CN114558822A - Cleaning method of injection pipe - Google Patents

Cleaning method of injection pipe Download PDF

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Publication number
CN114558822A
CN114558822A CN202111538348.2A CN202111538348A CN114558822A CN 114558822 A CN114558822 A CN 114558822A CN 202111538348 A CN202111538348 A CN 202111538348A CN 114558822 A CN114558822 A CN 114558822A
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cleaning
product
pipe
injection pipe
pure water
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CN114558822B (en
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叶天爱
余正飞
李长苏
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Hangzhou Dunyuan Poly Core Semiconductor Technology Co ltd
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Hangzhou Dunyuan Poly Core Semiconductor Technology Co ltd
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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
    • B08B3/02Cleaning by the force of jets or sprays
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B13/00Accessories or details of general applicability for machines or apparatus for cleaning
    • 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
    • B08B3/04Cleaning 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26DRYING
    • F26BDRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B21/00Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
    • F26B21/001Drying-air generating units, e.g. movable, independent of drying enclosure

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cleaning By Liquid Or Steam (AREA)

Abstract

The invention discloses a cleaning method of an injection pipe, aiming at solving the defect of poor cleaning effect of the injection pipe. In the cleaning process of the jet pipe, S2 is cleaned by ultrasonic wave, and the pollution of particles with the size of more than 2um caused by other processes can be removed. S3, performing stress etching, effectively and quickly removing stains by using a KOH solution, having small corrosion tendency to the injection pipe, and generating larger impact force in the process to quickly peel off the stains, thereby improving the cleaning effect of the injection pipe. The rapid spraying and sweeping treatment is carried out on the whole surface of the spraying pipe in the S5 sand blasting process, the corrosion of the potassium hydroxide solution on the surface of the product can be removed, but no residual film can be completely removed, and the step does not have great influence on the surface roughness of the spraying pipe. The SC2 cleaning method used in S7 can effectively remove the metal elements related to Na, Mg, Fe, and the like on the surface of the spray pipe. The cleaning effect is good in the cleaning process of the jet pipe, and the ideal cleaning requirement can be met.

