CN113675073A - Wafer cleaning method - Google Patents
Wafer cleaning method Download PDFInfo
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- CN113675073A CN113675073A CN202110976594.XA CN202110976594A CN113675073A CN 113675073 A CN113675073 A CN 113675073A CN 202110976594 A CN202110976594 A CN 202110976594A CN 113675073 A CN113675073 A CN 113675073A
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Images
Classifications
-
- 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
-
- 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
- B08B3/02—Cleaning by the force of jets or sprays
-
- 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
- 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
-
- 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
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
-
- 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
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
- H01L21/02052—Wet cleaning only
Abstract
The invention provides a wafer cleaning method, which comprises the following steps: the wafers were subjected to DIW cleaning, SPM cleaning, HQDR cleaning, QDR1 cleaning, QDR2 cleaning, high concentration SC1 cleaning, QDR3 cleaning, DHF cleaning, QDR4 cleaning, low concentration SC1 cleaning, QDR5 cleaning, SC2 cleaning, and QDR6 cleaning in this order. The cleaning method provided by the invention has strong pertinence to specific dirt, designs a cleaning flow from the dirt removing principle, and has the advantages of short cleaning flow and no operation danger.
Description
Technical Field
The invention belongs to the technical field of wafers, and particularly relates to a wafer cleaning method.
Background
The surface of the wafer to be initially processed has a lot of dirt particles, and in order to achieve the maximum and most efficient utilization rate of the wafer, the particles on the surface of the wafer need to be removed. The current mainstream cleaning process of the wafer adopts wet cleaning, the excellent wet cleaning process needs to effectively remove various stains on the surface of the wafer, meanwhile, the wafer surface is not damaged or seriously etched, various residues are not adhered, and the production and the use are simple and safe.
The surface of the wafer is contaminated mainly by inorganic matters, organic compounds and alloying dirt, and the shallow surface layer of the wafer is also contaminated by partially fusing with the wafer, and the shallow surface layer is the dirt embedded into an oxide layer after the surface of the wafer is oxidized.
Disclosure of Invention
In view of the above, the present invention provides a wafer cleaning method, which has less residual particles and high surface and shallow surface cleanliness after wafer cleaning.
The invention provides a wafer cleaning method, which comprises the following steps:
carrying out DIW cleaning, SPM cleaning, HQDR cleaning, QDR1 cleaning, QDR2 cleaning, high-concentration SC1 cleaning, QDR3 cleaning, DHF cleaning, QDR4 cleaning, low-concentration SC1 cleaning, QDR5 cleaning, SC2 cleaning and QDR6 cleaning on the wafer in sequence;
the reagent for cleaning the SPM comprises: h2SO4And H2O2；
The reagents for the high-concentration SC1 washing and the low-concentration SC1 washing comprise: NH (NH)4OH、H2O2And H2O；
The DHF cleaning reagent comprises: HF and H2O；
The SC2 cleaning reagent comprises: HCl, H2O2And H2O。
Preferably, the DIW cleaning time is 30-60 min; the flow rate is 0.5 to 1L/min.
Preferably, the temperature for cleaning the SPM is 90-140 ℃ and the time is 8-15 min.
Preferably, the temperature for cleaning the high-concentration SC1 is 50-75 ℃ and the time is 5-15 min.
Preferably, the time for cleaning the DHF is 15 s-10 min; the temperature was room temperature.
Preferably, the temperature for cleaning the low-concentration SC1 is 50-75 ℃ and the time is 5-15 min.
Preferably, the temperature of the SC2 cleaning is 70-80 ℃, and the time is 5-15 min.
Preferably, after the QDR6 is cleaned, the method further comprises:
drying the cleaned wafer;
the drying temperature is 30-50 ℃.
Preferably, H in the SPM-washed reagent2SO4And H2O2The volume ratio of (2-5) to (1).
Preferably, the high concentration of NH in the SC1 cleaning reagent4OH、H2O2And H2The volume ratio of O is 1 (1-2) to 5-6;
NH in the reagent for cleaning the low-concentration SC14OH、H2O2And H2The volume ratio of O is (0.1-0.5): 1: 5.
the improved cleaning mode of the traditional wet chemical cleaning process comprises soaking type chemical cleaning and/or spray type single-groove chemical cleaning; the adopted cleaning agent is selected from one or more of sulfuric acid-hydrogen peroxide mixed liquor (SPM), ammonia water-hydrogen peroxide-water mixed liquor (SC1), hydrochloric acid-hydrogen peroxide-water mixed liquor (SC2) and hydrofluoric acid-water mixed liquor (DHF) or liquid medicines with different concentrations; the cleaning agent can oxidize, dissolve and complex to remove organic contamination, inorganic pollutants and metal ions on the Wafer surface.
