WO2022222787A1 - 陶瓷件清洗方法 - Google Patents

陶瓷件清洗方法 Download PDF

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Publication number
WO2022222787A1
WO2022222787A1 PCT/CN2022/086313 CN2022086313W WO2022222787A1 WO 2022222787 A1 WO2022222787 A1 WO 2022222787A1 CN 2022086313 W CN2022086313 W CN 2022086313W WO 2022222787 A1 WO2022222787 A1 WO 2022222787A1
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Prior art keywords
cleaning
ceramic piece
ceramic
solution
hole
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English (en)
French (fr)
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张帅辉
符雅丽
郑友山
王宏伟
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Beijing Naura Microelectronics Equipment Co Ltd
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Beijing Naura Microelectronics Equipment 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
    • B08B3/04Cleaning 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B27/00Other grinding machines or devices
    • B24B27/033Other grinding machines or devices for grinding a surface for cleaning purposes, e.g. for descaling or for grinding off flaws in the surface

Definitions

  • the invention relates to the field of semiconductor manufacturing, in particular to a cleaning method for ceramic parts.
  • Alumina ceramics is a ceramic material with alumina (Al 2 O 3 ) as the main body, and alumina (Al 2 O 3 ) is the most stable substance in oxides. Therefore, alumina ceramics have high temperature resistance and corrosion resistance. , wear resistance, high mechanical strength, high hardness, high electrical insulation and low dielectric loss, etc., which make alumina ceramics more and more used in semiconductor equipment. However, this material inevitably produces some powder-like particles on the surface during the molding process of granulation, sintering, and machining, which may affect the process results once dropped on the wafer.
  • the nozzle usually adopts a porous structure, and the hole diameter is small, and the particles in the hole are not easy to clean. During the process, the fine particles attached to the hole will fall with the gas. On the wafer, resulting in an increase in the number of particles on the wafer surface, if these particles are not removed, it will seriously affect the process results and chip yield.
  • the existing cleaning methods for the ceramic parts can only remove the particles in the larger blind holes, wrinkles and non-welding gaps on the surface of the ceramic parts.
  • the existing cleaning methods for ceramic parts cannot effectively remove particles in the pores, resulting in poor cleaning effect in the pores.
  • the present invention aims to solve at least one of the technical problems existing in the prior art, and proposes a cleaning method for ceramic parts, which can effectively remove particles in the pores of the ceramic parts.
  • described ceramic piece has porous structure, it is characterized in that, described ceramic piece cleaning method comprises:
  • the ceramic pieces are immersed in a chemical solution and ultrasonically cleaned;
  • a neutralization step soaking the ceramic piece in a neutralizing solution to neutralize the chemical solution remaining on the ceramic piece;
  • a hole flushing step spraying a water column of a specified pressure into the hole to flush the hole;
  • the ceramic piece is immersed in deionized water and ultrasonically cleaned;
  • the ceramic piece is purged, and the ceramic piece is baked after the purging.
  • the chemical cleaning step and the neutralization step are alternately performed at least twice.
  • the cleaning method for the ceramic piece further includes:
  • the ceramic piece is rinsed with pure water
  • the rinsing step is performed at least once after each completion of the chemical cleaning step and after each completion of the neutralization step.
  • the chemical solution is an alkaline solution
  • the alkaline solution is a KOH solution with a concentration percentage of 8%-12%
  • the temperature of the alkaline solution is 55°C- 65°C
  • soaking time is 60min-65min.
  • the chemical solution is an alkaline solution
  • the neutralization solution is an acidic solution
  • the acidic solution is hydrochloric acid or fluoronitric acid solution
  • the soaking time is 5min-10min.
  • the physical grinding of the pore walls in the ceramic piece specifically includes:
  • deionized water is sprayed into the hole, and the resistivity of the deionized water is greater than 4M ⁇ cm; the specified pressure is 40psi to 60psi; the flushing time is 60min- 65min.
  • the ultrasonic cleaning step rotate the ceramic piece at a specified angle every 5min-10min; the resistivity of the deionized water is greater than 4M ⁇ cm; the ultrasonic power is 20-40watts/in2; the cleaning time is 15min-17min.
  • the cleaning method for the ceramic piece further includes:
  • the ceramic piece is wiped with a dust-free cloth dipped in isoacetone, and after wiping, the ceramic piece is rinsed with pure water.
  • the baking time is 2h-3h, and the baking temperature is 100°C-120°C.
  • the ceramic parts cleaning method provided by the embodiment of the present invention realizes the comprehensive cleaning of the ceramic parts by the combination of chemical cleaning, physical grinding and ultrasonic cleaning.