Description

Cleaning method of injection pipe
Technical Field
The invention relates to the field of semiconductor manufacturing, in particular to a cleaning method of an injection pipe.
Background
Semiconductor silicon material is an indispensable core material device in the manufacture of integrated circuit chips. Due to the rapid development of the integrated circuit industry in China, the requirements of related semiconductor devices and key parts are also increasing. At present, the main substrate material of integrated circuits at home and abroad is a silicon wafer, the line width of the silicon wafer is continuously reduced, higher and higher requirements are put on the processing of silicon parts, and the surface of a product cannot have microscopic processing defects such as a broken layer, microcracks and the like. Meanwhile, the product also needs to meet higher cleanliness, and the surface of the product cannot contain impurities such as organic pollution, particles, metal and the like. The injection pipe is used as a key part for introducing the process gas into the process cavity, and if the cleanliness of the injection pipe is not up to the standard, small particles attached to the injection pipe can be mixed with the reaction gas, so that serious pollution can be caused to the production and manufacturing process, and economic loss is caused.
The current injection pipe is made of silicon materials, so the acid resistance and alkali resistance of the injection pipe are strong, high-concentration acid and alkali can be utilized to remove dirt and tool marks flowing down in the machining process, in the cleaning process of the silicon injection pipe, the traditional cleaning operation method often cannot meet ideal requirements, the injection pipe is easy to damage and cannot be used due to the brittleness of the silicon materials, in addition, the dirt and an oxide layer attached to the surface of the injection pipe cannot be effectively removed, and therefore the cleaning process of the injection pipe needs to be researched urgently.
Disclosure of Invention
In order to overcome the defects, the invention provides the cleaning method of the injection pipe, the cleaning effect is good in the cleaning process of the injection pipe, and the ideal cleaning requirement can be met.
In order to solve the technical problems, the invention adopts the following technical scheme: a method of cleaning a spray tube comprising the steps of:
s1, pre-check: detecting the appearance and the size of the injection pipe product to be cleaned, and photographing and observing;
s2, ultrasonic cleaning: placing the jet pipe in an ultrasonic cleaning machine for ultrasonic cleaning, removing stains on the surface of a product, taking out the product from the ultrasonic cleaning machine, flushing with pure water, and drying by blowing;
s3, stress etching: corroding an oxide layer on the surface of the jet pipe by using KOH, then showering by using pure water, and then blowing to dry;
s4, surface preparation: the injection pipe is put into an ultrasonic cleaning machine again for hot water washing, and is taken out of the ultrasonic cleaning machine for pure water showering to remove alkali liquor remaining on the surface of the product and then is blown dry;
s5, sand blasting: placing the jet pipe into a sand blasting machine, and performing sand blasting treatment to remove residues on the surface of a product and knife lines left by machining;
s6, surface measurement: visually observing the product, observing whether the surface of the product has obvious knife lines, and then detecting the roughness of the surface of the product by using a roughness detector;
s7, final washing: putting the jet pipe into a cleaning machine, sequentially passing through an SC2 tank and a DIW tank on the cleaning machine to remove metal ions on the surface of a product, then flushing with pure water, and then drying by blowing;
s8, wet thermal oxidation: wiping the product with pure water and a clean cloth, and carrying out damp-heat oxidation;
s9, appearance detection: and observing the color change of the surface of the product, and comparing the color with the picture of the product obtained in the step S1 to judge the thickness of the oxide layer on the surface of the injection pipe.
In the cleaning process of the injection pipe, S2 is subjected to ultrasonic cleaning, so that the pollution of particles of more than 2um caused by other processes can be removed. S3, performing stress etching, effectively and quickly removing stains by using a KOH solution, having small corrosion tendency to the injection pipe, and generating larger impact force in the process to quickly peel off the stains, thereby improving the cleaning effect of the injection pipe. The rapid spraying and sweeping treatment is carried out on the whole surface of the spraying pipe in the S5 sand blasting process, the corrosion of the potassium hydroxide solution on the surface of the product can be removed, but no residual film can be completely removed, and the step does not have great influence on the surface roughness of the spraying pipe. The SC2 cleaning method used in S7 can effectively remove the metal elements related to Na, Mg, Fe, and the like on the surface of the ejector tube. The cleaning effect is good in the cleaning process of the jet pipe, and the ideal cleaning requirement can be met.
Preferably, in the S3 process, a comparison sample with the same material as the jet pipe is firstly put into KOH corrosive liquid for etching, and the etching time and the reduced thickness are calculated and recorded; the time required for the ejector tube to be etched is determined with reference to the etch time and reduced thickness of the control sample.
