WO2022242539A1 - 陶瓷件清洗方法 - Google Patents

陶瓷件清洗方法 Download PDF

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Publication number
WO2022242539A1
WO2022242539A1 PCT/CN2022/092423 CN2022092423W WO2022242539A1 WO 2022242539 A1 WO2022242539 A1 WO 2022242539A1 CN 2022092423 W CN2022092423 W CN 2022092423W WO 2022242539 A1 WO2022242539 A1 WO 2022242539A1
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Prior art keywords
ceramic
equal
cleaning
ceramic parts
solution
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English (en)
French (fr)
Inventor
王宏伟
张宝辉
符雅丽
郑友山
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Beijing Naura Microelectronics Equipment Co Ltd
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Beijing Naura Microelectronics Equipment Co Ltd
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B1/00—Cleaning by methods involving the use of tools
    • B08B1/10—Cleaning by methods involving the use of tools characterised by the type of cleaning tool
    • B08B1/14—Wipes; Absorbent members, e.g. swabs or sponges
    • B08B1/143—Wipes
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations

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 mainly composed of alumina (Al 2 O 3 ), which is the most stable substance among oxides.
  • alumina Al 2 O 3
  • This material will inevitably produce some powdery particles on the surface during the molding process of granulation, sintering and machining. Once these particles fall on the wafer during the semiconductor manufacturing process, it may affect The result of the process, for example, the conduction of different wires, the disconnection of the same wire, the formation of holes, resulting in greater energy consumption and heat generation, etc. If these particles are not removed, it will seriously affect the process results and chip yield.
  • 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 suspended particles and damaged layers on ceramic parts, thereby solving the problem that the number of ceramic particles exceeds the standard, Improve chip yield.
  • a chemical solution is used to dissolve the particles on the ceramic parts
  • a specified acidic solution is used to soften and corrode the particles on the ceramic parts and eliminate the damaged layer on the ceramic parts;
  • ultrasonic cleaning is used to clean the ceramic parts to remove residual particles and solutions on the ceramic parts.
  • the specified acidic solution includes fluoronitric acid solution
  • the fluoronitric acid solution is formed by mixing hydrofluoric acid solution, nitric acid solution and pure water.
  • the ratio of the hydrofluoric acid solution, nitric acid solution and pure water with a resistivity of 18M ⁇ cm is 1:1:1;
  • the range of the mass fraction of hydrofluoric acid contained in the hydrofluoric acid solution is greater than or equal to 5%, and less than or equal to 15%; the range of the mass fraction of nitric acid contained in the nitric acid solution is greater than or equal to 25%, and less than or equal to 35% %.
  • the second cleaning process is performed at least 4 times.
  • the second cleaning process specifically includes the following steps:
  • the ceramic part is rinsed at least 3 times with the specified acidic solution; in the step S22, the ceramic part rinsed with the specified acidic solution is soaked in the The range of soaking time in the specified acidic solution is greater than or equal to 10 minutes and less than or equal to 20 minutes; in the step S23, the soaked ceramic parts are rinsed 3 to 5 times with pure water; in the step S24, the The polishing tool made of nanomaterials wipes the ceramic parts rinsed with pure water for 3 to 5 times; in the step S25, the range of cleaning time for ultrasonic cleaning is greater than or equal to 15min and less than or equal to 30min; the step In S26, the range of time for rinsing the ceramic part after ultrasonic cleaning with pure water is greater than or equal to 15 minutes and less than or equal to 60 minutes.
  • the first cleaning process specifically includes the following steps:
  • the purity of the isopropanone solution is 99.7%;
  • the alkaline solution is a KOH solution with a concentration percentage greater than or equal to 15% and less than or equal to 20%, and the temperature range of the alkaline solution is greater than or equal to 75°C, and less than or equal to 85°C;
  • the time range for ultrasonic cleaning is greater than or equal to 1h, and less than or equal to 3h;
  • the step S13 use pure water to clean the ultrasonically
  • the ceramic parts are rinsed 3 to 5 times; in the step S14, the immersion time of the rinsed ceramic parts in the acid solution ranges from greater than or equal to 5 minutes to less than or equal to 10 minutes; in the step S15, using Rinse the ceramic parts soaked in the acidic solution 3 to 5 times with pure water; in the step S16, the immersion time of the rinsed ceramic parts in the alkaline solution is greater than or equal to 1h , and less than or equal to 3h.
  • the third cleaning process specifically includes the following steps:
  • the washing time range is greater than or equal to 45 minutes and less than or equal to 60 minutes; in the step S32, the time range for ultrasonic cleaning is greater than or equal to 30 minutes and less than or equal to 60 minutes; the step In S33, the range of soaking time is greater than or equal to 30min and less than or equal to 60min; in the step S33, the range of maintaining the temperature of the deionized water is greater than or equal to 32°C and less than or equal to 42°C; in the step S34 , the purging gas used includes nitrogen, and the purity of the nitrogen is 99.999%; the range of the included angle between the purging direction of the nitrogen and the surface of the ceramic part is greater than or equal to 30°C and less than or equal to 45°C.
  • the ceramic part includes a ceramic process kit for semiconductor equipment.