  • Large blind holes, folds and particles in non-welded gaps are cleaned, and then the chemical solution remaining on the ceramic parts is neutralized by the neutralization step, so as to reduce the corrosion of the ceramic parts by the chemical solution and avoid the chemical solution to the ceramic parts.
  • the sealing surface of the parts and the edge of the hole are damaged; after that, the particles that are not easy to be washed and contacted on the wall of the hole can be separated by the physical grinding step, and then the water column of the specified pressure can be sprayed into the hole by the hole washing step. Flushing, so that the particles separated from the hole can be washed out of the hole in a targeted manner.
  • This grinding + water column flushing method can specifically remove the particles in the hole with a smaller size to ensure the cleaning effect in the hole; finally reuse
  • the ultrasonic cleaning step fully cleans the ceramic parts, which can effectively improve the cleaning effect in the
  • FIG. 1 is a flow chart of a method for cleaning a ceramic piece provided by an embodiment of the present invention.
  • DIW deionized water
  • a certain pressure for example, 40-60 psi
  • step S03, step S06 and step S09 are to spray and rinse the ceramic piece as a whole, and the spray range is large. Particles in wrinkles and non-welded gaps, but cannot remove porous and small-sized particles in the hole, and water droplets sprayed on the edge of the hole can easily enlarge the cracks and defects at this position, causing it to generate a new surface damage.
  • the ceramic part is immersed in an acidic or alkaline solution to effectively remove particles on the ceramic part by the dissolving action of the acidic or alkaline solution, but the above-mentioned acidic or alkaline solution is easy to remain on the ceramic part. It may cause damage to the sealing surface of the ceramic part and the edge of the hole, affecting the sealing of the part.
  • step S08 can clean the particles on the ceramic parts by the water wave generated by ultrasonic vibration, this method cannot completely remove the porous and small-sized particles in the pores, and the cleaning effect of the particles in the pores cannot meet the requirements.
  • embodiments of the present invention provide a method for cleaning ceramic parts, which can be applied to the cleaning of ceramic parts such as ceramic covers of process chambers, ceramic nozzles, and ceramic layers of electrostatic chucks in semiconductor equipment, especially applicable
  • ceramic parts such as ceramic covers of process chambers, ceramic nozzles, and ceramic layers of electrostatic chucks in semiconductor equipment, especially applicable
  • porous ceramic parts such as nozzles
  • it can not only remove large blind holes, wrinkles and particles in non-welded gaps on the surface of ceramic parts, but also remove small holes. inner particles.
  • the method for cleaning a ceramic part provided by an embodiment of the present invention includes:
  • ultrasonic cleaning refers to the cleaning of particles on ceramic parts by water waves generated by ultrasonic vibration.
  • the above-mentioned chemical solution includes, for example, an alkaline solution or an acidic solution, which is capable of removing particles on the ceramic part by solution, so as to realize the removal of particles.
  • the above-mentioned chemical solution is an alkaline solution, such as a KOH solution with a concentration percentage of 8%-12%, and the temperature of the alkaline solution is 55°C-65°C; soaking time is 60min-65min.
  • the setting range of the soaking time can not only effectively dissolve the particles on the ceramic parts, but also avoid the damage to the sealing surface and the edge of the holes of the ceramic parts caused by the long soaking time of the ceramic parts in the alkaline solution, which will affect the sealing of the parts. sex.
  • a concentration detector can be used to detect the concentration value of the KOH solution, and the solution can be replaced or supplemented according to the detected concentration value to make it reach the target concentration value.
  • the above-mentioned neutralization step is used to neutralize the chemical solution remaining on the ceramic piece, so as to reduce the corrosion of the ceramic piece by the chemical solution, and prevent the chemical solution from causing damage to the sealing surface and the edge of the hole of the ceramic piece.
  • the neutralization solution used in the step S2 is an acidic solution; on the contrary, when the chemical solution used in the above step S1 is an acidic solution, then the step S2 uses The neutralizing solution is an alkaline solution.
  • the neutralization solution used in the step S2 is an acidic solution, such as hydrochloric acid or a fluoronitric acid solution, wherein the fluoronitric acid solution and the alkaline solution are. Solutions such as KOH solutions are more effective in dissolving.
  • the soaking time is, for example, 5min-10min.
  • the neutralization step may not use ultrasonic cleaning, that is, the ceramic piece may be immersed in the neutralization solution.
  • the above chemical cleaning step and the above neutralization step may be performed alternately at least twice.
  • large-sized blind holes, wrinkles and particles in non-welded gaps on the surface of the ceramic part can be removed effectively and in a targeted manner.
  • the same or different types of chemical solutions can be used in different chemical cleaning steps; the same or different types of neutralizing solutions can also be used in different neutralization steps.
  • the above-mentioned chemical cleaning step and the above-mentioned neutralization step can be carried out alternately twice.
