CN117463691A - Cleaning method before annealing of sapphire wafer - Google Patents

Cleaning method before annealing of sapphire wafer Download PDF

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Publication number
CN117463691A
CN117463691A CN202311715352.0A CN202311715352A CN117463691A CN 117463691 A CN117463691 A CN 117463691A CN 202311715352 A CN202311715352 A CN 202311715352A CN 117463691 A CN117463691 A CN 117463691A
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Prior art keywords
cleaning
sapphire wafer
before annealing
ultrasonic cleaning
adopting
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请求不公布姓名
陈应红
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First Semiconductor Materials Co ltd
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First Semiconductor Materials Co ltd
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Priority to CN202311715352.0A priority Critical patent/CN117463691A/en
Publication of CN117463691A publication Critical patent/CN117463691A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/08Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/02Cleaning by the force of jets or sprays
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/10Cleaning 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
    • B08B3/12Cleaning 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cleaning Or Drying Semiconductors (AREA)

Abstract

The method for cleaning the sapphire wafer before annealing is at least suitable for cleaning the surface of the 8-inch sapphire wafer after grinding boron carbide and before annealing, and comprises the following steps: s1, ultrasonically cleaning by adopting an aqueous solution prepared from an alkaline metal cleaning agent; s2, ultrasonically cleaning by adopting deionized water; s3, placing the sapphire wafer in pure water for double-sided brushing, and keeping flushing in the brushing process; s4, ultrasonically cleaning by adopting an acid solution; s5, washing the sapphire wafer by adopting deionized water on two sides, and simultaneously rotating the sapphire wafer; s6, ultrasonically cleaning by adopting alkali solution; s7, washing the sapphire wafer by adopting deionized water on two sides, and simultaneously rotating the sapphire wafer; s8, ultrasonically cleaning by adopting deionized water; s9, washing the sapphire wafer by adopting deionized water on two sides, and simultaneously rotating the sapphire wafer; s10, placing the sapphire wafer in an automatic spin dryer for spin-drying.