  • the method for cleaning ceramic parts divides the cleaning into three cleaning processes, wherein the first cleaning process uses a chemical solution to dissolve the particles on the ceramic parts, and this process can effectively remove the larger particles on the surface of the ceramic parts. Clean the particles in blind holes, folds and non-welded gaps; the second cleaning process uses a designated acid solution to soften and corrode the particles on the ceramic parts and eliminate the damage layer on the ceramic parts, because the existence of the damage layer is an important source of particle generation One, the above-mentioned second cleaning process eliminates the damage layer on the ceramic parts in a targeted manner through the above-mentioned designated acid solution, which can effectively remove particles at the source, which can greatly reduce the number of particles compared with the prior art; the third cleaning The process uses ultrasonic cleaning to clean the ceramic parts to remove the remaining particles and solution (acidic or alkaline solution) on the ceramic parts, so that the ceramic parts can be fully cleaned, and finally the cleaning effect can be effectively improved, and the problem of excessive ceramic particles can be solved. problem, improve chip
  • Fig. 1 is the block flow diagram of the cleaning method for ceramic parts provided by the embodiment of the present invention.
  • Fig. 2 is the block flow diagram of the second cleaning process that the embodiment of the present invention adopts
  • Fig. 3 is the block flow diagram of the first cleaning process that the embodiment of the present invention adopts
  • Fig. 4 is the block flow diagram of the 3rd cleaning process that the embodiment of the present invention adopts
  • Fig. 5 is a comparison diagram of the damage layer on the ceramic parts obtained respectively by the cleaning method of the ceramic parts in the prior art and the cleaning method of the ceramic parts provided by the embodiment of the present invention;
  • FIG. 6 is a comparison diagram of suspended particles on ceramic parts obtained by using the method for cleaning ceramic parts in the prior art and the method for cleaning ceramic parts provided by the embodiment of the present invention, respectively.
  • An embodiment of the present invention provides a method for cleaning ceramic parts, which can be applied to the cleaning of ceramic parts such as a process suite of a process chamber, a ceramic cover, and a ceramic layer of an electrostatic chuck in a semiconductor device.
  • the cleaning method of ceramic parts includes:
  • the first cleaning process S1 using a chemical solution to dissolve the particles on the ceramic piece;
  • the first cleaning process S1 can effectively clean the particles on the surface of the ceramic part, especially the particles in the larger blind holes, folds and non-welding gaps on the surface of the ceramic part.
  • the designated acid solution is used to soften and corrode the particles on the ceramic parts and eliminate the damaged layer on the ceramic parts;
  • the above-mentioned second cleaning process S2 uses the above-mentioned designated acid solution to eliminate the damaged layer on the ceramic parts in a targeted manner, which can effectively remove the particles at the source, which is different from existing The number of particles can be greatly reduced compared to other technologies.
  • ultrasonic cleaning is used to clean the ceramic parts to remove residual particles and solutions on the ceramic parts.
  • the so-called ultrasonic cleaning refers to the cleaning of particles on ceramic parts by water waves generated by ultrasonic vibration.
  • the third cleaning process S3 can fully clean the ceramic parts to remove residual particles and solutions (acidic or alkaline solutions) on the ceramic parts, and finally can effectively improve the cleaning effect.
  • the designated acidic solution includes fluoronitric acid solution, which is formed by mixing hydrofluoric acid solution, nitric acid solution and pure water, which can soften and corrode particles on ceramic parts and eliminate ceramics. Damaged layers on parts.
  • fluoronitric acid solution is formed by mixing hydrofluoric acid solution, nitric acid solution and pure water, which can soften and corrode particles on ceramic parts and eliminate ceramics. Damaged layers on parts.
  • any other acid solution that can play the same role can also be used.
  • the ratio of the above-mentioned hydrofluoric acid solution, nitric acid solution and pure water with a resistivity of 18M ⁇ cm is 1:1:1 ;
  • the range of the mass fraction of hydrofluoric acid contained in the hydrofluoric acid solution is greater than or equal to 5%, and less than or equal to 15%;
  • the range of the mass fraction of nitric acid contained in the nitric acid solution is greater than or equal to 25%, and less than or equal to 35% .
  • the above-mentioned second cleaning process S2 is performed at least 4 times.
  • the second cleaning process S2 specifically includes the following steps:
  • step S21 the ceramic piece is rinsed at least 3 times with a specified acidic solution.
  • the range of soaking time for immersing the ceramic parts rinsed with the specified acidic solution in the specified acidic solution is greater than or equal to 10min and less than or equal to 20min.
  • the soaked ceramic piece is rinsed 3 to 5 times with pure water.
  • a polishing tool made of nanomaterials is used to wipe the ceramic piece rinsed with pure water for 3 to 5 times.
  • the range of cleaning time for ultrasonic cleaning is greater than or equal to 15 minutes and less than or equal to 30 minutes.
  • the time for rinsing the ultrasonically cleaned ceramic piece with pure water is greater than or equal to 15 minutes and less than or equal to 60 minutes.
  • the first cleaning process S1 specifically includes the following steps:
  • the above step S11 can conduct electricity to the ceramic piece, so as to neutralize the charged ceramic particles on the ceramic piece.
  • the purity of the above-mentioned isopropanone solution is 99.7%.
  • Alkaline solution that is, used as the chemical solution in the first cleaning process S1
  • the above-mentioned alkaline solution is, for example, a KOH solution with a concentration percentage greater than or equal to 15% and less than or equal to 20%, and the temperature range of the alkaline solution is greater than or equal to 75°, and less than or equal to 85°; in step S12, the time range for ultrasonic cleaning is greater than or equal to 1h, and less than or equal to 3h, and the time of ultrasonic cleaning is set within the above range, which can effectively dissolve ceramics Particles on the parts can prevent the ceramic parts from being soaked in the alkaline solution for too long, which will cause damage to the sealing surface and the edge of the hole of the ceramic parts, which will affect the sealing performance of the parts.
