CN114558822B - Cleaning method of injection pipe - Google Patents
Cleaning method of injection pipe Download PDFInfo
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- CN114558822B CN114558822B CN202111538348.2A CN202111538348A CN114558822B CN 114558822 B CN114558822 B CN 114558822B CN 202111538348 A CN202111538348 A CN 202111538348A CN 114558822 B CN114558822 B CN 114558822B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/02—Cleaning by the force of jets or sprays
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B13/00—Accessories or details of general applicability for machines or apparatus for cleaning
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/001—Drying-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 spray pipe, S2 is subjected to ultrasonic cleaning, so that particle pollution of more than 2um caused by other processes can be removed. S3, carrying out stress etching, adopting KOH solution to effectively and quickly remove stains, 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. S5, in the sand blasting process, the full surface of the injection pipe is subjected to rapid spraying and sweeping treatment, so that the corrosion of the potassium hydroxide solution on the surface of a product can be removed, but no residual film which can be completely removed exists, and the step can not cause great influence on the surface roughness of the injection pipe. The SC2 cleaning method used in S7 can effectively remove the relevant metal elements such as Na, mg, and Fe 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
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 problem, the invention adopts the following technical scheme: a method of cleaning a spray tube comprising the steps of:
s1, pre-checking: 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 showering by pure water, and then blowing to dry;
s8, wet thermal oxidation: wiping the product clean by pure water and a clean cloth, and carrying out damp-heat oxidation;
s9, appearance detection: and observing the color change condition of the surface of the product, and comparing the color with the picture of the product in the step S1 so as to judge the thickness of the oxide layer on the surface of the injection pipe.
In the cleaning process of the jet pipe, S2 is cleaned by ultrasonic wave, and particle pollution of more than 2um caused by other processes can be removed. S3, carrying out stress etching, adopting KOH solution to effectively and quickly remove stains, 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. S5, in the sand blasting process, the full surface of the injection pipe is subjected to rapid spraying and sweeping treatment, so that the corrosion of the potassium hydroxide solution on the surface of a product can be removed, but no residual film which can be completely removed exists, and the step can not cause great influence on the surface roughness of the injection pipe. The SC2 cleaning method used in S7 can effectively remove the relevant metal elements such as Na, mg, fe, etc. 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.
Preferably, in the S3 process, a comparison sample which is made of 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 in the S3 process, KOH solution is added into the reaction tank for stirring, the temperature of the reaction tank is controlled at 50 ℃, a jet pipe product is placed into the reaction tank, and nitrogen 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 ultrasonic cleaning is controlled to be 50-80 ℃, the cleaning time is 10-20 minutes, and deionized water is added in 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 H 2 O:HCl:H 2 O 2 =5:1:1, the mass concentration of the hydrochloric acid is 49 percentAnd the mass concentration of hydrogen peroxide is 70%, 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 the SC2 tank.
The SC2 cleaning solution provides a low PH environment where alkaline metal ions, metal hydrides, will dissolve in the SC2 cleaning solution.
Preferably, in S7, after the cleaning in the SC2 tank is finished, the product is quickly placed 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.
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) +2H 2 O(g)——SiO 2 (S)+H 2 (g)。
Preferably, the products are dried by nitrogen in S2, S3, S4 and S7. 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 ℃, the time is longer than 5 minutes, and then the product is dried.
Preferably, in S2, the frequency of ultrasonic cleaning is 40kHz, the ultrasonic medium is pure water with the resistivity of more than 15M, the temperature is controlled between 50 ℃ and 70 ℃, and the time is controlled to be 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, and 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 quickly stripping off the stains by generating larger impact force in the process, so that the cleaning effect of the injection pipe can be improved; (4) S5, carrying out rapid spraying and sweeping treatment on the whole surface of the injection pipe in the 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 which can be completely removed exists, and the step can not cause great influence on the surface roughness of the injection pipe; (5) The SC2 cleaning method used in S7 can effectively remove the relevant metal elements such as Na, mg, fe, etc. on the surface of the spray pipe.