The invention adopts DIW pretreatment preferentially, can soak and soften organic or partial inorganic dirt on the surface of the wafer, and is convenient for subsequent corrosion cleaning; after the SPM is adopted, the sizes of the dirty particles are combined, and different ultrasonic frequencies are adopted to remove the particles with different sizes step by step; meanwhile, after DHF is cleaned by SC1 again, an oxide layer generated in a series of previous operations can be effectively removed; finally, the wafers were cleaned with different concentrations of SC1 to specifically remove the very fine adsorbed particles. Finally, the purpose that few particles on the surface of the wafer are remained is achieved, the surface cleanliness of the wafer is improved, the effective use area of the wafer is greatly increased, and the use area utilization rate of the wafer is improved.
Compared with the prior art, the wet cleaning process is designed on the basis of the cleaning principle, and is short in cleaning process and simple and convenient to operate; the invention combines the wafer wet cleaning principle, has the advantages of pertinently treating the pollutants on the surface of the wafer step by step and circularly, reducing the residual quantity of particles, dirt and metal ions and greatly improving the wafer quality.
Drawings
FIG. 1 is a picture of the results of the test of particles of 0.18 μm or more after the wafer is cleaned according to the method provided in example 1 of the present invention;
FIG. 2 is a picture of the results of the test of particles of 0.18 μm or more after the wafer is cleaned according to the method provided in example 2 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used were all conventional methods unless otherwise specified.
The invention provides a wafer cleaning method, which comprises the following steps:
the wafers were subjected to DIW cleaning, SPM cleaning, HQDR cleaning, QDR1 cleaning, QDR2 cleaning, high concentration SC1 cleaning, QDR3 cleaning, DHF cleaning, QDR4 cleaning, low concentration SC1 cleaning, QDR5 cleaning, SC2 cleaning, and QDR6 cleaning in this order.
In the present invention, the wafer is preferably a silicon carbide wafer and/or a silicon wafer.
In the present invention, the wafer is preferably a wafer after polishing and cleaning.
In the present invention, the grinding and polishing process preferably includes: double-sided grinding, double-sided rough grinding, double-sided finishing and double-sided polishing.
In the present invention, the surface roughness of the crystal after the grinding and polishing is preferably 1 μm or less.
In the invention, the cleaning treatment process preferably adopts a cleaning mode of removing organic matters and partial inorganic matters on the surface of the wafer by alkali liquor.
In the invention, the cleaning mode in the wafer cleaning process is preferably groove cleaning; the cleaning mode in the wafer cleaning process is preferably selected from one or more of ultrasonic cleaning, megasonic cleaning, wet oxidation cleaning, etching corrosion cleaning and complexing cleaning.
In the invention, the DIW cleaning reagent is preferably water, more preferably deionized water, and the resistivity of the deionized water is preferably 16-20M omega-cm, more preferably 17-19M omega-cm, and most preferably 18M omega-cm; the number of particles with the particle size of more than or equal to 0.05 micron in the deionized water is preferably 36/ml, the content of primary heavy metals (Fe, Cr, Ni, Cu, Zn, Au, Ag and Hg), secondary alkali metals (Li, Na and K) and light elements (Mg, Al, Ca, C, S, Cl and F) preferably meets the requirement of less than or equal to 5E10atoms/cm2。
In the present invention, the DIW cleaning is preferably a slow rinse. In the invention, the DIW cleaning time is preferably 30-60 min, more preferably 40-50 min, and most preferably 45 min; the flow rate is preferably 0.5-1L/min, more preferably 0.6-0.9L/min, and most preferably 0.7-0.8L/min; the temperature is preferably normal temperature, more preferably 20-30 ℃, more preferably 22-28 ℃, and most preferably 24-26 ℃.
The invention adopts DIW cleaning, and after the DIW cleaning is carried out by using deionized water, the surface of the wafer is cleaned after being softened by dirt.
In the invention, the SPM cleaning is used for removing most organic pollutants on the surface of the wafer, is wet oxidation cleaning, and removes most organic pollutants on the surface of the wafer by an oxidation corrosion principle. The surface of the wafer mainly has an organic film, and the organic film is generally hydrophobic, so that other cleaning liquids are prevented from reaching the surface of the wafer, and therefore the surface organic film needs to be removed in the cleaning treatment.
In the present invention, the SPM washing reagent includes: h2SO4And H2O2。
In the present invention, said H2SO4The mass concentration is preferably 96-98%More preferably 97 to 98%, most preferably 98%; said H2O2The mass concentration of (A) is 25 to 35%, more preferably 28 to 32%, most preferably 31%.
In the present invention, said H2SO4And H2O2The volume ratio of (2-5): 1 is preferable, the ratio of (3-4): 1 is more preferable, and the ratio of (3.5): 1 is most preferable.