Description

Cleaning method before annealing of sapphire wafer
Technical Field
The present disclosure relates to the field of semiconductor technology, and more particularly, to a method for cleaning a sapphire wafer before annealing.
Background
Sapphire, i.e. -Al 2 O 3 The monocrystal, commonly called corundum, has excellent optical performance, mechanical performance and chemical stability, high strength, high hardness and scouring resistance, and may be used widely in infrared military apparatus, high strength laser window material and semiconductor GaN/Al 2 O 3 Light Emitting Diodes (LEDs), large scale integrated circuits SOI and SOS, and superconducting nanostructured thin films, etc., are ideal substrate materials.
The processing procedure of the sapphire wafer generally comprises crystal bar processing, slicing, double-sided edging, chamfering, pre-annealing cleaning, annealing, pasting, single-sided grinding, polishing, cleaning and the like, but the surface defects of the wafer after annealing, such as surface dirt, white spots (also called white shift), water marks (also called chromatic aberration), bright spots and the like, are easily caused due to incomplete pre-annealing cleaning in the pre-annealing cleaning procedure.
The double-sided polishing is required to be performed on the surface of boron carbide during sapphire processing, and the sapphire substrate is considered to be high in hardness and difficult to process. However, after grinding the boron carbide, a large amount of grinding powder is difficult to remove on the surface of the sapphire, and the problems have long been the difficulty in the middle link of sapphire processing, especially the large area of an 8-inch sapphire wafer, so that the residual boron carbide powder is difficult to remove cleanly, and the yield of the annealed sapphire substrate is seriously affected. At present, the traditional cleaning mode of medicament, ultrasonic and hand washing is adopted in the industry, and the cleaning mode has a certain cleaning effect, but the overall effect is general, the stability is very poor, and the factors such as pollution exist locally.
Disclosure of Invention
In view of the problems in the background art, an object of the present disclosure is to provide a cleaning method before annealing a sapphire wafer, which can effectively remove residual boron carbide powder on the surface of the sapphire wafer caused in a processing process.
Another object of the present disclosure is to provide a cleaning method before annealing a sapphire wafer, which can effectively remove metal particles on the surface of the sapphire wafer after polishing, and impurities or residues such as a suspending agent, a dispersing agent, and the like in a boron carbide polishing liquid.
It is still another object of the present disclosure to provide a cleaning method before annealing a sapphire wafer, which can effectively remove surface defects such as dirt, chromatic aberration, oil stain, etc. on the surface of the polished sapphire wafer.
It is still another object of the present disclosure to provide a cleaning method before annealing a sapphire wafer, which can reduce the manual rubbing process.
Still another object of the present disclosure is to provide a cleaning method before annealing a sapphire wafer, which can achieve that at least a large-sized 8-inch sapphire wafer has no oil stain on the annealed surface, greatly reduce defects such as chromatic aberration, white spots, bright spots, and the like, and improve the yield after annealing at least a large-sized 8-inch sapphire wafer.
Thus, there is provided a method for cleaning a sapphire wafer before annealing, which is at least suitable for cleaning a surface of a sapphire wafer of 8 inches after grinding boron carbide and before annealing, the method for cleaning a sapphire wafer before annealing comprising the steps of: s1, ultrasonically cleaning by adopting an aqueous solution prepared from an alkaline metal cleaning agent; s2, ultrasonically cleaning by adopting deionized water; s3, placing the sapphire wafer in pure water for double-sided brushing, and keeping flushing in the brushing process; s4, ultrasonically cleaning by adopting an acid solution; s5, washing the sapphire wafer by adopting deionized water on two sides, and simultaneously rotating the sapphire wafer; s6, ultrasonically cleaning by adopting alkali solution; s7, washing the sapphire wafer by adopting deionized water on two sides, and simultaneously rotating the sapphire wafer; s8, ultrasonically cleaning by adopting deionized water; s9, washing the sapphire wafer by adopting deionized water on two sides, and simultaneously rotating the sapphire wafer; s10, placing the sapphire wafer in an automatic spin dryer for spin-drying.