  • KOH solution can be used as the chemical solution used in the two chemical cleaning steps.
  • the first neutralization step uses KOH solution.
  • the neutralization solution used in the second neutralization step can be hydrochloric acid solution; the neutralization solution used in the second neutralization step can be fluoronitric acid solution.
  • the cleaning method of the ceramic parts also includes:
  • the ceramic parts are rinsed with pure water
  • the rinsing step is performed at least once, for example, three times, after each of the above-mentioned chemical cleaning steps and after each of the above-mentioned neutralization steps.
  • S3 physical grinding step, carries out physical grinding to the hole wall in the above-mentioned ceramic piece;
  • the so-called physical grinding refers to the use of grinding tools to penetrate into the hole and rub against the hole wall to separate the particles attached to the hole wall.
  • it can be adapted to porous structures with small pore diameters, such as nozzles.
  • the above-mentioned grinding tool is, for example, a bundled brush, which is composed of, for example, one or more bundles of thin rod-shaped brushes, and the outer diameter of the bundled brush is the same as the inner diameter of the hole in the ceramic piece. It is adapted so that the tufted brush can extend into the opposite hole and rub against the hole wall to achieve physical grinding.
  • the inner diameter of different holes should be equipped with bundled brushes of different outer diameters.
  • the tufted brush is usually made of soft materials to avoid damage to the hole wall, and the outer diameter of the tufted brush can be appropriately larger than the inner diameter of the hole to ensure that the tufted brush extends into the hole when It can produce a certain extrusion deformation, so that a friction force sufficient to remove particles can be formed between the hole wall and the hole wall.
  • the above-mentioned physical grinding step may be repeated multiple times, eg, five times, according to the actual cleaning effect.
  • the above-mentioned water column should be adapted to the inner diameter of the hole, so that the hole can be washed individually in a targeted manner, so as to realize the cleaning in the hole, which is in contrast to the use of pure water in the above-mentioned washing step to wash the whole ceramic piece untargeted.
  • the way is completely different.
  • the spray range of the hole flushing step is limited to the inside of the hole, which is obviously smaller than the spray range of the above flushing step, and the flushing effects of the two are completely different.
  • the above-mentioned specified pressure should be set such that there is sufficient pressure to flush the particles separated by the physical grinding step in the hole to the outside of the hole.
  • deionized water is sprayed into the hole, and the resistivity of the deionized water is greater than 4M ⁇ cm; the above specified pressure is 40psi-60psi; and the flushing time is 60min-65min.
  • the above-mentioned hole washing step is used to spray the water column of the specified pressure into the hole for washing.
  • the separated particles are washed out of the hole, so that the cleaning effect in the hole can be guaranteed.
  • the above-mentioned ultrasonic cleaning step is used for comprehensive cleaning of the ceramic parts. Since the cleaning effect of ultrasonic cleaning with deionized water is the most obvious, after the ultrasonic cleaning step is completed, the cleaning effect of the ceramic parts can be guaranteed to meet the technological requirements. Moreover, the removal of the particles in the pores has been achieved by the previous physical grinding step and the step of rinsing the pores, which can make up for the deficiency that the ultrasonic cleaning cannot completely remove the particles in the pores.
  • the ceramic parts are rotated at a specified angle every 5min-10min to achieve comprehensive cleaning of the ceramic parts;
  • the resistivity of the deionized water is greater than 4M ⁇ cm;
  • the ultrasonic power is 20-40watts/ in 2 , further 10 to 20 watts/in 2 , this power range is suitable for cleaning small-sized or coated ceramic parts to avoid damage to the ceramic parts due to excessive cleaning force;
  • the cleaning time is 15min-17min.
  • deionized water is in a circulating flow state, that is, new deionized water is always introduced into the cleaning tank (such as the bottom of the self-cleaning tank), And the deionized water in the cleaning tank is discharged by overflow.
  • the ceramic pieces are placed in a purged purification furnace (or oven) for baking.
  • the baking time is 2h-3h; the baking temperature is 100°C-120°C.
  • the larger-sized particles on the ceramic piece may be removed in advance, for example, by wiping.
  • the cleaning method for the ceramic piece further includes:
  • the wiping step wipe the ceramic piece with a clean cloth dipped in isoacetone (IPA), and rinse the ceramic piece with pure water after wiping.
  • IPA isoacetone
  • the entire cleaning process should be carried out in a clean cleaning environment.
  • a clean cleaning environment For example, for ceramic nozzles, they should be placed in a class 100 clean room for cleaning to avoid contamination by particles in the air.
  • the ceramic parts cleaning method provided by the embodiment of the present invention realizes the comprehensive cleaning of the ceramic parts by the combination of chemical cleaning, physical grinding and ultrasonic cleaning.