In the invention, the temperature for cleaning the SPM is preferably 90-140 ℃, more preferably 100-130 ℃, and most preferably 110-120 ℃; the cleaning time is preferably 8-15 min, more preferably 9-14 min, more preferably 10-13 min, and most preferably 11-12 min.
In the invention, in the SPM cleaning process, the wafer is preferably completely immersed in the cleaning reagent, and the wafer is circularly washed by the circulating pump.
In the invention, the HQDR cleaning is used for washing away large oxidized particles, mainly removing particles larger than 5 microns, washing away SPM residual liquid and dirt particles adhered to the surface of a wafer, and simultaneously, impacting and crushing large dirt by using low-frequency ultrasound to accelerate the falling of the dirt.
In the present invention, the HQDR cleaning refers to cleaning of Hot DIW.
In the present invention, the HQDR cleaning is preferably a soak cleaning. In the invention, the HQDR cleaning is preferably ultrasonic cleaning, the ultrasonic frequency is preferably 20-30 kHZ, more preferably 22-28 kHZ, and most preferably 24-26 kHZ; the cleaning temperature is preferably 50-90 ℃, more preferably 60-80 ℃, and most preferably 70 ℃; the cleaning time is preferably 5-8 min, and more preferably 6-7 min.
In the present invention, the QDR is an abbreviation for quick dump ring.
In the invention, the QDR1 cleaning method is mainly used for removing particles with the particle size of 2-5 microns.
In the present invention, the solvent for QDR1 cleaning is the same as that for DIW cleaning, and is not described herein again.
In the invention, the QDR1 cleaning is preferably ultrasonic cleaning, and more preferably the wafer is placed in a water tank for ultrasonic cleaning; the ultrasonic frequency is preferably 30-50 kHZ, more preferably 35-45 kHZ and most preferably 40 kHZ; the cleaning temperature is preferably 20-30 ℃, more preferably 22-28 ℃, and most preferably 24-26 ℃; the cleaning time is preferably 3-5 min, and more preferably 4 min.
In the present invention, the QDR1 cleaning is preferably performed twice at a single spray-type cleaning interval, and the loosened contaminants on the wafer surface are preferably cleaned by using a quick rinse tank (QDR) after each cleaning.
In the invention, the QDR1 cleaning mainly removes the crushed particles in the last step, the particles with the corresponding size are processed by specific ultrasonic frequency, the particles with the size of 2-5 microns are mainly removed in the step, the loose dirt on the surface of the wafer is washed by using a quick discharge washing tank, and the particles are taken away by using DIW.
In the invention, the QDR2 cleaning mainly removes 1-5 micron particles, and simultaneously further softens dirt on the surface of the wafer, thereby facilitating the removal of the particles in the next step.
In the present invention, the QDR2 cleaning solvent is the same as the solvent for DIW cleaning, and is not described herein again.
In the invention, the QDR2 cleaning is preferably ultrasonic cleaning, and more preferably the wafer is placed in a water tank for ultrasonic cleaning; the ultrasonic frequency is preferably 70-90 kHZ, more preferably 75-85 kHZ, and most preferably 80 kHZ; the cleaning temperature is preferably room temperature, more preferably 20-30 ℃, more preferably 22-28 ℃, and most preferably 24-26 ℃; the cleaning time is preferably 3-5 min, and more preferably 4 min.
In the invention, the SC1 cleaning is micro-etching and complexing cleaning. In the present invention, the reagents for high concentration SC1 cleaning include: NH (NH)4OH、H2O2And H2O。
In the present invention, the NH4OH、H2O2And H2The volume ratio of O is preferably 1 (1-2): (5-6), more preferably 1 (1.2-1.8): 5.2-5.8), and most preferably 1 (1.4-1.6): 5.4-5.6).
In the invention, the temperature for cleaning the high-concentration SC1 is preferably 50-70 ℃, more preferably 55-65 ℃, and most preferably 60 ℃; the time is preferably 5-15 min, more preferably 8-12 min, and most preferably 10 min; the cleaning is preferably ultrasonic cleaning; the frequency of ultrasonic cleaning is preferably 160-180 kHZ, more preferably 165-175 kHZ and most preferably 170 kHZ.
In the invention, the high-concentration SC1 cleaning can slowly dissolve dirty particles, mainly remove particles larger than 0.5 micron, correspondingly increase the number of particles smaller than 0.5 micron, remove metal by utilizing self-complexation reaction, and effectively dissolve SiO on the surface of a wafer2Forming a new and non-fouling oxide layer, and having self-cleaning effect.