  • a concentration detector can be used to detect the concentration value of the KOH solution, and the solution is replaced or supplemented according to the detected concentration value so as to make it reach the target concentration value.
  • the ultrasonically cleaned ceramic parts are rinsed 3 to 5 times with pure water.
  • the above step S14 can neutralize the alkaline solution remaining on the ceramic part, so as to reduce the corrosion of the ceramic part by the alkaline solution and prevent the alkaline solution from damaging the sealing surface and the edge of the hole of the ceramic part.
  • the immersion time of immersing the rinsed ceramic piece in the acid solution ranges from greater than or equal to 5 minutes to less than or equal to 10 minutes.
  • the above-mentioned acidic solution is hydrochloric acid or fluoronitric acid solution, wherein the neutralization effect of fluoronitric acid solution and alkaline solution (such as KOH solution) is better.
  • step S14 may not use ultrasonic cleaning.
  • the above step S16 can further dissolve the particles on the ceramic piece.
  • the soaking time of the rinsed ceramic parts in the alkaline solution ranges from 1 hour to 3 hours.
  • ceramics can be effectively dissolved Particles on the parts can prevent the ceramic parts from being soaked in the alkaline solution for too long, which will cause damage to the sealing surface and the edge of the hole of the ceramic parts, which will affect the sealing performance of the parts.
  • the third cleaning process S3 specifically includes the following steps:
  • the range of the flushing time is greater than or equal to 45 minutes and less than or equal to 60 minutes;
  • the above step S32 can fully clean 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 process requirements. Moreover, the damage layer and suspended particles have been removed by the first cleaning process S1 and the second cleaning process S2, which can make up for the inability of ultrasonic cleaning to completely remove the damage layer and suspended particles.
  • the time range for ultrasonic cleaning is greater than or equal to 30 minutes and less than or equal to 60 minutes.
  • the resistivity of the above-mentioned deionized water is greater than or equal to 4M ⁇ cm.
  • step S33 during the soaking process, new deionized water is always introduced into the cleaning tank, and the deionized water in the cleaning tank is discharged in an overflow manner, so that the deionized water can be in a state of circulating flow, Thereby, the cleaning effect can be further improved.
  • the temperature of the deionized water is maintained within a range of greater than or equal to 32°C and less than or equal to 42°C.
  • the purging gas used in the above step S34 includes nitrogen, the purity of which is 99.999%; the range of the included angle between the purging direction of nitrogen and the surface of the ceramic part is greater than or equal to 30°C and less than or equal to 45°C , to avoid particles re-falling on the surface of ceramic parts.
  • the flow process of the cleaning method for ceramic parts in the prior art is as follows: first, soak the ceramic parts in an alkaline degreasing agent for 50min-80min, then put the ceramic parts into deionized water for rinsing (using pressurized deionized water to spray all over the surface of the ceramic piece); after that, immerse the ceramic piece in the acid solution for 5min-10min, then take the ceramic piece out of the solution, and immerse it in deionized water again for the above rinsing, and then immerse it in a Ultrasonic cleaning in deionized water for 10min-15min, then immerse the ceramic parts in deionized water with a resistivity ⁇ 8M ⁇ cm for hot water rinsing, and finally use nitrogen to dry the ceramic parts, and dry the ceramic parts to complete the
  • the ceramic parts cleaning method provided by the embodiment of the present invention includes the above three cleaning processes S1-S3, wherein the first cleaning process S1 includes the above steps S11-S16; the second cleaning process S2 includes the above steps S21-S26; the third cleaning process S3 includes the above steps S31-S34.
  • FIG. 5 is a comparison diagram of damaged layers on ceramic parts obtained by using the cleaning method for ceramic parts in the prior art and the cleaning method for ceramic parts provided by the embodiment of the present invention, respectively.
  • the ceramic parts obtained by the cleaning method of the ceramic parts in the prior art still have a machining damage layer on the surface, as shown in (a) in Figure 5, the thickness of the damage layer It is 10 ⁇ m-30 ⁇ m, and the existence of this damaged layer is one of the important sources of particle generation.
  • the damage layer on the ceramic part obtained by the ceramic part cleaning method provided by the embodiment of the present invention is significantly removed, so that the ceramic part can be avoided. There is a constant stream of falling particles during use on the device.
  • FIG. 6 is a comparison diagram of suspended particles on ceramic parts obtained by using the method for cleaning ceramic parts in the prior art and the method for cleaning ceramic parts provided by the embodiment of the present invention, respectively. Combined with the experimental data and shown in Figure 6, the ceramic parts obtained by the cleaning method of the ceramic parts in the prior art still have suspended particles of 0.2 ⁇ m to 1 ⁇ m on the ceramic surface, as shown in (a) of Figure 6. The white dots on the middle black area are suspended particles.
  • the number of particles per unit area falling on the wafer during the process of the ceramic parts obtained by the cleaning method of the ceramic parts in the prior art is ⁇ 500ea, which is much higher than the particle index (the number of particles per unit area ⁇ 2ea ), in addition, the detection value obtained by measuring the liquid particle count (ie, LPC) on the ceramic piece is 75856 PA/cm 2 .
  • the white dots on the black area in the figure are significantly reduced, so it can be seen that the ceramic parts obtained by the ceramic part cleaning method provided by the embodiment of the present invention , the suspended particles on the ceramic part are significantly reduced, the number of particles per unit area of the ceramic part falling on the wafer during the process is lower than the particle index (the number of particles per unit area ⁇ 2ea), and the LPC obtained by measuring it
  • the detection value of 729PA/cm 2 is far smaller than the above-mentioned LPC detection value of the prior art.