  • Large blind holes, folds and particles in non-welded gaps are cleaned, and then the chemical solution remaining on the ceramic parts is neutralized by the neutralization step, so as to reduce the corrosion of the ceramic parts by the chemical solution and avoid the chemical solution to the ceramic parts.
  • the sealing surface of the parts and the edge of the hole are damaged; after that, the particles that are not easy to be washed and contacted on the wall of the hole can be separated by the physical grinding step, and then the water column of the specified pressure can be sprayed into the hole by the hole washing step. Flushing, so that the particles separated from the hole can be washed out of the hole in a targeted manner.
  • This grinding + water column flushing method can specifically remove the particles in the hole with a smaller size to ensure the cleaning effect in the hole; finally reuse
  • the ultrasonic cleaning step fully cleans the ceramic parts, which can effectively improve the cleaning effect in the

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

Abstract

一种陶瓷件清洗方法,包括:化学清洗步骤,将陶瓷件浸泡在化学溶液中,并进行超声波清洗;中和步骤,将陶瓷件浸泡在中和溶液中,以中和残留在陶瓷件上的化学溶液;物理研磨步骤,对陶瓷件中的孔壁进行物理研磨;孔冲洗步骤,向孔内喷淋指定压力的水柱,以对孔内进行冲洗;超声波清洗步骤,将陶瓷件浸泡在去离子水中,并进行超声波清洗;吹扫和烘干步骤,对陶瓷件进行吹扫,并在吹扫后对陶瓷件进行烘烤。该陶瓷件清洗方法,可以有效去除陶瓷件的孔内颗粒。

Description

陶瓷件清洗方法 技术领域
本发明涉及半导体制造领域,具体地,涉及一种陶瓷件清洗方法。
背景技术
氧化铝陶瓷是一种以氧化铝(Al 2O 3)为主体的陶瓷材料,而氧化铝(Al 2O 3)是氧化物中最稳定的物质,因此,氧化铝陶瓷具有耐高温、耐腐蚀、耐磨、机械强度高、硬度大、电绝缘性高与介电损耗低等的优势,这使得氧化铝陶瓷越来越多地应用在半导体设备中。但是,这种材料在造粒、烧结和机加工等的成型过程中不可避免地会在表面产生一些粉末状的颗粒,这些颗粒一旦掉落在晶圆上,可能会影响工艺结果。尤其对于用于向腔室通入气体的陶瓷喷嘴,该喷嘴通常采用多孔结构,且孔径较小,孔内的颗粒不易清洗,在工艺过程中,附着在孔内的细微颗粒会随气体落在晶圆上,从而导致晶圆表面的颗粒数增多,这些颗粒如果不加以去除,会严重影响到工艺结果和芯片良率。