The etching is carried out through the comparison sample which is made of the same material as the jet pipe, the etching time and the reduced thickness are calculated, data are obtained and used as data reference of the jet pipe etching process, and the etching time of the jet pipe is conveniently and accurately controlled.
Preferably, pure water is poured into a reaction tank during S3, KOH solution is added, and the reaction tank is stirred while the temperature is controlled at 50 ℃, a jet pipe product is placed, and nitrogen gas is bubbled into the reaction tank. And nitrogen bubbles are filled in the reaction tank filled with the KOH solution, so that the etching effect is improved.
Preferably, in S4, the temperature of the ultrasonic cleaning is controlled at 50-80 ℃, the cleaning time is 10-20 minutes, and deionized water is added during the cleaning process to keep the ultrasonic cleaning machine in an overflow state.
Preferably, in S7, a cleaning solution is prepared in SC2, and the volume ratio of each component is H2O:HCl:H2O25: 1: 1, the mass concentration of hydrochloric acid is 49 percent, the mass concentration of hydrogen peroxide is 70 percent, the solution preparation is finished, the temperature of the cleaning solution is controlled to be about 50 ℃, then the product is put into an SC2 tank, soaked for more than 30 minutes, and nitrogen is bubbled into an SC2 tank.
The SC2 cleaning solution provides a low PH environment in which alkaline metal ions, metal hydrides will dissolve in the SC2 cleaning solution.
Preferably, in S7, after washing in the SC2 tank, the product is quickly placed in a DIW tank and soaked for 30 minutes or more, and after soaking, the product is showered with pure water and then dried by blowing.
Preferably, when the wet heat oxidation is performed in S8, the product is put into a vertical oxidation furnace, and wet heat oxidation is performed in the oxidation furnace using water as an oxidizing agent under high temperature and high pressure conditions.
Under the conditions of high temperature and high pressure, the surface of the injection pipe is subjected to wet heat oxidation, and Si(s) +2H2O(g)——SiO2(S)+H2(g)。
Preferably, the products of S2, S3, S4 and S7 are blown dry by nitrogen. The nitrogen has stable performance and is not easy to react.
Preferably, after S5 is finished, the product is placed in an ultrasonic cleaner for soaking and cleaning, the temperature is controlled to be near 50 ℃ for more than 5 minutes, and then the product is dried.
Preferably, in S2, the ultrasonic cleaning frequency is 40kHz, the ultrasonic medium is pure water with resistivity more than 15M, and the temperature is controlled between 50-70 ℃ and the time is controlled at 20 +/-2 minutes.
Compared with the prior art, the invention has the beneficial effects that: (1) the cleaning effect is good in the cleaning process of the jet pipe, and the ideal cleaning requirement can be met; (2) s2, ultrasonic cleaning is carried out, so that particle pollution of more than 2um caused by other processes can be removed; (3) s3, performing stress etching, effectively and quickly removing stains by using a KOH solution, having small corrosion tendency to the injection pipe, and generating larger impact force in the process to quickly peel off the stains, thereby improving the cleaning effect of the injection pipe; (4) the full surface of the injection pipe is subjected to rapid spraying and sweeping treatment in the S5 sand blasting process, so that the corrosion of the potassium hydroxide solution on the surface of a product can be removed, but no residual film can be completely removed, and the step does not cause great influence on the surface roughness of the injection pipe; (5) the SC2 cleaning method used in S7 can effectively remove the metal elements related to Na, Mg, Fe, and the like on the surface of the ejector tube.
Detailed Description
The technical scheme of the invention is further described in detail by the following specific examples:
the embodiment is as follows: a method of cleaning a spray tube comprising the steps of:
s1, pre-check: detecting the appearance and the size of the injection pipe product to be cleaned, and photographing and observing; checking whether the appearance of the product has obvious cracks and gaps, then measuring and recording the size of the injection pipe by using a three-dimensional measuring instrument, and photographing at a bright environment to leave a bottom;
s2, ultrasonic cleaning: placing the jet pipe in an ultrasonic cleaning machine for ultrasonic cleaning, removing stains on the surface of a product, taking out the product from the ultrasonic cleaning machine, flushing with pure water, and drying by blowing; in S2, the frequency of ultrasonic cleaning is 40kHz, the ultrasonic medium is pure water with the resistivity larger than 15M, the temperature is controlled between 50 ℃ and 70 ℃, and the time is controlled within 20 +/-2 minutes;
s3, stress etching: corroding an oxide layer on the surface of the jet pipe by using KOH, then showering by using pure water, and then blowing to dry; preparing an etching solution in the S3 process, pouring pure water into a reaction tank, adding a KOH solution, stirring to form the etching solution, controlling the temperature of the reaction tank at 50 ℃, putting a jet pipe product, and bubbling nitrogen into the reaction tank; in the S3 process, firstly, a comparison sample with the same material as the jet pipe is put into KOH corrosive liquid for etching, and the etching time and the reduced thickness are calculated and recorded; typically, the etch rate was controlled to around 10um and the etch time was recorded. Determining the time required for etching the ejector tube by referring to the etching time and the reduced thickness of the comparison sample;