In the invention, the hydrophobic organic film still exists on the surface of the wafer cleaned by the SPM, the high-concentration SC1 cleaning is combined with the SPM cleaning, so that the cleaning effect for removing the organic film on the surface and adhering dirt is stronger, and particularly for the wafer with serious organic pollution, the SPM cleaning at the temperature of more than 100 ℃ and the high-concentration SC1 cleaning at the temperature of 80 ℃ are combined for treatment.
In the invention, the QDR3 cleaning process has a critical adhesive layer, so that the particles are internally blasted under the action of external pressure, and megasonic waves of megasonic cleaning are mainly used for removing small particles of 0.1-0.3 microns.
In the present invention, the QDR3 cleaning solvent is identical to the DIW cleaning solvent, and will not be described herein.
In the invention, the QDR3 cleaning is preferably megasonic cleaning, the megasonic frequency is preferably 740-760 kHZ, more preferably 745-755 kHZ, and most preferably 750 kHZ; the cleaning temperature is preferably room temperature, more preferably 20-30 ℃, more preferably 22-28 ℃, and most preferably 24-26 ℃; the cleaning time is preferably 3-5 min, and more preferably 4 min.
In the invention, the DHF cleaning is micro-etching stripping cleaning, which mainly carries out micro-etching on embedded dirt particles on the surface of the wafer and particles in a superficial oxidation layer on the surface of the wafer so as to further clean the surface of the wafer. In the present invention, the DHF cleaning process is performed with free H+Is an etching body to corrode the wafer surface, accelerate the exposure of the wafer surface, and remove SiO containing metal or nonmetal dirt2And corroding and stripping the thermal growth layer.
In the present invention, the DHF cleaning agent comprises: HF and H2O。
In the present invention, the HF and H2The volume ratio of O is preferably 1 (20-50), more preferably 1 (30-40), and most preferably 1: 35.
In the invention, the time for cleaning the DHF is preferably 15 s-10 min, more preferably 30 s-8 min, more preferably 1-6 min, more preferably 2-5 min, and most preferably 3-4 min; the temperature is preferably room temperature, more preferably 20-30 ℃, more preferably 22-28 ℃, and most preferably 24-26 ℃.
In the invention, the QDR4 cleaning can remove residual DHF stains H on the surface of the wafer2O2The effect of (2) is to further accelerate the oxidation corrosion of the wafer surface and further remove the dirt on the wafer surface.
In the present invention, the QDR4 cleaning solvent is the same as the solvent for DIW cleaning, and is not described herein again. In the present invention, the solvent for QDR4 washing preferably further contains H2O2(ii) a Said H2O2The mass of (b) is preferably 8 to 12%, more preferably 9 to 11% of the mass of the solvent. Most preferably 10%.
In the invention, the QDR4 cleaning time is preferably 5-15 min, more preferably 8-12 min, and most preferably 10 min; the cleaning temperature is preferably room temperature, more preferably 20-30 ℃, more preferably 22-28 ℃, and most preferably 24-26 ℃.
In the present invention, the low concentration SC1 wash is capable of removing particles smaller than 0.5 microns. In the present invention, the reagents for low concentration SC1 cleaning include: NH (NH)4OH、H2O2And H2O。
In the present invention, the NH4OH、H2O2And H2The volume ratio of O is preferably (0.1-0.5): 1: 5, more preferably (0.2 to 0.4): 1: 5, most preferably 0.3: 1: 5.
in the invention, the low-concentration SC1 treatment reagent has the efficacy of a surfactant and can effectively remove organic matters, the low-concentration SC1 reagent is beneficial to removing particles smaller than 0.5 micron, and meanwhile, the low-concentration SC1 reagent can also avoid certain microroughness of the surface of a silicon wafer caused by uneven local micro-etching, so that the surface of the silicon wafer is protected from severe corrosion, and surface adhered particles can be effectively removed.
In the invention, the temperature for cleaning the low-concentration SC1 is preferably 50-75 ℃, more preferably 55-70 ℃, and most preferably 60-65 ℃; the cleaning time is preferably 5-15 min, more preferably 8-12 min, and most preferably 10 min; the cleaning is preferably megasonic cleaning, and the megasonic frequency is preferably 740 to 760kHZ, more preferably 745 to 755kHZ, and most preferably 750 kHZ.
In the present invention, the QDR5 cleaning is mainly to impact SC1 treated particles down to carry them away with DIW, which helps to further remove the particles.
In the present invention, the QDR5 cleaning solvent is the same as the solvent for DIW cleaning, and is not described herein again.
In the invention, the QDR5 cleaning is preferably megasonic cleaning, the megasonic frequency is preferably 740-760 kHZ, more preferably 745-755 kHZ, and most preferably 750 kHZ; the cleaning time is preferably 3-7 min, more preferably 4-6 min, and most preferably 5 min; the cleaning temperature is preferably room temperature, more preferably 20-30 ℃, more preferably 22-28 ℃, and most preferably 24-26 ℃.
