxide-metal organic framework composite material in an ultrasonic rapid cold spraying mode, the temperature of the ultrasonic rapid cold spraying is 75-80 ℃, and the thickness of the coating is 1-2 mm.
According to the further optimization of the technical scheme, the electrolyte is one or more of a sodium sulfate solution, a potassium sulfate solution, a sodium phosphate solution and a potassium phosphate solution.
According to the further optimization of the technical scheme, the strong base in the strong base solution is one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide, rubidium hydroxide and strontium hydroxide.
According to the further optimization of the technical scheme, the ozone added into the anode tank is added in the mode of ozone ice blocks, and the concentration of the ozone in the ozone ice blocks is 12 ppm-13 ppm.
The invention has the beneficial effects that:
the surface of the silicon carbide wafer is firstly subjected to activation treatment, and then the strong oxidizing liquid generated by electrolysis is utilized to be matched with the action of an electric field, so that the surface of the silicon carbide wafer can be effectively cleaned, organic pollutants on the surface can be effectively removed, and particle pollutants on the surface can be thoroughly removed; the invention can not damage the surface of the wafer, thereby obtaining the most excellent cleaning effect.
Drawings
FIG. 1 is a graph of the trend between concentration of the activation solution and removal of particulate contaminants having a particle size of 200nm or greater.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Step 1, putting a silicon carbide wafer (preferably the silicon carbide wafer cleaned of metal pollutants) into an ultrasonic cleaning tank, pouring an activating solution into the ultrasonic cleaning tank, wherein the activating solution is 1.6% by mass of 1-butyl-3-methylimidazolium dibutyl phosphate solution, and the 1-butyl-3-methylimidazolium dibutyl phosphate solution is prepared by dissolving 1-butyl-3-methylimidazolium dibutyl phosphate in water and is an ionic liquid, which is abbreviated as [ BMIM ]](C4H9O)2PO2(ii) a Soaking for 10 min; then ultrasonic cleaning is carried out in an ultrasonic cleaning tank, the temperature in the tank is kept at 68 ℃, the ultrasonic frequency is 66kHz, and the ultrasonic cleaning time is 15 min; after ultrasonic cleaning, the mixture is sent into a constant-temperature oven for drying.
The cathode of the electrolytic cell adopts low-carbon steel as an electrode, and the anode of the electrolytic cell adopts a catalytic coating titanium electrode; the catalytic coating titanium electrode is characterized in that a coating is formed on the surface of a titanium plate by using a powdery cerium dioxide-metal organic framework composite material in an ultrasonic rapid cold spraying mode, the temperature of the ultrasonic rapid cold spraying is 75-80 ℃, and the thickness of the coating is 2 mm. The ozone added in the anode tank is added in the form of ozone ice blocks, and the ozone concentration in the ozone ice blocks is 13 ppm. The ceria-metal organic framework composite material refers to a metal organic framework loaded with ceria, and the preparation method thereof belongs to the prior art, and is not described herein again, and can also be obtained by a purchase method, such as a CeO2-DR material from dekkebel environmental systems ltd, guan.
Example 2
Step 1, placing a silicon carbide wafer into an ultrasonic cleaning tank, pouring an activating solution into the ultrasonic cleaning tank, wherein the activating solution is 1.6% of dibutyl 1-butyl-3-methylimidazolium phosphate solution in mass fraction, and soaking for 10-15 min; then ultrasonic cleaning is carried out in an ultrasonic cleaning tank, the temperature in the tank is kept at 65 ℃, the ultrasonic frequency is 72kHz, and the ultrasonic cleaning time is 20 min; after ultrasonic cleaning, the mixture is sent into a constant-temperature oven for drying.
The cathode of the electrolytic cell adopts low-carbon steel as an electrode, and the anode of the electrolytic cell adopts a catalytic coating titanium electrode; the catalytic coating titanium electrode is characterized in that a coating is formed on the surface of a titanium plate by using a powdery cerium dioxide-metal organic framework composite material in an ultrasonic rapid cold spraying mode, the temperature of the ultrasonic rapid cold spraying is 75-80 ℃, and the thickness of the coating is 1 mm. The ozone added in the anode tank is added in the form of ozone ice blocks, and the concentration of the ozone in the ozone ice blocks is 12 ppm.