  • the ceramic part in the embodiment of the present invention includes, for example, a ceramic process kit for semiconductor equipment.
  • the ceramic process kit can be components made of ceramic materials such as inner liner, medium window, nozzle, screen tube, main and auxiliary medium cylinders of three-dimensional induction coil, observation window protection cylinder and the like.
  • the method for cleaning ceramic parts divides the cleaning into three cleaning processes, wherein the first cleaning process uses a chemical solution to dissolve the particles on the ceramic parts, and this process can effectively clean the surface of the ceramic parts.
  • the particles in the blind holes, folds and non-welding gaps with large size on the upper surface are cleaned;
  • the second cleaning process uses a designated acid solution to soften and corrode the particles on the ceramic parts and eliminate the damage layer on the ceramic parts, because the existence of the damage layer is One of the important sources of particle generation, the above-mentioned second cleaning process uses the above-mentioned designated acid solution to eliminate the damaged layer on the ceramic parts in a targeted manner, which can effectively remove particles at the source, which can greatly reduce particles compared with the existing technology Quantity;
  • the third cleaning process uses ultrasonic cleaning to clean ceramic parts to remove residual particles and solutions (acidic or alkaline solutions) on ceramic parts, so that ceramic parts can be fully cleaned, and finally the cleaning effect can be effectively improved.

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

Abstract

本发明实施例提供一种陶瓷件清洗方法，包括：第一清洗过程，采用化学溶液溶解陶瓷件上的颗粒；第二清洗过程，采用指定酸性溶液软化腐蚀陶瓷件上的颗粒以及消弭陶瓷件上的损伤层；第三清洗过程，采用超声波清洗的方式清洗陶瓷件，以去除陶瓷件上残留的颗粒和溶液。本发明实施例提供的陶瓷件清洗方法，可以有效去除陶瓷件上的悬浮颗粒和损伤层，从而可以解决陶瓷颗粒数量超标的问题，提高芯片良率。

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
集成电路作为信息产业的基础和核心，是关系着国民经济和社会发展的全局战略性产业。由于集成电路中沟槽和线宽尺寸很小，微小的颗粒都能够对晶圆(如硅片)的工艺结果造成很大的损害，颗粒污染问题已经严重制约集成电路领域向更低技术节点的延伸。颗粒控制能力，也是集成电路工艺中衡量设备稳定性和工艺稳定性的一项重要指标，尤其是目前先进的工艺制程中，对颗粒控制的要求越来越高，这就对集成电路设备提出了更大的挑战。
氧化铝陶瓷是一种以氧化铝(Al 2O 3)为主体的陶瓷材料，是氧化物中最稳定的物质，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，这使得氧化铝陶瓷材料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，这些颗粒一旦在半导体制备工艺过程中掉落在晶圆上，可能会影响工艺结果，例如，不同导线的导通、同一导线的断连、形成空穴而造成更大能耗和发热等。这些颗粒如果不去除，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难以将陶瓷件清洗干净，在清洗后陶瓷件上的损伤层及悬浮颗粒依旧存在，无法满足半导体制备工艺对陶瓷件上颗粒数量的要求。