In the invention, the SC2 cleaning is ion complexing cleaning which is mainly used for generating soluble ion complex, removing alkali metal ions and metal hydroxide, and dissolving residual metal to form a protective and passivated hydrated oxide film.
In the present invention, the SC2 cleaning reagent comprises: HCl, H2O2And H2O。
In the invention, the HCl and H2O2And H2The volume ratio of O is preferably 1: 1: (5-10), more preferably 1: 1: (6-9), most preferably 1: 1: (7-8).
In the invention, the temperature of SC2 cleaning is preferably 70-80 ℃, more preferably 72-78 ℃, and most preferably 74-76 ℃; the cleaning time is preferably 5-15 min, more preferably 8-12 min, and most preferably 10 min.
In the present invention, the QDR6 cleaning is used to clean a chemical solution such as a contaminant chemical solution or an ion complex metal substance remaining on the wafer surface.
In the present invention, the QDR6 cleaning solvent is the same as the solvent for DIW cleaning, and is not described herein again.
In the invention, the QDR6 cleaning time is preferably 3-7 min, more preferably 4-6 min, and most preferably 5 min; the cleaning temperature is preferably 20-30 ℃, more preferably 22-28 ℃, and most preferably 24-26 ℃.
In the invention, the purity of the sulfuric acid, the hydrogen peroxide, the ammonia water, the hydrochloric acid and the hydrofluoric acid is preferably electronic grade.
In the present invention, after the QDR6 is cleaned, the method preferably further includes:
the cleaned wafer is dried.
In the invention, the drying temperature is preferably 30-50 ℃, more preferably 35-45 ℃, and most preferably 40 ℃; the drying time is preferably 3-15 min, more preferably 5-12 min, and most preferably 8-10 min. In the present invention, the method of drying is preferably spin drying; the rotation speed of the rotary drying is preferably 600-1000 rpm, more preferably 700-900 rpm, and most preferably 800 rpm; the gas used for the spin drying is preferably hot nitrogen gas, more preferably filtered hot nitrogen gas.
The invention provides a wafer cleaning method improved on the traditional wet cleaning process, which comprises the following steps: and carrying out improved wet cleaning process cleaning on the wafer after the grinding, polishing and cleaning treatment, wherein the improved wet cleaning process comprises DIW cleaning, SPM cleaning, HQDR cleaning, QDR1 cleaning, QDR2 cleaning, high-concentration SC1 cleaning, QDR3 cleaning, DHF cleaning, QDR4 cleaning, low-concentration SC1 cleaning, QDR5 cleaning, SC2 cleaning, QDR6 cleaning and spin drying.
The improved cleaning mode of the traditional wet chemical cleaning process comprises soaking type chemical cleaning and/or spray type single-groove chemical cleaning; the adopted cleaning agent is selected from one or more of sulfuric acid-hydrogen peroxide mixed liquor (SPM), ammonia water-hydrogen peroxide-water mixed liquor (SC1), hydrochloric acid-hydrogen peroxide-water mixed liquor (SC2) and hydrofluoric acid-water mixed liquor (DHF) or liquid medicines with different concentrations; the cleaning agent can oxidize, dissolve and complex to remove organic contamination, inorganic pollutants and metal ions on the Wafer surface.
Compared with the prior art, the wet cleaning process is designed on the basis of the cleaning principle, and is short in cleaning process and simple and convenient to operate; the invention combines the wafer wet cleaning principle, has the advantages of pertinently treating the pollutants on the surface of the wafer step by step and circularly, reducing the residual quantity of particles, dirt and metal ions and greatly improving the wafer quality.
The wafer cleaning process provided by the invention has strong pertinence to cleaning of dirt, is designed from the dirt removal principle, is short and has no operation danger. The experimental results show that: the average number of particles with the particle diameter of more than or equal to 0.18 mu m of the cleaned wafer can reach within 100 per wafer.
For further illustration of the present invention, the following examples are provided to describe the method of the present invention for improving the conventional wet cleaning process in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
The silicon carbide wafer which is cleaned by alkali liquor and has the surface roughness less than or equal to 1 micron is used as the wafer by double-sided grinding, double-sided coarse grinding, double-sided fine trimming and double-sided polishing.
The wafer was rinsed slowly with DIW for 30min at a flow rate of 0.5L/min at room temperature with a reagent of 18 mohm cm of deionized water.
The wafer after DIW rinsing was processed using SPM, reagents: h2SO4(98% by mass) and H2O2The dosage (mass concentration is 31%) is respectively 13.33L and 6.67L, the temperature is 100 ℃, the treatment time is 12min, the wafer is completely immersed, and the wafer is circularly washed by a circulating pump. The wet oxidizing agent is effective in removing organic contaminants from the wafer surface, and the oxidation of the peroxide therein plays a crucial role.