Example 3
Test for particle contamination
When each wafer is detected, a metallographic microscope is used for observation, and the metallographic microscope can be G-100 type equipment of Ann electronic technology Limited, Shenzhen city; randomly selecting 20 points as test points, observing the number of the particle pollutants on the surface of the wafer in the visual field, and counting and sorting the obtained data to respectively obtain the average value of the total number of the particle pollutants on the surface; according to the particle size statistics, the removal rate =1- (number of particle pollutants after removal/number of particle pollutants before removal) is respectively counted and calculated according to the scales of 40nm, 100nm and 200 nm.
By adopting the cleaning method in the embodiment 1, the removal rate of the particulate pollutants with the particle size of more than or equal to 40nm and less than 100nm can reach more than 99.67%, the removal rate of the particulate pollutants with the particle size of more than or equal to 100nm and less than 200nm can reach more than 99.83%, and the removal rate of the particulate pollutants with the particle size of more than or equal to 200nm can reach more than 99.98%.
Example 4
Effect of activation liquid concentration on particulate contamination cleaning test
Only the concentration of the activating solution in example 1 was changed, i.e., [ BMIM ]](C4H9O)2PO2The mass fraction of (A) is 1.0-2.2 respectively, and the rest conditions are unchanged. And finally, calculating the removal rate of the particle pollutants with the particle size of more than or equal to 200nm according to a particle pollutant detection test, wherein the test data are shown in a table 1:
TABLE 1
| Concentration of | Removal Rate (%) |
| 1.0 | 85.18 |
| 1.1 | 93.55 |
| 1.2 | 97.63 |
| 1.3 | 99.22 |
| 1.4 | 99.35 |
| 1.5 | 99.67 |
| 1.6 | 99.98 |
| 1.7 | 99.55 |
| 1.8 | 98.26 |
| 1.9 | 97.25 |
| 2.0 | 97.23 |
| 2.1 | 97.27 |
| 2.2 | 97.21 |
According to the data in Table 1, a trend graph was prepared between the concentration of the activation solution and the removal rate of particulate contaminants having a particle size of 200nm or more, as shown in FIG. 1. The analysis shows that: concentration of activating solution, [ BMIM ]](C4H9O)2PO2When the mass fraction of the active liquid is 1.3-1.7%, the removal rate of the particle pollutants with the particle size of more than or equal to 200nm exceeds 99%, and when the concentration of the active liquid is 1.6%, the removal rate reaches the maximum; therefore, the concentration of the activating solution is preferably 1.6%.
Example 5
Effect of Ionic liquid species on particle contaminant cleaning tests
Only the ionic liquid species in example 1 was modified, as is [ BMIM ] in example 1](C4H9O)2PO2Are respectively replaced by [ BMIM]BF4(1-butyl-3-methylimidazolium tetrafluoroborate), [ BMIM]OTF (1-butyl-3-methylimidazole trifluoromethanesulfonate), the concentration of the activating solution is 1.6%, and the rest conditions are unchanged. Finally, according to a particle pollutant detection test, the removal rate of the particle pollutants with the particle size of more than or equal to 200nm is calculated, and the test data is shown in a table 2:
TABLE 2
| Species of ionic liquids | [BMIM](C4H9O)2PO2 | [BMIM]BF4 | [BMIM]OTF |
| Removal rate | 99.98% | 59.12% | 63.57% |
Example 6
Putting the silicon carbide wafer cleaned of the metal pollutants into an ultrasonic cleaning tank, pouring deionized water into the ultrasonic cleaning tank, and soaking for 10 min; then ultrasonic cleaning is carried out in an ultrasonic cleaning tank, the temperature in the tank is kept at 68 ℃, the ultrasonic frequency is 66kHz, and the ultrasonic cleaning time is 15 min; after ultrasonic cleaning, the mixture is sent into a constant-temperature oven for drying.
And finally, according to a particle pollutant detection test, calculating that the removal rate of the particle pollutants with the particle size of more than or equal to 200nm is less than or equal to 22.38%.
Example 7
Step 1, putting the silicon carbide wafer cleaned of the metal pollutants into an ultrasonic cleaning tank, pouring deionized water into the ultrasonic cleaning tank, and soaking for 10 min; then ultrasonic cleaning is carried out in an ultrasonic cleaning tank, the temperature in the tank is kept at 68 ℃, the ultrasonic frequency is 66kHz, and the ultrasonic cleaning time is 15 min; after ultrasonic cleaning, the mixture is sent into a constant-temperature oven for drying.