The beneficial effects of the present disclosure are as follows.
The cleaning method before annealing the sapphire wafer can effectively remove residual boron carbide powder on the surface of the sapphire wafer caused in the processing procedure.
In addition, the cleaning method before annealing the sapphire wafer can effectively remove metal particles on the surface of the sapphire wafer after grinding, suspending agents in boron carbide grinding liquid, dispersing agents and other impurities or residues.
In addition, the cleaning method before annealing the sapphire wafer can effectively remove dirt, chromatic aberration, greasy dirt and other surface defects on the surface of the sapphire wafer caused in the processing procedure.
In addition, the cleaning method before annealing the sapphire wafer can reduce the manual scrubbing links.
The cleaning method before annealing of the sapphire wafer can achieve that the surface of the annealed 8-inch sapphire wafer with at least a large size is free of greasy dirt, defects such as chromatic aberration, white spots and bright spots are greatly reduced, and the yield of the annealed 8-inch sapphire wafer with at least a large size is improved.
Drawings
Fig. 1 is a flow chart of a method of cleaning a sapphire wafer prior to annealing according to the present disclosure.
Detailed Description
The drawings illustrate embodiments of the present disclosure, and it is to be understood that the disclosed embodiments are merely examples of the disclosure that may be embodied in various forms and that, therefore, specific details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously practice the disclosure.
[ cleaning method before annealing sapphire wafer ]
Referring to fig. 1, a cleaning method before annealing a sapphire wafer according to the present disclosure is at least suitable for cleaning after grinding and before annealing boron carbide on the surface of an 8-inch sapphire wafer, and includes the steps of:
s1, ultrasonically cleaning by adopting an aqueous solution prepared from an alkaline metal cleaning agent;
s2, ultrasonically cleaning by adopting deionized water;
s3, placing the sapphire wafer in pure water for double-sided brushing, and keeping flushing in the brushing process;
s4, ultrasonically cleaning by adopting an acid solution;
s5, washing the sapphire wafer by adopting deionized water on two sides, and simultaneously rotating the sapphire wafer;
s6, ultrasonically cleaning by adopting alkali solution;
s7, washing the sapphire wafer by adopting deionized water on two sides, and simultaneously rotating the sapphire wafer;
s8, ultrasonically cleaning by adopting deionized water;
s9, washing the sapphire wafer by adopting deionized water on two sides, and simultaneously rotating the sapphire wafer;
s10, placing the sapphire wafer in an automatic spin dryer for spin-drying.
In the cleaning method before annealing the sapphire wafer, the step S1 removes metal particles on the surface of the sapphire wafer, the step S2 soaks and loosens large-particle boron carbide embedded on the surface of the sapphire wafer to fall off, the step S3 brushes out and washes out small-particle boron carbide embedded on the surface of the sapphire wafer to deeply clean the surface of the sapphire wafer, the step S4 removes impurities or residues such as suspending agents, dispersing agents and the like in boron carbide grinding fluid from the surface of the sapphire wafer, the step S5 removes residual agents on the surface of the sapphire wafer, the step S6 neutralizes the residual agents on the surface of the sapphire wafer, the step S7 removes the residual agents after neutralization on the surface of the sapphire wafer, the step S9 removes the residues on the surface of the sapphire wafer by deep cleaning the embedded residues on the surface of the sapphire wafer through the step S8, and the step S10 enables the surface of the sapphire wafer to be sufficiently dried.
The cleaning method before annealing the sapphire wafer can effectively remove residual boron carbide powder on the surface of the sapphire wafer caused in the processing procedure.
In addition, the cleaning method before annealing the sapphire wafer can effectively remove metal particles on the surface of the sapphire wafer after grinding, suspending agents in boron carbide grinding liquid, dispersing agents and other impurities or residues.
In addition, the cleaning method before annealing the sapphire wafer can effectively remove dirt, chromatic aberration, greasy dirt and other surface defects on the surface of the sapphire wafer caused in the processing procedure.