Further, the wafer was immersed in an HQDR at an ultrasonic frequency of 25kHZ and a temperature of 80 ℃ under a constant DIW temperature of 80 ℃ controlled by the HQDR (the reagent was deionized water having a resistivity of 18 M.OMEGA.. multidot.cm). The step can effectively remove the dirty liquid medicine which is difficult to wash away, and simultaneously, the residual organic matters on the surface are further crushed, so that the particles larger than 5 microns are mainly dropped, and the large particle residue is reduced.
Next, carrying out QDR1 treatment on the HQDR-treated wafer (the reagent is deionized water with the resistivity of 18M omega cm), wherein the ultrasonic frequency is 40kHZ, the temperature is room temperature, and the treatment time is 5min, wherein particles with the particle size of 2-5 microns are mainly removed in the step, the wafer is mainly treated for 2 times at intervals by adopting a spraying type single-groove cleaning method, and after cleaning each time, loose dirt on the surface of the wafer is washed by using a quick discharge washing groove (QDR, quick dump ring, the same below).
And then cleaning the wafer by QDR2 (the reagent is deionized water with the resistivity of 18M omega cm), wherein the ultrasonic frequency is 80kHZ, the temperature is room temperature, and the processing time is 5min, and the wafer is mainly used for removing particles with the particle size of 1-5 mu M.
The processed wafer is cleaned by SC1, and the chemical liquid for cleaning the SC1 comprises the following components in percentage by weight: NH (NH)4OH、H2O2And H2The volume ratio of O is 1: 2: 6, the temperature is 50 ℃, the time is 15min, the ultrasonic frequency is 170kHZ, the cleaning mode can slowly dissolve the dirt particles, mainly remove the particles larger than 0.5 micron, correspondingly increase the number of the particles smaller than 0.5 micron, then remove metal by utilizing the self complexing reaction, and simultaneously can effectively dissolve SiO on the surface of the wafer2Forming a new and non-fouling oxide layer, and having self-cleaning effect.
The wafer was further subjected to QDR3 cleaning (reagent is deionized water with a resistivity of 18M Ω · cm), megasonic frequency of 750kHZ, temperature of room temperature, processing time of 5min, mainly for removal of fine particles.
And cleaning the wafer by DHF, wherein the liquid medicine for cleaning the wafer by DHF comprises the following components in percentage by weight: HF and H2The volume ratio of O is 1: and 20, keeping the temperature at room temperature for 5min, mainly carrying out micro etching on embedded dirt particles on the surface of the wafer and particles in a shallow oxidation layer on the surface of the wafer, and further cleaning the surface of the wafer.
Then, the wafer is cleaned by QDR4 (the reagent is deionized water with the resistivity of 18M omega c.m) for 10min, the temperature is room temperature, and the method is mainly used for removing the residual DHF stains on the surface of the wafer.
The wafer cleaned by QDR4 is cleaned again by SC1, and the chemical liquid for cleaning SC1 comprises the following components in percentage by weight: NH (NH)4OH、H2O2And H2The volume ratio of O is 0.1: 1: 5 at a temperature of 70 ℃ for 10min, the low concentration of SC1 removed mainly particles smaller than 0.5 microns.
The wafers were then subjected to QDR5 rinse (reagent is deionized water with a resistivity of 18M Ω · cm) for 5min at room temperature and at megasonic frequency of 750kHZ, which was operated to essentially knock down the SC1 treated particles and carry them away with DIW.
Then the wafer is processed by SC2, and the chemical liquid for cleaning the SC2 comprises the following components in percentage by weight: HCl, H2O2And H2The volume ratio of O is 1: 1: and 8, the temperature is 75 ℃, the time is 8min, and the method is mainly used for generating a soluble ion complex and removing alkali metal ions and metal hydroxides.
The wafer after the SC2 treatment was cleaned with QDR6 (deionized water having a resistivity of 18M Ω · cm) at room temperature for 5min, and the chemical solution such as an ionic complex remaining on the wafer surface was rinsed off.
And finally, carrying out hot nitrogen spin-drying on the wet wafer, wherein the treatment mode is the filtered dry hot nitrogen, the temperature is 40 ℃, the rotating speed is 900rpm, and the treatment time is 10 min.
The Candela surface defect detector is adopted for detection, 24191 particles with the particle size of more than 0.18 micron are on the surface of the wafer before cleaning, and compared with the traditional process, the wafer subjected to the cleaning treatment can control the particle size of more than 0.18 micron to 54 particles per wafer, as shown in figure 1.