为了去除陶瓷件上的颗粒,就需要对陶瓷件进行清洗,但是,现有的陶瓷件清洗方法只能去除陶瓷件表面上尺寸较大的盲孔、褶皱及非焊接缝隙处的颗粒,而对于诸如喷嘴等的多孔陶瓷件,由于孔径较小,现有的陶瓷件清洗方法无法有效去除孔内颗粒,从而导致孔内清洗效果较差。
发明内容
本发明旨在至少解决现有技术中存在的技术问题之一,提出了一种陶瓷件清洗方法,其可以有效去除陶瓷件的孔内颗粒。
为实现本发明的目的而提供一种陶瓷件清洗方法,所述陶瓷件具有多孔 结构,其特征在于,所述陶瓷件清洗方法包括:
化学清洗步骤,将陶瓷件浸泡在化学溶液中,并进行超声波清洗;
中和步骤,将所述陶瓷件浸泡在中和溶液中,以中和残留在所述陶瓷件上的所述化学溶液;
物理研磨步骤,对所述陶瓷件中的孔壁进行物理研磨;
孔冲洗步骤,向所述孔内喷淋指定压力的水柱,以对所述孔内进行冲洗;
超声波清洗步骤,将所述陶瓷件浸泡在去离子水中,并进行超声波清洗;
吹扫和烘干步骤,对所述陶瓷件进行吹扫,并在吹扫后对所述陶瓷件进行烘烤。
可选的,在进行所述物理研磨步骤之前,循环交替进行所述化学清洗步骤和所述中和步骤至少两次。
可选的,所述陶瓷件清洗方法还包括:
冲洗步骤,使用纯水对所述陶瓷件进行冲洗;
其中,在每次所述化学清洗步骤完成之后,和在每次所述中和步骤完成之后均进行所述冲洗步骤至少一次。
可选的,在所述化学清洗步骤中,所述化学溶液为碱性溶液,所述碱性溶液为浓度百分比为8%-12%的KOH溶液,所述碱性溶液的温度为55℃-65℃;浸泡时间为60min-65min。
可选的,在所述化学清洗步骤中,所述化学溶液为碱性溶液;在所述中和步骤中,所述中和溶液为酸性溶液,且所述酸性溶液为盐酸或者氟硝酸溶液;浸泡时间为5min-10min。
可选的,所述对所述陶瓷件中的孔壁进行物理研磨具体包括:
使用外径与所述陶瓷件中的孔的内径相适配的束状毛刷,伸入所述孔中,对所述孔的内壁进行清洗至少5次。
可选的,在所述孔冲洗步骤中,向所述孔内喷淋去离子水,所述去离子 水的电阻率大于4MΩ·cm;所述指定压力为40psi~60psi;冲洗时间为60min-65min。
可选的,在所述超声波清洗步骤中,每间隔5min-10min旋转所述陶瓷件指定角度;所述去离子水的电阻率大于4MΩ·cm;超声波功率为20-40watts/in2;清洗时间为15min-17min。
可选的,在所述化学清洗步骤之前,所述陶瓷件清洗方法还包括:
擦拭步骤,使用沾有异丙酮的无尘布擦拭所述陶瓷件,并在擦拭之后使用纯水对所述陶瓷件进行冲洗。
可选的,在所述吹扫和烘干步骤中,烘烤时间为2h-3h;烘烤温度为100℃-120℃。
本发明具有以下有益效果:
本发明实施例提供的陶瓷件清洗方法,其利用化学清洗、物理研磨和超声波清洗相结合的方式实现对陶瓷件进行全面清洗,具体来说,首先利用化学清洗步骤可以有效对陶瓷件表面上尺寸较大的盲孔、褶皱及非焊接缝隙处的颗粒进行清洗,之后再利用中和步骤中和残留在陶瓷件上的化学溶液,从而可以减少化学溶液对陶瓷件的腐蚀,避免化学溶液对陶瓷件的密封面和孔边缘处产生损伤;之后,利用物理研磨步骤可以将附着在孔壁上不易冲洗、不易接触到的颗粒分离出来,再利用孔冲洗步骤向孔内喷淋指定压力的水柱进行冲洗,以能够有针对性地将孔内分离出来的颗粒冲刷至孔外,这种研磨+水柱冲洗方式可以有针对性地去除尺寸较小的孔内颗粒,保证孔内清洗效果;最后再利用超声波清洗步骤对陶瓷件进行全面清洗,最终可以有效提高清洗效果。
附图说明
图1为本发明实施例提供的陶瓷件清洗方法的流程框图。
具体实施方式
为使本领域的技术人员更好地理解本发明的技术方案,下面结合附图来对本发明实施例提供的陶瓷件清洗方法进行详细描述。
作为本发明实施例的一个对比实施例,提供一种陶瓷件清洗方法,包括以下步骤:
S01、将陶瓷件浸入酸性或碱性脱脂剂中,浸泡时间为15-30分钟;
S02、将陶瓷件浸入去离子水(电阻率≥200kΩ·cm)中,浸泡时间为3分钟以上;
S03、使用一定压力(例如为40-60psi)的去离子水(DIW)喷淋陶瓷件,以冲洗陶瓷件上所有的盲孔、褶皱以及非焊接缝隙;
S04、将陶瓷件浸入酸性或者碱性溶液中,浸泡时间为30-120分钟;
S05、将陶瓷件浸入去离子水中,浸泡时间为3分钟以上;