s4, surface preparation: the injection pipe is put into a horizontal ultrasonic cleaning machine again for hot water washing, and is taken out of the ultrasonic cleaning machine for pure water showering to remove alkali liquor remaining on the surface of the product and then is dried by blowing; s4, controlling the temperature of ultrasonic cleaning at 50-80 ℃, cleaning for 10-20 minutes, and adding deionized water in the cleaning process to keep the ultrasonic cleaning machine in an overflow state;
s5, sand blasting: placing the injection pipe into a sand blasting machine for sand blasting treatment, uniformly and stably spraying 800-mesh sand on the surface of a product, and removing residues on the surface of the product and knife lines left by machining; the pressure before the sand blasting machine is started should be between 0.2 and 0.4Mpa, and the pressure in the sand blasting process is slightly reduced, so that a pressure gauge needs to be paid attention to constantly to prevent overlarge fluctuation, and the sand blasting is not uniform; s5, after the completion, placing the product in an ultrasonic cleaner for soaking and cleaning, controlling the temperature to be near 50 ℃ and the time to be more than 5 minutes, and then drying the product;
s6, surface measurement: visually observing the product, observing whether the surface of the product has obvious knife lines or uneven chromatic aberration, and if the surface of the product has no obvious appearance problem, detecting whether the roughness of the surface of the product reaches a satisfactory value by using a roughness detector; then the obtained product is sent into a three-dimensional coordinate instrument to check the size of the injection pipe;
s7, final washing: putting the jet pipe into a cleaning machine, sequentially passing through an SC2 tank and a DIW tank on the cleaning machine to remove metal ions on the surface of a product, then flushing with pure water, and then drying by blowing;s7, preparing a cleaning solution in SC2, wherein the volume ratio of each component is H2O:HCl:H2O25: 1: 1, the mass concentration of hydrochloric acid is 49 percent, the mass concentration of hydrogen peroxide is 70 percent, the solution preparation is finished, the temperature of the cleaning solution is controlled to be about 50 ℃, then the product is put into an SC2 tank, soaked for more than 30 minutes, and nitrogen is bubbled into an SC2 tank. And S7, after the cleaning in the SC2 tank is finished, quickly putting the product into a DIW tank, soaking for more than 30 minutes, after the soaking is finished, spraying with pure water, and then drying by blowing.
S8, wet thermal oxidation: wiping the product with pure water and a clean cloth, and carrying out damp-heat oxidation; s8, when carrying out damp-heat oxidation, putting the product into a vertical oxidation furnace, and carrying out damp-heat oxidation by using gaseous water as an oxidant under the conditions of high temperature and high pressure in the oxidation furnace; the temperature in the oxidation furnace is 120-320 ℃, and the pressure is 0.5-20 MPa;
s9, appearance detection: and removing the product to observe the color change of the surface of the product, and comparing the color with the picture of the product in the step S1 to judge the thickness of the oxide layer on the surface of the injection pipe. And S2, S3, S4 and S7 adopt nitrogen to blow the product dry.
Different colors can be seen along with the change of the thickness of the oxide layer on the surface of the product, and the different colors can quickly judge whether the unevenness occurs. By adopting a colorimetric method, the phenomenon that oxide films with different thicknesses can present interference colors with different colors under white vertical irradiation is utilized, a metallographic microscope is used for observing and contrasting a standard colorimetric sample, and the thickness of the oxide layer is directly obtained from the contrast of the colors. The corresponding relationship is shown in the following table.
Figure BDA0003413220450000051
In the cleaning process of the spray pipe, the ultrasonic cleaning is performed in S2, so that the particle pollution of more than 2um caused by other processes can be removed. S3, performing stress etching, effectively and quickly removing stains by using a KOH solution, having small corrosion tendency to the injection pipe, and generating larger impact force in the process to quickly peel off the stains, thereby improving the cleaning effect of the injection pipe. The rapid spraying and sweeping treatment is carried out on the whole surface of the spraying pipe in the S5 sand blasting process, the corrosion of the potassium hydroxide solution on the surface of the product can be removed, but no residual film can be completely removed, and the step does not have great influence on the surface roughness of the spraying pipe. The SC2 cleaning method used in S7 can effectively remove the metal elements related to Na, Mg, Fe, and the like on the surface of the spray pipe. The cleaning effect is good in the cleaning process of the jet pipe, and the ideal cleaning requirement can be met.
The above-described embodiments are merely preferred embodiments of the present invention, which is not intended to be limiting in any way, and other variations and modifications are possible without departing from the scope of the invention as set forth in the appended claims.