Example 2
The silicon wafer which is cleaned by alkali liquor and has the surface roughness less than or equal to 1 micron is used as the wafer by double-sided grinding, double-sided coarse grinding, double-sided fine trimming and double-sided polishing.
Slowly washing the wafer by using DIW (DiW), wherein the washing time is 1h, the flow rate is 0.7L/min, and the temperature is normal temperature; the reagent was deionized water with a resistivity of 18M Ω cm. .
The DIW-rinsed wafer was treated with SPM, reagent H2SO4(98% by mass) and H2O2The mass concentration is 31 percent, the dosage is respectively 16L and 4L, the temperature is 110 ℃, the processing time is 10min, the wafer is completely immersed, and the circulating pump circularly washes the liquid medicine on the surface of the wafer; in this case, the organic film is mainly present on the wafer surface, and the organic film is generally hydrophobic, and prevents other cleaning liquids from reaching the wafer surface.
Further soaking the wafer in HQDR (reagent is deionized water with resistivity of 18M omega cm), and ultrasonic frequency is 25kHZ and temperature is 75 deg.C; the HQDR constant temperature is controlled to be 75 ℃ under the DIW temperature. The HQDR mainly aims to wash away SPM residual liquid and dirt particles adhered to the surface of a wafer, and simultaneously utilizes low-frequency ultrasound to impact and crush large dirt blocks so as to accelerate the falling of the dirt.
Then, carrying out QDR1 treatment on the HQDR treated wafer (the reagent is deionized water with the resistivity of 18M omega cm), wherein the ultrasonic frequency is 40kHZ, the temperature is room temperature, and the treatment time is 10min, the step mainly removes the crushed particles in the previous step, the specific ultrasonic frequency treats the particles with the corresponding size, the step mainly removes the particles with the size of 2-5 microns, the loose dirt on the surface of the wafer is washed by using a quick discharge washing tank, and the particles are taken away by using DIW.
And then cleaning the wafer by QDR2 (the reagent is deionized water with the resistivity of 18M omega cm), wherein the ultrasonic frequency is 80kHZ, the temperature is room temperature, the processing time is 10min, and after QDR2 processing, 1-5 mu M of dirt particles on the surface of the wafer are removed, and meanwhile, the dirt on the surface of the wafer is further softened, so that the particles can be conveniently removed in the next step.
Then the wafer is cleaned by SC1, and the liquid medicine for cleaning SC1 comprises the following components in percentage by weight: NH (NH)4OH、H2O2And H2The volume ratio of O is 1: 1: 5, the temperature is 80 ℃, the time is 7min, the ultrasonic frequency is 170kHZ, a hydrophobic organic film still exists on the surface of the wafer treated by SPM, SC1 is combined with SPM, the cleaning effect on removing the organic film on the surface and adhering dirt is stronger, especially for the wafer with serious organic pollution, the SPM with the temperature of more than 100 ℃ is required to be combined with the SC1 with the temperature of 80 DEG CAnd (6) processing.
Further, the wafer is subjected to QDR3 cleaning (the reagent is deionized water with the resistivity of 18M omega cm), the megasonic frequency is 750kHZ, the temperature is room temperature, the treatment time is 5min, a 0.61 micron critical adhesive layer is formed, particles are subjected to internal blasting by external pressure, and the 750kHZ megasonic wave is mainly used for removing 0.1-0.3 micron small particles.
And cleaning the wafer by DHF, wherein the liquid medicine for cleaning the wafer by DHF comprises the following components in percentage by weight: HF and H2The volume ratio of O is 1: 20 at room temperature for 5min, free H in DHF+Is an etching body to corrode the wafer surface, accelerate the exposure of the wafer surface, and remove SiO containing metal or nonmetal dirt2And corroding and stripping the thermal growth layer.
The wafer was then subjected to QDR4 (reagent was deionized water having a resistivity of 18M Ω. cm and also contained a certain amount of H)2O2，H2O210% in the reagent), and cleaning for 10min at room temperature, wherein the cleaning solution is mainly used for removing residual DHF (dehydroepiandrosterone) stains on the surface of the wafer, and H is used for removing residual DHF stains on the surface of the wafer2O2The effect of (2) is to further accelerate the oxidation corrosion of the wafer surface and further remove the dirt on the wafer surface.
The wafer cleaned by QDR4 is cleaned again by SC1, and the chemical liquid for cleaning SC1 comprises the following components in percentage by weight: NH (NH)4OH、H2O2And H2The volume ratio of O is 0.5: 1: 5, the temperature is 70 ℃, the time is 10min, the low-concentration SC1 has the efficacy of a surfactant and can effectively remove organic matters, the low-concentration SC1 is beneficial to removing particles smaller than 0.5 micron, and meanwhile, the low-concentration SC1 can also avoid certain microroughness of the surface of the silicon wafer caused by uneven local micro-etching, so that the surface of the silicon wafer is protected from severe corrosion, and surface adhered particles can be effectively removed.