The cathode of the electrolytic cell adopts low-carbon steel as an electrode, and the anode of the electrolytic cell adopts a catalytic coating titanium electrode; the catalytic coating titanium electrode is characterized in that a coating is formed on the surface of a titanium plate by using a powdery cerium dioxide-metal organic framework composite material in an ultrasonic rapid cold spraying mode, the temperature of the ultrasonic rapid cold spraying is 75-80 ℃, and the thickness of the coating is 2 mm. The ozone added in the anode tank is added in the form of ozone ice blocks, and the ozone concentration in the ozone ice blocks is 13 ppm.
And finally, according to a particle pollutant detection test, calculating that the removal rate of the particle pollutants with the particle size of more than or equal to 200nm is 78.17%.
Example 8
Putting the silicon carbide wafer cleaned of the metal pollutants into an ultrasonic cleaning tank, pouring an activating solution into the ultrasonic cleaning tank, wherein the activating solution is 1.6% of 1-butyl-3-methylimidazol dibutyl phosphate solution by mass percent, and soaking for 10 min; then ultrasonic cleaning is carried out in an ultrasonic cleaning tank, the temperature in the tank is kept at 68 ℃, the ultrasonic frequency is 66kHz, and the ultrasonic cleaning time is 15 min; after ultrasonic cleaning, the mixture is sent into a constant-temperature oven for drying.
And finally, according to a particle pollutant detection test, calculating the removal rate of the particle pollutants with the particle size of more than or equal to 200nm to be-57.43 to-35.28 percent. Instead, the particle contamination is increased due to the introduction of new ions, and the particle contamination cannot be removed only by the ultrasonic cleaning means, and thus, the removal rate of the particle contamination becomes negative.
Example 9
The cathode of the electrolytic cell adopts low-carbon steel as an electrode, and the anode of the electrolytic cell adopts a catalytic coating titanium electrode; the catalytic coating titanium electrode is characterized in that a coating is formed on the surface of a titanium plate by using a powdery cerium dioxide-metal organic framework composite material in an ultrasonic rapid cold spraying mode, the temperature of the ultrasonic rapid cold spraying is 75-80 ℃, and the thickness of the coating is 2 mm. The ozone added in the anode tank is added in the form of ozone ice blocks, and the ozone concentration in the ozone ice blocks is 13 ppm.
And finally, according to a particle pollutant detection test, calculating that the removal rate of the particle pollutants with the particle size of more than or equal to 200nm is 76.75%.
Example 10
Effect of Anode materials of electrolytic cells on particle contamination cleaning tests
Only the anode material of the electrolytic cell in the example 1 is changed, that is, the ceria-metal organic framework composite material is replaced by a titania-metal organic framework composite material, a titania film electrode, an iridium coating titanium electrode or a diamond boron-doped electrode, and the rest conditions are not changed.
Finally, according to the XPS technology test for organic pollutant content on the surface of the wafer, the removal rate of the organic pollutants is calculated, and the test data are shown in Table 3:
TABLE 3
| Anode material of electrolytic cell | Removal rate of organic pollutants |
| Ceria-metal organic framework composite material | 57.8% |
| Titanium dioxide-metal organic framework composite material | 33.5% |
| Titanium dioxide film electrode | 23.9% |
| Iridium-based coating titanium electrode | 21.3% |
| Diamond boron-doped electrode | 28.1% |
The titanium dioxide-metal organic framework composite material refers to a metal organic framework loaded with titanium dioxide, and the preparation method thereof belongs to the prior art, and is not described herein again, and can also be obtained by a purchase method, such as a TiO2-DR type composite material of Dekkel environmental systems, Inc. of Dongguan. The manufacturing method of the titanium dioxide thin film electrode belongs to the prior art, and is not repeated herein, and can also be obtained by a purchasing method, such as a DBm type electrode of Shanghai Europe nanometer technology Limited company. The manufacturing method of the iridium-based coating titanium electrode belongs to the prior art, and is not repeated herein, and can also be obtained by a purchasing method, such as the YC type electrode manufactured by titanium electrode manufactured by Youji city, Inc. The manufacturing method of the diamond boron-doped electrode belongs to the prior art, and is not repeated herein, and can also be obtained by a purchasing method, such as the DAEO-B type electrode of Hunan Xinfeng technology Limited.