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上的悬浮颗粒和损伤层，从而可以解决陶瓷颗粒数量超标的问题，提高芯片良率。
为实现本发明的目的而提供一种陶瓷件清洗方法，包括：
第一清洗过程，采用化学溶液溶解陶瓷件上的颗粒；
第二清洗过程，采用指定酸性溶液软化腐蚀所述陶瓷件上的颗粒以及消弭所述陶瓷件上的损伤层；
第三清洗过程，采用超声波清洗的方式清洗所述陶瓷件，以去除所述陶瓷件上残留的颗粒和溶液。
可选的，所述指定酸性溶液包括氟硝酸溶液，所述氟硝酸溶液由氢氟酸溶液、硝酸溶液和纯水混合而成。
可选的，所述氢氟酸溶液、硝酸溶液和电阻率为18MΩ·cm的纯水的配比为1:1:1；其中，
所述氢氟酸溶液包含的氢氟酸的质量分数的范围为大于等于5％，且小于等于15％；所述硝酸溶液包含的硝酸的质量分数的范围为大于等于25％，且小于等于35％。
可选的，在进行第三清洗过程之前，所述第二清洗过程执行至少4次。
可选的，所述第二清洗过程具体包括以下步骤：
S21、采用所述指定酸性溶液对所述陶瓷件进行冲洗；
S22、将采用所述指定酸性溶液冲洗后的所述陶瓷件浸泡在所述指定酸性溶液中；
S23、采用纯水对浸泡后的所述陶瓷件冲洗；
S24、采用纳米材料制作的打磨工具擦拭采用纯水冲洗后的所述陶瓷件；
S25、将擦拭后的所述陶瓷件浸泡在去离子水中，并进行超声波清洗；
S26、采用纯水对超声波清洗后的所述陶瓷件冲洗。
可选的，所述步骤S21中，采用所述指定酸性溶液对所述陶瓷件冲洗至少3次；所述步骤S22中，将采用所述指定酸性溶液冲洗后的所述陶瓷件浸泡在所述指定酸性溶液中的浸泡时间的范围为大于等于10min，且小于等于20min；所述步骤S23中，采用纯水对浸泡后的所述陶瓷件冲洗3次到5次；所述步骤S24中，采用纳米材料制作的打磨工具擦拭采用纯水冲洗后的所述陶瓷件3次到5次；所述步骤S25中，进行超声波清洗的清洗时间的范围为大于等于15min，且小于等于30min；所述步骤S26中，采用纯水对超声波清洗后的所述陶瓷件冲洗的时间的范围为大于等于15min，且小于等于60min。
可选的，所述第一清洗过程具体包括以下步骤：
S11、采用沾有异丙酮溶液的无尘布擦拭所述陶瓷件；
S12、将擦拭后的所述陶瓷件浸泡在碱性溶液中，并进行超声波清洗；
S13、采用纯水对超声波清洗后的所述陶瓷件冲洗；
S14、将冲洗后的所述陶瓷件浸泡在酸性溶液中；
S15、采用纯水对在所述酸性溶液浸泡后的所述陶瓷件冲洗；
S16、将冲洗后的所述陶瓷件浸泡在碱性溶液中。
可选的，所述异丙酮溶液的纯度为99.7％；所述碱性溶液为浓度百分比的范围为大于等于15％，且小于等于20％的KOH溶液，所述碱性溶液的温度的范围为大于等于75℃，且小于等于85℃；所述步骤S12中，进行超声波清洗的时间的范围为大于等于1h，且小于等于3h；所述步骤S13中，采用纯水对超声波清洗后的所述陶瓷件冲洗3次到5次；所述步骤S14中，将冲洗后的所述陶瓷件浸泡在酸性溶液中的浸泡时间的范围为大于等于5min，且小于等于10min；所述步骤S15中，采用纯水对在所述酸性溶液浸泡后的所述陶瓷件冲洗3次到5次；所述步骤S16中，冲洗后的所述陶瓷件浸泡在 碱性溶液中的浸泡时间的范围为大于等于1h，且小于等于3h。
可选的，所述第三清洗过程具体包括以下步骤：
S31、采用纯水对所述陶瓷件冲洗；
S32、将冲洗后的所述陶瓷件浸泡在去离子水中，并进行超声波清洗；
S33、将超声波清洗后的所述陶瓷件浸泡在去离子水中，在浸泡过程中，始终向清洗槽中通入新的去离子水，并采用溢流的方式排出所述清洗槽中的去离子水；
S34、对浸泡后的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，所述步骤S31中，冲洗时间的范围为大于等于45min，且小于等于60min；所述步骤S32中，进行超声波清洗的时间的范围为大于等于30min，且小于等于60min；所述步骤S33中，浸泡时间的范围为大于等于30min，且小于等于60min；所述步骤S33中，所述去离子水的温度维持的范围为大于等于32℃，且小于等于42℃；所述步骤S34中，采用的吹扫气体包括氮气，所述氮气的纯度为99.999％；所述氮气的吹扫方向与所述陶瓷件表面之间的夹角的范围为大于等于30℃，且小于等于45℃。
可选的，所述陶瓷件包括用于半导体设备的陶瓷工艺套件。
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，其将清洗分为三个清洗过程，其中，第一清洗过程采用化学溶液溶解陶瓷件上的颗粒，该过程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；第二清洗过程采用指定酸性溶液软化腐蚀陶瓷件上的颗粒以及消弭陶瓷件上的损伤层，由于该损伤层的存在是颗粒产生的重要源头之一，上述第二清洗过程通过上述指定酸性溶液有针对性地消弭陶瓷件上的损伤层，可以有效在源头上去除颗粒，这与现有技术相比，可以大大减少颗粒数量；第三清洗过程采用 超声波清洗的方式清洗陶瓷件，以去除陶瓷件上残留的颗粒和溶液(酸性或碱性溶液)，从而可以对陶瓷件进行全面清洗，最终可以有效提高清洗效果，解决陶瓷颗粒数量超标的问题，提高芯片良率。
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；