The wafer was then subjected to QDR5 rinse (reagent is deionized water with a resistivity of 18M Ω · cm) for a treatment time of 5min at room temperature and at a megasonic frequency of 750kHZ, which facilitates further removal of wafer particles.
Then the wafer is processed by SC2, and the chemical liquid for cleaning the SC2 comprises the following components in percentage by weight: HCl, H2O2And H2Volume of O is 1: 1: and 7, the temperature is 50-70 ℃, the temperature does not need to be accurately controlled, the treatment time is 9min, the alkali metal ions and the metal hydroxide are favorably removed, and the residual metal is dissolved to form a protective and passivated hydrated oxide film.
The wafer after the SC2 treatment is cleaned by using QDR6 (the reagent is deionized water with the resistivity of 18M Ω · cm), the temperature is normal temperature, the treatment time is 5min, and the residual dirty liquid medicine and the complex metal on the surface of the wafer are mainly washed clean.
And finally, carrying out hot nitrogen spin-drying on the wet wafer, wherein the treatment mode is the filtered dry hot nitrogen, the temperature is 40 ℃, the rotating speed is 1000rpm, and the treatment time is 12 min.
The wafer surface before cleaning had 21680 particles/wafer, measured as in example 1, of > 0.18 μm; the wafers processed as above can control the particles > 0.18 micron to 36 particles/wafer than the conventional process, as shown in FIG. 2.
According to the above embodiments, the improved cleaning manner of the conventional wet chemical cleaning process in the present invention includes immersion type chemical cleaning and/or spray type single-tank chemical cleaning; the adopted cleaning agent is selected from one or more of sulfuric acid-hydrogen peroxide mixed liquor (SPM), ammonia water-hydrogen peroxide-water mixed liquor (SC1), hydrochloric acid-hydrogen peroxide-water mixed liquor (SC2) and hydrofluoric acid-water mixed liquor (DHF) or liquid medicines with different concentrations; the cleaning agent can oxidize, dissolve and complex to remove organic contamination, inorganic pollutants and metal ions on the Wafer surface.
Compared with the prior art, the wet cleaning process is designed on the basis of the cleaning principle, and is short in cleaning process and simple and convenient to operate; the invention combines the wafer wet cleaning principle, has the advantages of pertinently treating the pollutants on the surface of the wafer step by step and circularly, reducing the residual quantity of particles, dirt and metal ions and greatly improving the wafer quality.
While only the preferred embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A wafer cleaning method, comprising:
carrying out DIW cleaning, SPM cleaning, HQDR cleaning, QDR1 cleaning, QDR2 cleaning, high-concentration SC1 cleaning, QDR3 cleaning, DHF cleaning, QDR4 cleaning, low-concentration SC1 cleaning, QDR5 cleaning, SC2 cleaning and QDR6 cleaning on the wafer in sequence;
the reagent for cleaning the SPM comprises: h2SO4And H2O2；
The reagents for the high-concentration SC1 washing and the low-concentration SC1 washing comprise: NH (NH)4OH、H2O2And H2O；
The DHF cleaning reagent comprises: HF and H2O；
The SC2 cleaning reagent comprises: HCl, H2O2And H2O。
2. The method of claim 1, wherein the DIW cleaning time is 30-60 min; the flow rate is 0.5 to 1L/min.
3. The method as claimed in claim 1, wherein the temperature of the SPM cleaning is 90-140 ℃ and the time is 8-15 min.
4. The method according to claim 1, wherein the temperature of the high-concentration SC1 cleaning is 50-75 ℃ for 5-15 min.
5. The method according to claim 1, wherein the DHF wash time is 15s to 10 min; the temperature was room temperature.
6. The method according to claim 1, wherein the temperature of the low-concentration SC1 cleaning is 50-75 ℃ and the time is 5-15 min.
7. The method of claim 1, wherein the SC2 cleaning temperature is 70-80 ℃ and the time is 5-15 min.
8. The method of claim 1, wherein the QDR6 cleaning further comprises:
drying the cleaned wafer;
the drying temperature is 30-50 ℃.
9. The method as claimed in claim 1, wherein the reagent washed by SPM is H2SO4And H2O2The volume ratio of (2-5) to (1).
10. The method of claim 1, wherein the high concentration of NH in the SC1 washing reagent4OH、H2O2And H2The volume ratio of O is 1 (1-2) to 5-6;
NH in the reagent for cleaning the low-concentration SC14OH、H2O2And H2The volume ratio of O is (0.1-0.5): 1: 5.
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