In addition, the cleaning method before annealing the sapphire wafer can reduce the manual scrubbing links.
The cleaning method before annealing of the sapphire wafer can achieve that the surface of the annealed 8-inch sapphire wafer with at least a large size is free of greasy dirt, defects such as chromatic aberration, white spots and bright spots are greatly reduced, and the yield of the annealed 8-inch sapphire wafer with at least a large size is improved.
Of course, for small-sized less than 8 inch sapphire wafer pre-anneal cleaning, the pre-anneal cleaning method of the present disclosure is equally applicable.
Specifically, in one example, in step S1, the mass fraction of the alkali metal cleaner in the aqueous solution prepared from the alkali metal cleaner is 5 to 10%; the model of the alkali metal cleaning agent is Inboard CL801. In one example, in step S1, the intensity of the ultrasonic cleaning is 20-30Hz; the temperature of ultrasonic cleaning is 60-80 ℃; the ultrasonic cleaning time is 15-30min.
Specifically, in one example, in step S2, the intensity of the ultrasonic cleaning is 25-35Hz; the temperature of ultrasonic cleaning is 50-70 ℃; the ultrasonic cleaning time is 10-20min.
Specifically, in one example, in step S3, the double-sided brush is applied for 10-30 seconds; the brushing adopts a nylon roller brush.
Specifically, in one example, in step S4, an acid solution is formulated from hydrofluoric acid and water in a volume ratio of 1 (10-20). In one example, in step S4, the intensity of the ultrasonic cleaning is 15-20Hz; the temperature of ultrasonic cleaning is 50-70 ℃; the ultrasonic cleaning time is 15-30s.
Specifically, in one example, in step S5, the time for flushing is 80-90S; the flow rate of the flushing was 2000ml/min.
Specifically, in an example, in step S6, the alkaline solution is prepared from hydrogen peroxide, ammonia water and pure water in a volume ratio of 2:1:1. The strong oxidizing property of the hydrogen peroxide can effectively remove particles and organic matters on the surface of the sapphire wafer, and the wafer surface with high cleanliness is obtained; ammonia water has a dissolving effect on substances on the surface of the wafer; the organic contamination is changed into water-soluble compounds through the strong oxidation of hydrogen peroxide and the dissolution of ammonia water, and the organic contamination can be removed through the deionized water washing in the step S7. In one example, in step S6, the intensity of the ultrasonic cleaning is 25-35Hz; the temperature of ultrasonic cleaning is 75-80 ℃; the ultrasonic cleaning time is 5-10min.
Specifically, in one example, in step S7, the time of flushing is 80-90S; the flow rate of the flushing was 2000ml/min.
Specifically, in one example, in step S8, the intensity of the ultrasonic cleaning is 20-30Hz; the temperature of ultrasonic cleaning is 25-45 ℃; the ultrasonic cleaning time is 15-30min.
Specifically, in one example, in step S9, the time of flushing is 80-90S; the flow rate of the flushing was 2000ml/min.
Specifically, in an example, in step S10, the spin speed of the automatic spin dryer is 4000-5000rpm.
In one example, in step S5, step S7 and step S9, the rotation of the sapphire wafer is performed using a mechanical rotation.
[ test ]
Example 1
Example 1 the following steps were taken for the pre-anneal cleaning of an 8 inch sapphire wafer:
s1, performing ultrasonic cleaning by adopting an aqueous solution prepared from an alkaline metal cleaning agent, wherein the model of the alkaline metal cleaning agent is Insal CL801, the mass fraction of the alkaline metal cleaning agent in the aqueous solution prepared from the alkaline metal cleaning agent is 5%, the ultrasonic cleaning strength is 20Hz, the ultrasonic cleaning temperature is 80 ℃, and the ultrasonic cleaning time is 15min;
s2, ultrasonically cleaning by deionized water, wherein the ultrasonic cleaning strength is 25Hz, the ultrasonic cleaning temperature is 70 ℃, and the ultrasonic cleaning time is 20min;
s3, placing the sapphire wafer in pure water for double-sided brushing, and keeping flushing water in the brushing process, wherein a nylon roller brush is adopted for brushing for 10 seconds;
s4, ultrasonically cleaning by adopting an acid solution, wherein the acid solution is prepared from hydrofluoric acid and water in a volume ratio of 1:10, and the ultrasonic cleaning strength is 20Hz; the temperature of ultrasonic cleaning is 70 ℃; the ultrasonic cleaning time is 15s;
s5, washing the sapphire wafer by adopting deionized water on two sides, rotating the sapphire wafer at the same time, wherein the washing time is 80S, the washing flow rate is 2000ml/min, and the rotation is mechanical rotation;