XPS technique test of organic contaminant content on wafer surface
The X-ray photoelectron spectroscopy (XPS) technology is a nondestructive measurement technology for detecting surface information of a material through a photon beam with a depth of 3-10 nm incident on the surface of a sample. Quantitatively analyzing the constituent elements of a detected sample, and checking the content of atoms in the elements by the spectral line intensity (area occupied by a characteristic peak) in a spectrum; in XPS, the current application of quantitative analysis is mostly based on the ratio of the intensities of the peaks in the spectrum, converting the observed signal intensity into the content of the element, i.e. converting the peak area of the spectrum into the content of the corresponding element.
In the invention, the content of organic pollutants on the surface of the wafer is characterized by the oxygen atom content, and the relative atomic percent of oxygen is calculated by combining the characteristic absorption peak of oxygen element.
The removal rate of organic contaminants was 1- (relative atomic percent of oxygen after removal of organic contaminants/relative atomic percent of oxygen before removal of organic contaminants).
Example 11
Effect of ozone addition on particle contamination cleaning test
Only the way of adding ozone in example 1 is changed, the way of adding ozone ice blocks is replaced by the way of adding ozone water or adding ozone gas, and the rest conditions are not changed. Finally, according to the particle pollutant detection test, the removal rate of the particle pollutants is calculated, and the test data is shown in table 4:
TABLE 4
| Ozone ice | Ozone water | Ozone gas | |
| Removal rate of particulate contaminants having particle size of 40nm or more and less than 100nm | 99.67% | 92.76% | 90.11% |
| Removing rate of particle pollutants with particle size of more than or equal to 100nm and less than 200nm | 99.83% | 96.18% | 95.83% |
| Removal rate of particle pollutants with particle size of more than or equal to 200nm | 99.98% | 99.97% | 99.95% |
The ozone ice cake is added in a mode of ozone ice cake, and the concentration of ozone in the ozone ice cake is 12 ppm-13 ppm.
The ozone water is added in an ozone water mode, and the concentration of ozone in the ozone water is 6 ppm-7 ppm.
The ozone gas is added in such a way that the concentration of ozone in the ozone gas is 3 percent (volume fraction).
Utilizing high-voltage static electricity generated by an ozone generator to ionize oxygen molecules in the air near the electrodes to generate ozone in a short time, and utilizing an air-water mixer to mix the ozone in water to generate ozone water; cooling, freezing and freezing the ozone water to generate ozone ice; the corresponding process is the prior art, and for example, a paper "comparative analysis of preparation method of high-concentration ozone ice" published by Sun yoga of the university of Western Ann transportation can be seen.
Ozone is easily dissolved in water and decomposed. Ozone is added in an ozone ice mode, so that the stability of the ozone in a system can be improved, the ozone is released continuously and stably, and the oxidizability of the system is improved.
In the above embodiment, although the metal contamination on the surface of the silicon carbide wafer can be removed by the existing cleaning method; but the organic pollutants on the surface of the material are very difficult to clean; in addition, no matter the cleaning mode of adding a medicament (a surfactant and a metal chelating agent) or ultrasonic vibration cleaning is adopted, the particle pollutants on the surface of the silicon carbide wafer can not be removed by 100 percent in the primary cleaning; especially in the existing methods for cleaning organic contaminants, new particulate contaminants are easily introduced.
In the existing process of cleaning the surface of a silicon carbide wafer,the invention can remove the organic matters introduced in the previous process. The use of ionic liquids as activators also accelerates the chemical reaction process. The cleaning principle is to oxidize organic pollutants on the surface of the silicon carbide wafer in a catalytic way by means of electrolysis, and especially, a large amount of particles with strong oxidizing property are generated in the electrolysis process. Further, the hydroxyl radical in the cell is O3The oxidation property is further enhanced by (1). O released from ozone ice3Can combine and under the electric field force effect with the hydroxyl free radical at low temperature, further improve oxidation performance, be greater than the independent oxidizing power of ozone water and ozone gas far away, when oxidation organic pollutant, can be with the particle size increase, the structure collapse of its near granule footpath granule pollutant, reduce the adsorption affinity to make the degree of difficulty of getting rid of some granule footpath granule pollutants show and reduce.