S06、使用一定压力(例如为40-60psi)的去离子水(电阻率≥4MΩ·cm)对陶瓷件进行第二次喷淋冲洗;
S07、将陶瓷件浸入去离子水(电阻率≥4MΩ·cm,温度38~46℃)中浸泡5分钟;
S08、将陶瓷件浸入去离子水(电阻率≥4MΩ·cm),并进行超声波清洗,清洗时间为10~20分钟;
S09、使用一定压力(例如为40-60psi)的去离子水(电阻率≥4MΩ·cm)对陶瓷件进行第三次喷淋冲洗;
S010、对陶瓷件进行吹扫和烘干。
上述陶瓷件清洗方法在实际应用中不可避免地存在以下问题:
其一,上述步骤S03、步骤S06和步骤S09是对陶瓷件在整体上进行喷淋冲洗,喷淋范围较大,这种喷淋冲洗的方式没有针对性,只能去除陶瓷件上盲孔、褶皱以及非焊接缝隙处的颗粒,但无法去除多孔,且尺寸较小的孔 内颗粒,而且喷淋在孔边缘处的水滴很容易加大该位置处的裂纹和缺陷,使其产生新的表面损伤。
其二,上述步骤S04中,将陶瓷件浸入酸性或者碱性溶液中,以利用酸性或者碱性溶液的溶解作用有效去除陶瓷件上的颗粒,但是,上述酸性或者碱性溶液容易残留在陶瓷件上,可能导致陶瓷件的密封面和孔边缘处产生损伤,影响零件的密封性。
其三,上述步骤S08虽然可以通过超声波震荡产生的水波清洗陶瓷件上的颗粒,但是,这种方式也无法完全去除多孔,且尺寸较小的孔内颗粒,孔内颗粒清洗效果无法达到要求。
为了解决上述问题,本发明实施例提供一种陶瓷件清洗方法,其可以应用于半导体设备中工艺腔室的陶瓷盖、陶瓷喷嘴和静电卡盘的陶瓷层等的陶瓷件的清洗,尤其可应用于多孔,且孔径尺寸较小的陶瓷件(例如喷嘴)的清洗,既可以去除陶瓷件表面上的尺寸较大的盲孔、褶皱以及非焊接缝隙处的颗粒,又可以去除尺寸较小的孔内颗粒。
具体地,请参阅图1,本发明实施例提供的陶瓷件清洗方法包括:
S1、化学清洗步骤,将陶瓷件浸泡在化学溶液中,并进行超声波清洗;
所谓超声波清洗,是指通过超声波震荡产生的水波清洗陶瓷件上的颗粒。
上述化学溶液例如包括碱性溶液或酸性溶液等的能够溶液去除陶瓷件上的颗粒的溶液,以实现颗粒的去除。
为了有效溶解陶瓷件上的颗粒,提高清洗效果,可选的,上述化学溶液为碱性溶液,该碱性溶液例如为浓度百分比为8%-12%的KOH溶液,该碱性溶液的温度为55℃-65℃;浸泡时间为60min-65min。该浸泡时间的设定范围既可以有效溶解陶瓷件上的颗粒,又可以避免陶瓷件在碱性溶液中的浸泡时间过长而导致陶瓷件的密封面和孔边缘处产生损伤,影响零件的密封性。
在实际应用中,可以利用浓度检测仪检测KOH溶液的浓度值,并根据检测到的浓度值对溶液进行更换或者补充,以使其达到目标浓度值。
S2、中和步骤,将上述陶瓷件浸泡在中和溶液中;
上述中和步骤用于中和残留在陶瓷件上的化学溶液,以减少化学溶液对陶瓷件的腐蚀,避免化学溶液对陶瓷件的密封面和孔边缘处产生损伤。
容易理解,当上述步骤S1中使用的化学溶液为碱性溶液时,则步骤S2使用的中和溶液为酸性溶液;反之,当上述步骤S1中使用的化学溶液为酸性溶液时,则步骤S2使用的中和溶液为碱性溶液。
可选的,当上述步骤S1中使用的化学溶液为碱性溶液时,则步骤S2使用的中和溶液为酸性溶液,该酸性溶液例如为盐酸或者氟硝酸溶液,其中,氟硝酸溶液与碱性溶液(例如KOH溶液)的溶解作用更优。
可选的,在上述中和步骤中,浸泡时间例如为5min-10min。另外,中和步骤可以不使用超声波清洗,即,将陶瓷件浸泡在中和溶液中即可。
可选的,在进行下述步骤S3之前,可以循环交替进行上述化学清洗步骤和上述中和步骤至少两次。这样,可以有效且有针对性地对陶瓷件表面上的尺寸较大的盲孔、褶皱以及非焊接缝隙处的颗粒进行去除。需要说明的是,不同次的化学清洗步骤中可以采用相同或不同种类的化学溶液;不同次的中和步骤中也可以采用相同或不同种类的中和溶液。
例如,可以循环交替进行上述化学清洗步骤和上述中和步骤两次,具体地,两次化学清洗步骤所使用的化学溶液均可以采用KOH溶液,在此基础上,第一次中和步骤所使用的中和溶液可以采用盐酸溶液;第二次中和步骤所使用的中和溶液可以采用氟硝酸溶液。通过实验发现,这种溶液的组合可以有效对陶瓷件表面上的尺寸较大的盲孔、褶皱以及非焊接缝隙处的颗粒进行去除。