图2为本发明实施例采用的第二清洗过程的流程框图；
图3为本发明实施例采用的第一清洗过程的流程框图；
图4为本发明实施例采用的第三清洗过程的流程框图；
图5为采用现有技术中的陶瓷件清洗方法和本发明实施例提供的陶瓷件清洗方法分别获得的陶瓷件上的损伤层的对比图；
图6为采用现有技术中的陶瓷件清洗方法和本发明实施例提供的陶瓷件清洗方法分别获得的陶瓷件上的悬浮颗粒的对比图。
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。
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工艺套件、陶瓷盖和静电卡盘的陶瓷层等的陶瓷件的清洗。
具体地，请参阅图1，陶瓷件清洗方法包括：
第一清洗过程S1，采用化学溶液溶解陶瓷件上的颗粒；
第一清洗过程S1可以有效对陶瓷件表面上的颗粒进行清洗，尤其是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。
第二清洗过程S2，采用指定酸性溶液软化腐蚀陶瓷件上的颗粒以及消弭陶瓷件上的损伤层；
由于该损伤层的存在是颗粒产生的重要源头之一，上述第二清洗过程S2 通过上述指定酸性溶液有针对性地消弭陶瓷件上的损伤层，可以有效在源头上去除颗粒，这与现有技术相比，可以大大减少颗粒数量。
第三清洗过程S3，采用超声波清洗的方式清洗陶瓷件，以去除陶瓷件上残留的颗粒和溶液。
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。第三清洗过程S3可以对陶瓷件进行全面清洗，以去除陶瓷件上残留的颗粒和溶液(酸性或碱性溶液)，最终可以有效提高清洗效果。
具体地，在上述第二清洗过程S2中，指定酸性溶液包括氟硝酸溶液，该氟硝酸溶液由氢氟酸溶液、硝酸溶液和纯水混合而成，能够软化腐蚀陶瓷件上的颗粒以及消弭陶瓷件上的损伤层。当然，在实际应用中，还可以采用其他任意可起到相同作用的酸性溶液。
为了强化上述氟硝酸溶液对陶瓷件上的损伤层的软化和消弭作用，可选的，上述氢氟酸溶液、硝酸溶液和电阻率为18MΩ·cm的纯水的配比为1:1:1；其中，氢氟酸溶液包含的氢氟酸的质量分数的范围为大于等于5％，且小于等于15％；硝酸溶液包含的硝酸的质量分数的范围为大于等于25％，且小于等于35％。
为了强化上述对陶瓷件上的损伤层的软化和消弭作用，可选的，在进行第三清洗过程S3之前，上述第二清洗过程S2执行至少4次。
下面对上述第二清洗过程S2的具体实施方式进行详细描述。具体地，如图2所示，第二清洗过程S2具体包括以下步骤：
S21、采用上述指定酸性溶液对陶瓷件进行冲洗；
可选的，步骤S21中，采用指定酸性溶液对陶瓷件冲洗至少3次。
S22、将采用上述指定酸性溶液冲洗后的陶瓷件浸泡在上述指定酸性溶液中；
可选的，上述步骤S22中，将采用指定酸性溶液冲洗后的陶瓷件浸泡在 指定酸性溶液中的浸泡时间的范围为大于等于10min，且小于等于20min。
S23、采用纯水对浸泡后的陶瓷件冲洗；
可选的，上述步骤S23中，采用纯水对浸泡后的陶瓷件冲洗3次到5次。
S24、采用纳米材料制作的打磨工具擦拭采用纯水冲洗后的陶瓷件；
可选的，上述步骤S24中，采用纳米材料制作的打磨工具擦拭采用纯水冲洗后的陶瓷件3次到5次。
S25、将擦拭后的陶瓷件浸泡在去离子水中，并进行超声波清洗；
可选的，上述步骤S25中，进行超声波清洗的清洗时间的范围为大于等于15min，且小于等于30min。
S26、采用纯水对超声波清洗后的陶瓷件冲洗。
可选的，上述步骤S26中，采用纯水对超声波清洗后的所述陶瓷件冲洗的时间为大于等于15min，且小于等于60min。
下面对上述第一清洗过程S1的具体实施方式进行详细描述。具体地，如图3所示，第一清洗过程S1具体包括以下步骤：
S11、采用沾有异丙酮(IPA)溶液的无尘布擦拭陶瓷件；
上述步骤S11可以对陶瓷件进行导电，以中和陶瓷件上带电的陶瓷颗粒。
可选的，上述异丙酮溶液的纯度为99.7％。
应当注意的是，在擦拭过程中，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。
S12、将擦拭后的陶瓷件浸泡在碱性溶液中，并进行超声波清洗；
碱性溶液(即用作上述第一清洗过程S1中的化学溶液)可以溶解陶瓷件上的颗粒，结合超声波清洗，可以有效实现颗粒的去除。
为了有效溶解陶瓷件上的颗粒，提高清洗效果，可选的，上述碱性溶液例如为浓度百分比的范围为大于等于15％，且小于等于20％的KOH溶液，该碱性溶液的温度的范围为大于等于75°，且小于等于85°；步骤S12中，进 行超声波清洗的时间的范围为大于等于1h，且小于等于3h，该超声波清洗的时间通过设定在上述范围，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。
S13、采用纯水对超声波清洗后的陶瓷件冲洗；
可选的，上述步骤S13中，采用纯水对超声波清洗后的陶瓷件冲洗3次到5次。
S14、将冲洗后的陶瓷件浸泡在酸性溶液中；
上述步骤S14可以中和残留在陶瓷件上的碱性溶液，以减少碱性溶液对陶瓷件的腐蚀，避免碱性溶液对陶瓷件的密封面和孔边缘处产生损伤。
可选的，上述步骤S14中，将冲洗后的陶瓷件浸泡在酸性溶液中的浸泡时间的范围为大于等于5min，且小于等于10min。
可选的，上述酸性溶液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)的中和作用更优。
另外，上述步骤S14可以不使用超声波清洗。