Detailed Description
The technical scheme of the invention is further described in detail by the following specific examples:
example (b): a method of cleaning a spray tube comprising the steps of:
s1, pre-checking: 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 the product out of 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 pure water, and then blowing to dry; s3, preparing an etching solution, pouring pure water into a reaction tank, adding a KOH solution, stirring to form the etching solution, controlling the temperature of the reaction tank to be 50 ℃, putting a jet pipe product, and bubbling nitrogen into the reaction tank; s3, in the process, firstly, a comparison sample with the same material as the injection pipe is put into KOH corrosive liquid for etching, and the etching time and the reduced thickness are calculated and recorded; the etching amount is generally controlled to be about 10um, and the etching time is 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 to be 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 product is soaked and cleaned in an ultrasonic cleaning machine, controlling the temperature to be close to 50 ℃ for 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; in S7, a cleaning solution is prepared in SC2, and the volume ratio of each component is H 2 O:HCl:H 2 O 2 =5:1:1, 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 the 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, and after the soaking is finished, spraying with pure water and 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 color change condition of the surface of the product to be observed, and comparing the color with the picture of the product in the step S1, thereby judging the thickness of the oxide layer on the surface of the injection pipe. And S2, S3, S4 and S7, drying the product by adopting nitrogen.
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.
In the cleaning process of the jet pipe, S2 is subjected to ultrasonic cleaning, so that particle pollution of more than 2um caused by other processes can be removed. S3, stress etching is carried out, the KOH solution is adopted to effectively and quickly remove stains, the corrosion tendency to the injection pipe is small, and large impact force is generated in the process to quickly peel off the stains, so that the cleaning effect of the injection pipe can be improved. S5, carrying out rapid spraying and sweeping treatment on the whole surface of the injection pipe in the sand blasting process, removing the corrosion of the potassium hydroxide solution on the surface of the product but not having a residual film which can be completed, and not causing great influence on the surface roughness of the injection pipe. The SC2 cleaning method used in S7 can effectively remove the relevant metal elements such as Na, mg, fe, etc. 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 (7)
1. A cleaning method of an injection pipe is characterized by comprising the following steps:
s1, pre-checking: 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 the product out of 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; s3, in the process, firstly, a comparison sample with the same material as the injection pipe is put into KOH corrosive liquid for etching, and the etching time and the reduced thickness are calculated and recorded; determining the time required for etching the ejector tube by referring to the etching time and the reduced thickness of the comparison sample; s3, pouring pure water into a reaction tank, adding a KOH solution, stirring, controlling the temperature of the reaction tank at 50 ℃, putting a product of an injection pipe, and bubbling nitrogen into the reaction tank;
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; deionized water is added in the cleaning process to keep the ultrasonic cleaning machine in an overflow state;
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; s8, when carrying out damp-heat oxidation, putting the product into a vertical oxidation furnace, and carrying out damp-heat oxidation by using water as an oxidant under the conditions of high temperature and high pressure in the oxidation furnace;
s9, appearance detection: and observing the color change condition of the surface of the product, and comparing the color with the picture of the product in the step S1 so as to judge the thickness of the oxide layer on the surface of the injection pipe.
2. The method for cleaning an injection pipe according to claim 1, wherein the ultrasonic cleaning temperature is controlled to 50 to 80 ℃ and the cleaning time is 10 to 20 minutes in S4.
3. The method for cleaning an injection pipe according to claim 1, wherein in S7, a cleaning solution is prepared in SC2, and the volume ratio of each component is H 2 O:HCl:H 2 O 2 =5:1:1, 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 the SC2 tank.
4. The method as claimed in claim 1, wherein the cleaning in the SC2 tank is finished in S7, and the product is quickly put into a DIW tank to be soaked for 30 minutes or more, and after the soaking is finished, the product is showered by pure water and then dried.
5. The method for cleaning a spray tube of any one of claims 1 to 4, wherein S2, S3, S4, S7 uses nitrogen to blow dry the product.
6. The method for cleaning a spray pipe according to any one of claims 1 to 4, wherein after completion of S5, the product is subjected to immersion cleaning in an ultrasonic cleaner at a temperature of about 50 ℃ for more than 5 minutes, and then is dried.
7. The method of cleaning a spray pipe according to any one of claims 1 to 4, 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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| TWI538043B (en) * | 2013-05-28 | 2016-06-11 | 國立中央大學 | Method for manufacturing bowl shape surface structures of single-crystalline silicon substrates and a single-crystalline silicon substrate with bowl shape surface structures |
| CN105750275B (en) * | 2014-12-18 | 2018-09-21 | 宁夏隆基硅材料有限公司 | A kind of silicon material washing 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 |
| CN110571134B (en) * | 2019-08-06 | 2021-10-22 | 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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