The invention adopts a special anode and a catalytic coating titanium electrode, so that the service life of particles with strong oxidizing property in the solution near the anode is kept high, thereby improving the stability of oxidation and the catalytic activity. When the catalytic coating titanium electrode is used for preparing a coating, if a thermal spraying mode is adopted, the cerium dioxide-metal organic framework composite material loses catalytic activity, and the removal rate of organic pollutants is directly reduced. Therefore, by means of ultrasonic rapid cold spraying, the company entrusts university of great graduate with the coating processing.
The surface of the silicon carbide wafer is firstly subjected to activation treatment, and then the strong oxidizing liquid generated by electrolysis is utilized to be matched with the action of an electric field, so that the surface of the silicon carbide wafer can be effectively cleaned, organic pollutants on the surface can be effectively removed, and particle pollutants on the surface can be thoroughly removed; the invention can not damage the surface of the wafer, thereby obtaining the most excellent cleaning effect.
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.
Claims (7)
1. A method for cleaning organic pollutants on the surface of a silicon carbide wafer is characterized by comprising the following steps:
step one, surface treatment
Putting the silicon carbide wafer into an ultrasonic cleaning tank, pouring an activating solution into the ultrasonic cleaning tank, and soaking for 10-15 min; then carrying out ultrasonic cleaning in an ultrasonic cleaning tank, wherein the temperature in the tank is kept at 65-68 ℃, the ultrasonic frequency is 66-72 kHz, and the ultrasonic cleaning time is 15-20 min; after ultrasonic cleaning, sending the mixture into a constant-temperature oven for drying;
step two, deep cleaning
An ion exchange membrane is arranged in the middle of the electrolytic cell, the electrolytic cell is divided into a cathode cell and an anode cell by a semi-homogeneous ion exchange membrane, the cathode of the electrolytic cell is positioned in the cathode cell, and the anode of the electrolytic cell is positioned in the anode cell; pouring electrolyte between the cathode and the anode of the electrolytic cell, controlling the pH of the solution in the cathode to be more than 13 by using strong alkali solution, adding ozone into the anode cell, and electrolyzing for 3-5 min; and (3) putting the silicon carbide wafer subjected to surface treatment into an electrolytic bath, continuing to electrolyze for 3-5 min, taking out the silicon carbide wafer, cleaning with pure water, drying and storing.
2. The method for cleaning organic contaminants on the surface of a silicon carbide wafer according to claim 1, wherein: the activating solution is 1-butyl-3-methylimidazole dibutyl phosphate solution with the mass fraction of 1.3-1.7%.
3. The method for cleaning organic contaminants on the surface of a silicon carbide wafer according to claim 2, wherein: the activating liquid is 1.6 mass percent of 1-butyl-3-methylimidazol dibutyl phosphate solution.
4. The method for cleaning organic contaminants on the surface of a silicon carbide wafer according to claim 1, wherein: the cathode of the electrolytic cell adopts low-carbon steel as an electrode, and the anode of the electrolytic cell adopts a catalytic coating titanium electrode; the catalytic coating titanium electrode is characterized in that a coating is formed on the surface of a titanium plate by using a powdery cerium dioxide-metal organic framework composite material in an ultrasonic rapid cold spraying mode, the temperature of the ultrasonic rapid cold spraying is 75-80 ℃, and the thickness of the coating is 1-2 mm.
5. The method for cleaning organic contaminants on the surface of a silicon carbide wafer according to claim 1, wherein: the electrolyte is one or more of a sodium sulfate solution, a potassium sulfate solution, a sodium phosphate solution and a potassium phosphate solution.
6. The method for cleaning organic contaminants on the surface of a silicon carbide wafer according to claim 1, wherein: the strong base in the strong base solution is one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide, rubidium hydroxide and strontium hydroxide.
7. The method for cleaning organic pollutants on the surface of a silicon carbide wafer according to claim 1, characterized in that: the ozone added into the anode tank is added in the form of ozone ice blocks, and the concentration of the ozone in the ozone ice blocks is 12 ppm-13 ppm.
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