S15、采用纯水对在所述酸性溶液浸泡后的陶瓷件冲洗；
S16、将冲洗后的陶瓷件浸泡在碱性溶液中。
上述步骤S16可以进一步溶解陶瓷件上的颗粒。
可选的，上述步骤S16中，冲洗后的陶瓷件浸泡在碱性溶液中的浸泡时间的范围为大于等于1h，且小于等于3h，通过该浸泡时间设定在上述范围，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。
下面对上述第三清洗过程S3的具体实施方式进行详细描述。具体地， 如图4所示，第三清洗过程S3具体包括以下步骤：
S31、采用纯水对陶瓷件冲洗；
可选的，上述步骤S31中，冲洗时间的范围为大于等于45min，且小于等于60min；
S32、将冲洗后的陶瓷件浸泡在去离子水中，并进行超声波清洗；
上述步骤S32可以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，利用前面的第一清洗过程S1和第二清洗过程S2已经实现了损伤层和悬浮颗粒的去除，从而可以弥补超声波清洗无法完全去除损伤层和悬浮颗粒的不足。
可选的，上述步骤S32中，进行超声波清洗的时间的范围为大于等于30min，且小于等于60min。
可选的，上述去离子水的电阻率大于等于4MΩ·cm。
S33、将超声波清洗后的陶瓷件浸泡在去离子水中，在浸泡过程中，始终向清洗槽中通入新的去离子水，并采用溢流的方式排出清洗槽中的去离子水；
上述步骤S33中，通过在浸泡过程中，始终向清洗槽中通入新的去离子水，并采用溢流的方式排出该清洗槽中的去离子水，可以使去离子水处于循环流动状态，从而可以进一步提高清洗效果。
可选的，上述步骤S33中，去离子水的温度维持的范围为大于等于32℃，且小于等于42℃。
S34、对浸泡后的陶瓷件进行吹扫，并在吹扫后对陶瓷件进行烘烤。
可选的，上述步骤S34采用的吹扫气体包括氮气，该氮气的纯度为99.999％；氮气的吹扫方向与陶瓷件表面之间的夹角的范围为大于等于30℃，且小于等于45℃，以避免颗粒重新掉落在陶瓷件表面。
可选的，首先使用干燥氮气对陶瓷件进行全面吹扫；然后使用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。
下面将采用现有技术中的陶瓷件清洗方法和本发明实施例提供的陶瓷件清洗方法分别获得的陶瓷件进行对比实验。具体地，现有技术中的陶瓷件清洗方法的流程为：首先将陶瓷件浸入碱性脱脂剂中浸泡50min-80min，再将陶瓷件放入去离子水中漂洗(使用加压去离子水喷淋陶瓷件表面各处)；之后，将陶瓷件浸入酸性溶液中浸泡5min-10min，然后将陶瓷件从溶液中取出，并再次浸入去离子水中进行上述漂洗，之后浸入电阻率≥4MΩ·cm、常温的去离子水中进行超声波清洗10min-15min，之后将陶瓷件浸入电阻率≥8MΩ·cm的去离子水中进行热水浸洗，最后使用氮气吹干陶瓷件，并烘干陶瓷件，完成整个清洗流程。
本发明实施例提供的陶瓷件清洗方法包括上述三个清洗过程S1-S3，其中，第一清洗过程S1包括上述步骤S11-S16；第二清洗过程S2包括上述步骤S21-S26；第三清洗过程S3包括上述步骤S31-S34。
图5为采用现有技术中的陶瓷件清洗方法和本发明实施例提供的陶瓷件清洗方法分别获得的陶瓷件上的损伤层的对比图。结合实验数据和图5所示，采用现有技术中的陶瓷件清洗方法获得的陶瓷件，其表层仍然存在机加工损伤层，如图5中的(a)图所示，该损伤层的厚度为10μm-30μm，而该损伤层的存在是颗粒产生的重要源头之一。与之相比，如图5中的(b)图可以看出，采用本发明实施例提供的陶瓷件清洗方法获得的陶瓷件，该陶瓷件上的损伤层被显著去除，从而可以避免陶瓷件在设备上使用过程中源源不断地掉落颗粒。
图6为采用现有技术中的陶瓷件清洗方法和本发明实施例提供的陶瓷件清洗方法分别获得的陶瓷件上的悬浮颗粒的对比图。结合实验数据和图6所 示，采用现有技术中的陶瓷件清洗方法获得的陶瓷件，其陶瓷表面仍然存在0.2μm～1μm的悬浮颗粒，如图6中的(a)图所示，图中黑色区域上的白色点状物即为悬浮颗粒。此外，现有技术中的陶瓷件清洗方法获得的陶瓷件，其在工艺过程中落在晶圆上的每单位面积的颗粒数量≥500ea，远高于颗粒指标(每单位面积的颗粒数量<2ea)，另外，测量陶瓷件上的液体颗粒计数(即，LPC)获取的检测值为75856PA/cm 2。与之相比，如图6中的(b)图可以看出，图中黑色区域上的白色点状物显著减少，由此可知，采用本发明实施例提供的陶瓷件清洗方法获得的陶瓷件，该陶瓷件上的悬浮颗粒显著减少，该陶瓷件在工艺过程中落在晶圆上的每单位面积的颗粒数量低于颗粒指标(每单位面积的颗粒数量<2ea)，并且测量其LPC获取的检测值为729PA/cm 2，远远小于现有技术的上述LPC检测值。
本发明实施例中的陶瓷件例如包括用于半导体设备的陶瓷工艺套件。该陶瓷工艺套件可以是诸如内衬、介质窗、喷嘴、筛管、立体感应线圈的主、副介质筒、观察窗保护筒等采用陶瓷材料制备的部件。通过提高上述部件的清洗效果，可有效解决陶瓷颗粒数量超标的问题，提高芯片良率。
综上所述，本发明实施例提供的陶瓷件清洗方法，其将清洗分为三个清洗过程，其中，第一清洗过程采用化学溶液溶解陶瓷件上的颗粒，该过程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；第二清洗过程采用指定酸性溶液软化腐蚀陶瓷件上的颗粒以及消弭陶瓷件上的损伤层，由于该损伤层的存在是颗粒产生的重要源头之一，上述第二清洗过程通过上述指定酸性溶液有针对性地消弭陶瓷件上的损伤层，可以有效在源头上去除颗粒，这与现有技术相比，可以大大减少颗粒数量；第三清洗过程采用超声波清洗的方式清洗陶瓷件，以去除陶瓷件上残留的颗粒和溶液(酸性或碱性溶液)，从而可以对陶瓷件进行全面清洗，最终可以有效提高清洗效果，解决陶瓷颗粒数量超标的问题，提高芯片良率。