s6, ultrasonic cleaning is carried out by adopting an alkali solution, wherein the alkali solution is prepared by hydrogen peroxide, ammonia water and pure water in a volume ratio of 2:1:1, the ultrasonic cleaning strength is 25Hz, the ultrasonic cleaning temperature is 80 ℃, and the ultrasonic cleaning time is 5min;
s7, washing the sapphire wafer by adopting deionized water on two sides, rotating the sapphire wafer at the same time, wherein the washing time is 90S, the washing flow rate is 2000ml/min, and the rotation is mechanical rotation;
s8, ultrasonic cleaning is carried out by adopting deionized water, the ultrasonic cleaning strength is 20Hz, the ultrasonic cleaning temperature is 25 ℃, and the ultrasonic cleaning time is 30min;
s9, washing the sapphire wafer by adopting deionized water on two sides, rotating the sapphire wafer at the same time, wherein the washing time is 90S, the washing flow rate is 2000ml/min, and the rotation is mechanical rotation;
s10, placing the sapphire wafer into an automatic spin dryer for spin-drying, wherein the rotating speed of the automatic spin dryer is 5000rpm.
After the completion of the cleaning before annealing in example 1, 50 pieces of 8-inch sapphire wafers of the same lot were annealed, and visual inspection was performed after annealing, and the test results are shown in table 1.
Table 1 based on the detection results after annealing of the sapphire wafer after the cleaning before annealing of example 1 was completed
Example 2
Example 2 the following steps were taken for the pre-anneal cleaning of an 8 inch sapphire wafer:
s1, performing ultrasonic cleaning by adopting an aqueous solution prepared from an alkaline metal cleaning agent, wherein the model of the alkaline metal cleaning agent is Insal CL801, the mass fraction of the alkaline metal cleaning agent in the aqueous solution prepared from the alkaline metal cleaning agent is 10%, the ultrasonic cleaning strength is 30Hz, the ultrasonic cleaning temperature is 60 ℃, and the ultrasonic cleaning time is 30min;
s2, ultrasonically cleaning by deionized water, wherein the ultrasonic cleaning strength is 35Hz, the ultrasonic cleaning temperature is 50 ℃, and the ultrasonic cleaning time is 10min;
s3, placing the sapphire wafer in pure water for double-sided brushing, and keeping flushing water in the brushing process, wherein a nylon roller brush is adopted for brushing for double-sided brushing for 30 seconds;
s4, ultrasonically cleaning by adopting an acid solution, wherein the acid solution is prepared from hydrofluoric acid and water in a volume ratio of 1:20, and the ultrasonic cleaning strength is 15Hz; the temperature of ultrasonic cleaning is 50 ℃, and the time of ultrasonic cleaning is 30s;
s5, washing the sapphire wafer by adopting deionized water on two sides, rotating the sapphire wafer at the same time, wherein the washing time is 90S, the washing flow rate is 2000ml/min, and the rotation is mechanical rotation;
s6, ultrasonic cleaning is carried out by adopting an alkali solution, wherein the alkali solution is prepared by hydrogen peroxide, ammonia water and pure water in a volume ratio of 2:1:1, the ultrasonic cleaning strength is 35Hz, the ultrasonic cleaning temperature is 75 ℃, and the ultrasonic cleaning time is 10min;
s7, washing the sapphire wafer by adopting deionized water on two sides, rotating the sapphire wafer at the same time, wherein the washing time is 80S, the washing flow rate is 2000ml/min, and the rotation is mechanical rotation;
s8, ultrasonic cleaning is carried out by adopting deionized water, the ultrasonic cleaning strength is 30Hz, the ultrasonic cleaning temperature is 45 ℃, and the ultrasonic cleaning time is 15min;
s9, washing the sapphire wafer by adopting deionized water on two sides, rotating the sapphire wafer at the same time, wherein the washing time is 80S, the washing flow rate is 2000ml/min, and the rotation is mechanical rotation;
s10, placing the sapphire wafer into an automatic spin dryer for spin-drying, wherein the rotating speed of the automatic spin dryer is 4000rpm.
After the completion of the cleaning before annealing in example 2, 50 pieces of 8-inch sapphire wafers of the same lot were annealed, and visual inspection was performed after annealing, and the test results are shown in table 2.
Table 2 based on the detection results after annealing the sapphire wafer after the cleaning before annealing in example 2
The various exemplary embodiments are described using the above detailed description, but are not intended to be limited to the combinations explicitly disclosed herein. Thus, unless otherwise indicated, the various features disclosed herein may be combined together to form a number of additional combinations that are not shown for the sake of brevity.