为了进一步减少残留在陶瓷件表面上的化学溶液以及颗粒,可选的,陶 瓷件清洗方法还包括:
冲洗步骤,使用纯水对陶瓷件进行冲洗;
其中,在每次上述化学清洗步骤完成之后,和在每次上述中和步骤完成之后均进行冲洗步骤至少一次,例如为三次。
S3、物理研磨步骤,对上述陶瓷件中的孔壁进行物理研磨;
所谓物理研磨,是指使用研磨工具伸入孔中与孔壁接触摩擦,以将附着在孔壁上的颗粒分离出来,这种方式可以有效清除孔内吸附比较牢固,且不易接触到的颗粒,尤其可以适应于多孔,且孔径较小的结构,例如喷嘴。
可选的,上述研磨工具例如为束状毛刷,该束状毛刷例如由一束或多束细杆状毛刷组成,且束状毛刷的外径与陶瓷件中的孔的内径相适配,以使束状毛刷能够伸入对孔中,并与孔壁接触摩擦,从而实现物理研磨。不同的孔的内径应配备不同外径的束状毛刷。
在实际应用中,束状毛刷通常采用软质材料,以避免对孔壁造成损伤,而且束状毛刷的外径可以适当大于孔的内径,以保证束状毛刷在伸入孔中时能够产生一定的挤压变形,从而能够与孔壁之间形成足以剔除颗粒的摩擦力。
可选的,上述物理研磨步骤可以根据实际清洗效果重复进行多次,例如五次。
S4、孔冲洗步骤,向孔内喷淋指定压力的水柱,以对孔内进行冲洗;
上述水柱应与孔的内径相适配,以能够有针对性地对孔进行单独冲刷,从而实现孔内清洗,这与上述冲洗步骤中使用纯水无针对性地对陶瓷件的整体进行冲洗的方式完全不同。换句话说,孔冲洗步骤的喷淋范围仅限于孔内,明显小于上述冲洗步骤的喷淋范围,且二者的冲洗效果也完全不同。
另外,上述指定压力的设定应满足:有足够的压力将孔内经物理研磨步骤分离出来的颗粒冲刷至孔外。例如,可选的,在上述孔冲洗步骤中,向孔内喷淋去离子水,该去离子水的电阻率大于4MΩ·cm;上述指定压力为40psi ~60psi;冲洗时间为60min-65min。
在通过物理研磨步骤将附着在孔壁上的颗粒分离出来之后,再利用上述孔冲洗步骤向孔内喷淋指定压力的水柱进行冲洗,这种研磨+水柱冲洗方式可以有针对性地将孔内分离出来的颗粒冲刷至孔外,从而可以保证孔内清洗效果。
S5、超声波清洗步骤,将陶瓷件浸泡在去离子水中,并进行超声波清洗;
上述超声波清洗步骤用于对陶瓷件进行全面清洗,由于使用去离子水进行超声波清洗的清洗效果最明显,在完成超声波清洗步骤之后,可以保证陶瓷件的清洗效果满足工艺要求。而且,利用前面的物理研磨步骤和孔冲洗步骤已经实现了孔内颗粒的清除,从而可以弥补超声波清洗无法完全去除孔内颗粒的不足。
可选的,在上述超声波清洗步骤中,每间隔5min-10min旋转陶瓷件指定角度,以实现对陶瓷件进行全面清洗;上述去离子水的电阻率大于4MΩ·cm;超声波功率为20-40watts/in 2,进一步为10~20watts/in 2,该功率范围适应于尺寸较小或者具有涂层的陶瓷件的清洗,以避免陶瓷件因清洗力度过大而产生损伤;清洗时间为15min-17min。
可选的,为了进一步提高清洗效果,在进行上述超声波清洗步骤的过程中,去离子水处于循环流动状态,即,始终向清洗槽中(例如自清洗槽底部)通入新的去离子水,并采用溢流的方式排出清洗槽中的去离子水。
S6、吹扫和烘干步骤,对上述陶瓷件进行吹扫,并在吹扫后对陶瓷件进行烘烤。
可选的,首先使用经滤孔尺寸为0.1μm的过滤器过滤后的干燥氮气对陶瓷件进行全面吹扫;然后使用经滤孔尺寸为0.1μm的过滤器过滤后的干燥氮气吹扫净化炉(或烘箱),以烘干其内部;最后,将陶瓷件放入吹扫后的净化炉(或烘箱)中进行烘烤。进一步可选的,烘烤时间为2h-3h;烘烤温 度为100℃-120℃。
可选的,可以在进行上述步骤S1之前,预先将陶瓷件上尺寸较大的颗粒进行清除,例如,采用擦拭的方式进行清除。具体地,在上述化学清洗步骤(步骤S1)之前,陶瓷件清洗方法还包括:
擦拭步骤,使用沾有异丙酮(IPA)的无尘布擦拭陶瓷件,并在擦拭之后使用纯水对陶瓷件进行冲洗。
应当注意的是,若无尘布表面有污渍,需要重新清洗无尘布,以避免对陶瓷件表面的纹理和光滑表面造成损伤。
在实际应用中,整个清洗过程应在干净的清洗环境中进行,例如对于陶瓷喷嘴,应将其放置在百级净化室中进行清洗,以避免其受到空气中的颗粒污染。