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 (11)

  1. 一种陶瓷件清洗方法，其特征在于，包括：
    第一清洗过程，采用化学溶液溶解陶瓷件上的颗粒；
    第二清洗过程，采用指定酸性溶液软化腐蚀所述陶瓷件上的颗粒以及消弭所述陶瓷件上的损伤层；
    第三清洗过程，采用超声波清洗的方式清洗所述陶瓷件，以去除所述陶瓷件上残留的颗粒和溶液。
  2. 根据权利要求1所述的陶瓷件清洗方法，其特征在于，所述指定酸性溶液包括氟硝酸溶液，所述氟硝酸溶液由氢氟酸溶液、硝酸溶液和纯水混合而成。
  3. 根据权利要求2所述的陶瓷件清洗方法，其特征在于，所述氢氟酸溶液、硝酸溶液和电阻率为18MΩ·cm的纯水的配比为1:1:1；其中，
    所述氢氟酸溶液包含的氢氟酸的质量分数的范围为大于等于5％，且小于等于15％；所述硝酸溶液包含的硝酸的质量分数的范围为大于等于25％，且小于等于35％。
  4. 根据权利要求1-3任意一项所述的陶瓷件清洗方法，其特征在于，在进行第三清洗过程之前，所述第二清洗过程执行至少4次。
  5. 根据权利要求1-3任意一项所述的陶瓷件清洗方法，其特征在于，所述第二清洗过程具体包括以下步骤：
    S21、采用所述指定酸性溶液对所述陶瓷件进行冲洗；
    S22、将采用所述指定酸性溶液冲洗后的所述陶瓷件浸泡在所述指定酸性溶液中；
    S23、采用纯水对浸泡后的所述陶瓷件冲洗；
    S24、采用纳米材料制作的打磨工具擦拭采用纯水冲洗后的所述陶瓷件；
    S25、将擦拭后的所述陶瓷件浸泡在去离子水中，并进行超声波清洗；
    S26、采用纯水对超声波清洗后的所述陶瓷件冲洗。
  6. 根据权利要求5所述的陶瓷件清洗方法，其特征在于，所述步骤S21中，采用所述指定酸性溶液对所述陶瓷件冲洗至少3次；所述步骤S22中，将采用所述指定酸性溶液冲洗后的所述陶瓷件浸泡在所述指定酸性溶液中的浸泡时间的范围为大于等于10min，且小于等于20min；所述步骤S23中，采用纯水对浸泡后的所述陶瓷件冲洗3次到5次；所述步骤S24中，采用纳米材料制作的打磨工具擦拭采用纯水冲洗后的所述陶瓷件3次到5次；所述步骤S25中，进行超声波清洗的清洗时间的范围为大于等于15min，且小于等于30min；所述步骤S26中，采用纯水对超声波清洗后的所述陶瓷件冲洗的时间的范围为大于等于15min，且小于等于60min。
  7. 根据权利要求1所述的陶瓷件清洗方法，其特征在于，所述第一清洗过程具体包括以下步骤：
    S11、采用沾有异丙酮溶液的无尘布擦拭所述陶瓷件；
    S12、将擦拭后的所述陶瓷件浸泡在碱性溶液中，并进行超声波清洗；
    S13、采用纯水对超声波清洗后的所述陶瓷件冲洗；
    S14、将冲洗后的所述陶瓷件浸泡在酸性溶液中；
    S15、采用纯水对在所述酸性溶液浸泡后的所述陶瓷件冲洗；
    S16、将冲洗后的所述陶瓷件浸泡在碱性溶液中。
  8. 根据权利要求7所述的陶瓷件清洗方法，其特征在于，所述异丙酮溶液的纯度为99.7％；所述碱性溶液为浓度百分比的范围为大于等于15％，且小于等于20％的KOH溶液，所述碱性溶液的温度的范围为大于等于75℃， 且小于等于85℃；所述步骤S12中，进行超声波清洗的时间的范围为大于等于1h，且小于等于3h；所述步骤S13中，采用纯水对超声波清洗后的所述陶瓷件冲洗3次到5次；所述步骤S14中，将冲洗后的所述陶瓷件浸泡在酸性溶液中的浸泡时间的范围为大于等于5min，且小于等于10min；所述步骤S15中，采用纯水对在所述酸性溶液浸泡后的所述陶瓷件冲洗3次到5次；所述步骤S16中，冲洗后的所述陶瓷件浸泡在碱性溶液中的浸泡时间的范围为大于等于1h，且小于等于3h。
  9. 根据权利要求1所述的陶瓷件清洗方法，其特征在于，所述第三清洗过程具体包括以下步骤：
    S31、采用纯水对所述陶瓷件冲洗；
    S32、将冲洗后的所述陶瓷件浸泡在去离子水中，并进行超声波清洗；
    S33、将超声波清洗后的所述陶瓷件浸泡在去离子水中，在浸泡过程中，始终向清洗槽中通入新的去离子水，并采用溢流的方式排出所述清洗槽中的去离子水；
    S34、对浸泡后的所述陶瓷件进行吹扫，并在吹扫后对所述陶瓷件进行烘烤。
  10. 根据权利要求9所述的陶瓷件清洗方法，其特征在于，所述步骤S31中，冲洗时间的范围为大于等于45min，且小于等于60min；所述步骤S32中，进行超声波清洗的时间的范围为大于等于30min，且小于等于60min；所述步骤S33中，浸泡时间的范围为大于等于30min，且小于等于60min；所述步骤S33中，所述去离子水的温度维持的范围为大于等于32℃，且小于等于42℃；所述步骤S34中，采用的吹扫气体包括氮气，所述氮气的纯度为99.999％；所述氮气的吹扫方向与所述陶瓷件表面之间的夹角的范围为大于等于30℃，且小于等于45℃。
  11. 根据权利要求1-10任一所述的陶瓷件清洗方法，其特征在于，所述陶瓷件包括用于半导体设备的陶瓷工艺套件。
PCT/CN2022/092423 2021-05-20 2022-05-12 陶瓷件清洗方法 Ceased WO2022242539A1 (zh)

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