Claims (10)

1. A cleaning method before annealing of sapphire wafers is characterized in that,
the cleaning method before annealing the sapphire wafer is at least suitable for cleaning the surface of the 8-inch sapphire wafer after grinding boron carbide and before annealing,
the cleaning method before annealing the sapphire wafer comprises the following steps:
s1, ultrasonically cleaning by adopting an aqueous solution prepared from an alkaline metal cleaning agent;
s2, ultrasonically cleaning by adopting deionized water;
s3, placing the sapphire wafer in pure water for double-sided brushing, and keeping flushing in the brushing process;
s4, ultrasonically cleaning by adopting an acid solution;
s5, washing the sapphire wafer by adopting deionized water on two sides, and simultaneously rotating the sapphire wafer;
s6, ultrasonically cleaning by adopting alkali solution;
s7, washing the sapphire wafer by adopting deionized water on two sides, and simultaneously rotating the sapphire wafer;
s8, ultrasonically cleaning by adopting deionized water;
s9, washing the sapphire wafer by adopting deionized water on two sides, and simultaneously rotating the sapphire wafer;
s10, placing the sapphire wafer in an automatic spin dryer for spin-drying.
2. The method for cleaning a sapphire wafer before annealing according to claim 1,
in the step S1 of the process,
the mass fraction of the alkali metal cleaning agent in the aqueous solution prepared by the alkali metal cleaning agent is 5-10%; the model of the alkali metal cleaning agent is Inboard CL801.
3. The method for cleaning a sapphire wafer before annealing according to claim 1,
in the step S1, the intensity of ultrasonic cleaning is 20-30Hz, the temperature of ultrasonic cleaning is 60-80 ℃, and the time of ultrasonic cleaning is 15-30min; and/or
In the step S2, the intensity of ultrasonic cleaning is 25-35Hz, the temperature of ultrasonic cleaning is 50-70 ℃, and the time of ultrasonic cleaning is 10-20min; and/or
In the step S3, the double-sided brushing is performed for 10-30S, and a nylon roller brush is adopted for brushing.
4. The method for cleaning a sapphire wafer before annealing according to claim 1,
in the step S4 of the process of the present invention,
the acid solution is prepared from hydrofluoric acid and water in a volume ratio of 1 (10-20).
5. The method for cleaning a sapphire wafer before annealing according to claim 1,
in the step S4, the intensity of ultrasonic cleaning is 15-20Hz, the temperature of ultrasonic cleaning is 50-70 ℃, and the time of ultrasonic cleaning is 15-30S; and/or
In step S5, the rinsing time is 80-90S, and the flow rate of rinsing is 2000ml/min.
6. The method for cleaning a sapphire wafer before annealing according to claim 1,
in the step S6 of the process of the present invention,
the alkali solution is prepared from hydrogen peroxide, ammonia water and pure water in a volume ratio of 2:1:1.
7. The method for cleaning a sapphire wafer before annealing according to claim 1,
in the step S6 of the process of the present invention,
the intensity of ultrasonic cleaning is 25-35Hz;
the temperature of ultrasonic cleaning is 75-80 ℃;
the ultrasonic cleaning time is 5-10min.
8. The method for cleaning a sapphire wafer before annealing according to claim 1,
in the step S7 of the process of the present invention,
the flushing time is 80-90s;
the flow rate of the flushing was 2000ml/min.
9. The method for cleaning a sapphire wafer before annealing according to claim 1,
in the step S8 of the process of the present invention,
the intensity of ultrasonic cleaning is 20-30Hz;
the temperature of ultrasonic cleaning is 25-45 ℃;
the ultrasonic cleaning time is 15-30min.
10. The method for cleaning a sapphire wafer before annealing according to claim 1,
in the step S9, the flushing time is 80-90S, and the flushing flow rate is 2000ml/min; and/or
In step S10, the spin speed of the automatic spin dryer is 4000-5000rpm.
CN202311715352.0A 2023-12-13 2023-12-13 Cleaning method before annealing of sapphire wafer Pending CN117463691A (en)

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Application Number Priority Date Filing Date Title
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Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311715352.0A CN117463691A (en) 2023-12-13 2023-12-13 Cleaning method before annealing of sapphire wafer

Publications (1)

Publication Number Publication Date
CN117463691A true CN117463691A (en) 2024-01-30

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Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

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