本发明实施例提供的陶瓷件清洗方法,其利用化学清洗、物理研磨和超声波清洗相结合的方式实现对陶瓷件进行全面清洗,具体来说,首先利用化学清洗步骤可以有效对陶瓷件表面上尺寸较大的盲孔、褶皱及非焊接缝隙处的颗粒进行清洗,之后再利用中和步骤中和残留在陶瓷件上的化学溶液,从而可以减少化学溶液对陶瓷件的腐蚀,避免化学溶液对陶瓷件的密封面和孔边缘处产生损伤;之后,利用物理研磨步骤可以将附着在孔壁上不易冲洗、不易接触到的颗粒分离出来,再利用孔冲洗步骤向孔内喷淋指定压力的水柱进行冲洗,以能够有针对性地将孔内分离出来的颗粒冲刷至孔外,这种研磨+水柱冲洗方式可以有针对性地去除尺寸较小的孔内颗粒,保证孔内清洗效果;最后再利用超声波清洗步骤对陶瓷件进行全面清洗,最终可以有效提高清洗效果。
可以理解的是,以上实施方式仅仅是为了说明本发明的原理而采用的示例性实施方式,然而本发明并不局限于此。对于本领域内的普通技术人员而言,在不脱离本发明的精神和实质的情况下,可以做出各种变型和改进,这 些变型和改进也视为本发明的保护范围。

Claims (10)

  1. 一种陶瓷件清洗方法,所述陶瓷件具有多孔结构,其特征在于,所述陶瓷件清洗方法包括:
    化学清洗步骤,将陶瓷件浸泡在化学溶液中,并进行超声波清洗;
    中和步骤,将所述陶瓷件浸泡在中和溶液中,以中和残留在所述陶瓷件上的所述化学溶液;
    物理研磨步骤,对所述陶瓷件中的孔壁进行物理研磨;
    孔冲洗步骤,向所述孔内喷淋指定压力的水柱,以对所述孔内进行冲洗;
    超声波清洗步骤,将所述陶瓷件浸泡在去离子水中,并进行超声波清洗;
    吹扫和烘干步骤,对所述陶瓷件进行吹扫,并在吹扫后对所述陶瓷件进行烘烤。
  2. 根据权利要求1所述的陶瓷件清洗方法,其特征在于,在进行所述物理研磨步骤之前,循环交替进行所述化学清洗步骤和所述中和步骤至少两次。
  3. 根据权利要求1或2所述的陶瓷件清洗方法,其特征在于,所述陶瓷件清洗方法还包括:
    冲洗步骤,使用纯水对所述陶瓷件进行冲洗;
    其中,在每次所述化学清洗步骤完成之后,和在每次所述中和步骤完成之后均进行所述冲洗步骤至少一次。
  4. 根据权利要求1或2所述的陶瓷件清洗方法,其特征在于,在所述化学清洗步骤中,所述化学溶液为碱性溶液,所述碱性溶液为浓度百分比为8%-12%的KOH溶液,所述碱性溶液的温度为55℃-65℃;浸泡时间为60min-65min。
  5. 根据权利要求1或2所述的陶瓷件清洗方法,其特征在于,在所述化学清洗步骤中,所述化学溶液为碱性溶液;在所述中和步骤中,所述中和溶液为酸性溶液,且所述酸性溶液为盐酸或者氟硝酸溶液;浸泡时间为5min-10min。
  6. 根据权利要求1所述的陶瓷件清洗方法,其特征在于,所述对所述陶瓷件中的孔壁进行物理研磨具体包括:
    使用外径与所述陶瓷件中的孔的内径相适配的束状毛刷,伸入所述孔中,对所述孔的内壁进行清洗至少5次。
  7. 根据权利要求1所述的陶瓷件清洗方法,其特征在于,在所述孔冲洗步骤中,向所述孔内喷淋去离子水,所述去离子水的电阻率大于4MΩ·cm;所述指定压力为40psi~60psi;冲洗时间为60min-65min。
  8. 根据权利要求1所述的陶瓷件清洗方法,其特征在于,在所述超声波清洗步骤中,每间隔5min-10min旋转所述陶瓷件指定角度;所述去离子水的电阻率大于4MΩ·cm;超声波功率为20-40 watts/in2;清洗时间为15min-17min。
  9. 根据权利要求1所述的陶瓷件清洗方法,其特征在于,在所述化学清洗步骤之前,所述陶瓷件清洗方法还包括:
    擦拭步骤,使用沾有异丙酮的无尘布擦拭所述陶瓷件,并在擦拭之后使用纯水对所述陶瓷件进行冲洗。
  10. 根据权利要求1所述的陶瓷件清洗方法,其特征在于,在所述吹扫和烘干步骤中,烘烤时间为2h-3h;烘烤温度为100℃-120℃。
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