Claims (10)

1. A cleaning method of an injection pipe is characterized by comprising the following steps:
s1, pre-check: detecting the appearance and the size of the injection pipe product to be cleaned, and photographing and observing;
s2, ultrasonic cleaning: placing the jet pipe in an ultrasonic cleaning machine for ultrasonic cleaning, removing stains on the surface of a product, taking out the product from the ultrasonic cleaning machine, flushing with pure water, and drying by blowing;
s3, stress etching: corroding an oxide layer on the surface of the jet pipe by using KOH, then showering by using pure water, and then blowing to dry;
s4, surface preparation: the injection pipe is put into an ultrasonic cleaning machine again for hot water washing, and is taken out of the ultrasonic cleaning machine for pure water showering to remove alkali liquor remaining on the surface of the product and then is blown dry;
s5, sand blasting: placing the jet pipe into a sand blasting machine, and performing sand blasting treatment to remove residues on the surface of a product and knife lines left by machining;
s6, surface measurement: visually observing the product, observing whether the surface of the product has obvious knife lines, and then detecting the roughness of the surface of the product by using a roughness detector;
s7, final washing: putting the jet pipe into a cleaning machine, sequentially passing through an SC2 tank and a DIW tank on the cleaning machine to remove metal ions on the surface of a product, then flushing with pure water, and then drying by blowing;
s8, wet thermal oxidation: wiping the product with pure water and a clean cloth, and carrying out damp-heat oxidation;
s9, appearance detection: and observing the color change of the surface of the product, and comparing the color with the picture of the product obtained in the step S1 to judge the thickness of the oxide layer on the surface of the injection pipe.
2. The method for cleaning the injection pipe as claimed in claim 1, wherein in the step of S3, a reference sample made of the same material as the injection pipe is first etched in KOH etchant, and the etching time and the reduced thickness are calculated and recorded; the time required for the ejector tube to be etched is determined with reference to the etch time and reduced thickness of the control sample.
3. The method for cleaning a spray pipe of claim 1, wherein pure water is poured into the reaction tank during the step of S3, KOH solution is added thereto and stirred, the temperature of the reaction tank is controlled at 50 ℃, the spray pipe product is put into the reaction tank, and nitrogen gas is bubbled into the reaction tank.
4. The method as claimed in claim 1, wherein the ultrasonic cleaning temperature is controlled to 50-80 ℃ for 10-20 minutes in S4, and deionized water is added during the cleaning process to keep the ultrasonic cleaning machine in an overflow state.
5. The method for cleaning an injection nozzle as claimed in claim 1, wherein in S7, a cleaning solution is prepared in SC2, and the volume ratio of each component is H2O:HCl:H2O25: 1: 1, the mass concentration of hydrochloric acid is 49 percent, the mass concentration of hydrogen peroxide is 70 percent, the solution preparation is finished, the temperature of the cleaning solution is controlled to be about 50 ℃, then the product is put into an SC2 tank, soaked for more than 30 minutes, and nitrogen is bubbled into an SC2 tank.
6. The method of claim 1, wherein the cleaning in the SC2 tank is finished in S7, the product is quickly put into a DIW tank for soaking for more than 30 minutes, and after the soaking is finished, the product is showered by pure water and then dried by blowing.
7. The method of claim 1, wherein the wet heat oxidation of the spray pipe is performed at S8, and the wet heat oxidation is performed in a vertical oxidation furnace using water as an oxidant under high temperature and high pressure conditions in the oxidation furnace.
8. The method of cleaning an injection tube as set forth in any one of claims 1 to 7, wherein the products of S2, S3, S4, S7 are dried by nitrogen gas.
9. The method for cleaning a spray pipe of any one of claims 1 to 7, wherein the product is subjected to immersion cleaning in an ultrasonic cleaner at a temperature of about 50 ℃ for more than 5 minutes after completion of S5, and then is dried.
10. The method of cleaning a spray pipe according to any one of claims 1 to 7, wherein in S2, the frequency of ultrasonic cleaning is 40kHz, the ultrasonic medium is pure water having a resistivity of more than 15M, and the temperature is controlled to be between 50 and 70 ℃ for 20 ± 2 minutes.
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140352771A1 (en) * 2013-05-28 2014-12-04 National Central University Method for manufacturing bowl-shaped surface structures of single-crystalline silicon substrates and a single-crystalline silicon substrate with bowl-shaped surface structures
CN105750275A (en) * 2014-12-18 2016-07-13 宁夏隆基硅材料有限公司 Silicon material cleaning method
CN107195728A (en) * 2017-06-23 2017-09-22 江阴鑫辉太阳能有限公司 A kind of solar cell is done over again the processing method of piece
CN108746855A (en) * 2018-06-11 2018-11-06 杭州和源精密工具有限公司 A kind of coating saw blade process of surface treatment
CN109112464A (en) * 2018-09-20 2019-01-01 安徽富乐德科技发展有限公司 A kind of molten preparation method for penetrating layer of semiconductor cleaning chamber ceramics
CN109731859A (en) * 2019-01-11 2019-05-10 湖州胜纯管道有限公司 A kind of stainless steel pipe cleaning method
CN110571134A (en) * 2019-08-06 2019-12-13 成都拓维高科光电科技有限公司 Cleaning process for molybdenum and oxides thereof on baffle

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140352771A1 (en) * 2013-05-28 2014-12-04 National Central University Method for manufacturing bowl-shaped surface structures of single-crystalline silicon substrates and a single-crystalline silicon substrate with bowl-shaped surface structures
CN105750275A (en) * 2014-12-18 2016-07-13 宁夏隆基硅材料有限公司 Silicon material cleaning method
CN107195728A (en) * 2017-06-23 2017-09-22 江阴鑫辉太阳能有限公司 A kind of solar cell is done over again the processing method of piece
CN108746855A (en) * 2018-06-11 2018-11-06 杭州和源精密工具有限公司 A kind of coating saw blade process of surface treatment
CN109112464A (en) * 2018-09-20 2019-01-01 安徽富乐德科技发展有限公司 A kind of molten preparation method for penetrating layer of semiconductor cleaning chamber ceramics
CN109731859A (en) * 2019-01-11 2019-05-10 湖州胜纯管道有限公司 A kind of stainless steel pipe cleaning method
CN110571134A (en) * 2019-08-06 2019-12-13 成都拓维高科光电科技有限公司 Cleaning process for molybdenum and oxides thereof on baffle

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