CN100586585C - A method for cleaning the surface of ceramic material parts in a polysilicon etching chamber - Google Patents
A method for cleaning the surface of ceramic material parts in a polysilicon etching chamber Download PDFInfo
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Abstract
本发明所述的多晶硅刻蚀腔室中陶瓷材料零件表面的清洗方法,在清洗过程中采用有机溶剂、碱性溶液、酸性溶液和超纯水对零部件进行清洗,可以有效的去除附着于多晶硅刻蚀腔室中陶瓷材料零件表面的聚合物,且步骤简单方便,清洗效果理想,而且不会对多晶硅刻蚀腔室中陶瓷材料零件造成损伤。应用此方法对半导体工艺一段时间后的多晶硅刻蚀腔室中陶瓷材料零件清洗后,多晶硅刻蚀腔室中陶瓷材料零件表面的污染物完全被除去,且多晶硅刻蚀腔室中陶瓷材料零件表面没有遭到损伤,清洗后的多晶硅刻蚀腔室中陶瓷材料零件完全满足正常工艺的要求,清洗方法完全达到良好的污染物去除效果。The method for cleaning the surface of ceramic material parts in a polysilicon etching chamber according to the present invention uses organic solvents, alkaline solutions, acid solutions and ultrapure water to clean the parts during the cleaning process, which can effectively remove the parts attached to the polysilicon. The polymer on the surface of the ceramic material part in the etching chamber is simple and convenient, the cleaning effect is ideal, and the ceramic material part in the polysilicon etching chamber will not be damaged. After using this method to clean the ceramic material parts in the polysilicon etching chamber after a period of time in the semiconductor process, the pollutants on the surface of the ceramic material parts in the polysilicon etching chamber are completely removed, and the surface of the ceramic material parts in the polysilicon etching chamber Without damage, the cleaned ceramic material parts in the polysilicon etching chamber fully meet the requirements of the normal process, and the cleaning method fully achieves a good pollutant removal effect.
Description
技术领域 technical field
本发明涉及一种零件表面的清洗方法,尤其涉及微电子工艺过程中的一种多晶硅刻蚀腔室中陶瓷材料零件表面的清洗方法。The invention relates to a method for cleaning the surface of a part, in particular to a method for cleaning the surface of a ceramic material part in a polysilicon etching chamber in a microelectronic process.
背景技术 Background technique
随着半导体芯片技术的发展,技术节点已从250nm发展到65nm,甚至45nm以下,硅片的大小也从200mm增加到300mm,在这样的情况下,每片硅片的成本变得越来越高。对加工硅片的工艺要求越来越严格。半导体的加工需要经过多道工序,包括沉积、光刻、刻蚀等,刻蚀工艺是其中较为复杂的一个,等离子体刻蚀过程中等离子体的状态、各项工艺过程参数等与刻蚀结果直接相关。With the development of semiconductor chip technology, the technology node has developed from 250nm to 65nm, or even below 45nm, and the size of silicon wafers has also increased from 200mm to 300mm. Under such circumstances, the cost of each silicon wafer becomes higher and higher . The technological requirements for processing silicon wafers are becoming more and more stringent. The processing of semiconductors needs to go through multiple processes, including deposition, photolithography, etching, etc. The etching process is one of the more complicated ones. The state of the plasma and various process parameters during the plasma etching process are related to the etching results. D.
微电子工艺过程中,半导体多晶硅刻蚀工艺过程中,随着反应地进行,往往会产生很多副产物。副产物在反应室的工艺环境中,会发生一系列的分裂聚合反应,重新组合为成分结构复杂的聚合物。虽然在每次工艺后进行干法清洗,即采用SF6等等离子气体对腔室中的副产物或污染物进行清除,大部分这类副产物可与含SF6等离子体反应而被分子泵和干泵排出反应室,但还有小部分的副产物附着在反应室内壁上。这种附着于内壁上的副产物聚合物膜会随着工艺的继续进行而不断累积,而且这层薄膜稳定性不强,随时会从内壁上脱落下来污染到硅片,而且会影响到腔室得工艺状态,使得刻蚀速率漂移、刻蚀速率均匀性降低。其次还会造成硅片污染、关键尺寸损失及刻蚀缺陷产生。所以需要对反应室内部裸露于工艺环境的零件进行定期清洗。In the process of microelectronics process and semiconductor polysilicon etching process, many by-products are often produced as the reaction proceeds. In the process environment of the reaction chamber, the by-products will undergo a series of split polymerization reactions and recombine into polymers with complex components and structures. Although dry cleaning is carried out after each process, that is, plasma gases such as SF6 are used to remove by-products or pollutants in the chamber, most of these by-products can react with SF6-containing plasma and be removed by molecular pumps and dry pumps. The reaction chamber is discharged, but there is still a small part of by-products attached to the inner wall of the reaction chamber. This by-product polymer film attached to the inner wall will continue to accumulate as the process continues, and this film is not stable, and will fall off from the inner wall at any time to pollute the silicon wafer and affect the chamber. The process state is obtained, so that the etching rate drifts and the uniformity of the etching rate decreases. Secondly, it will also cause silicon wafer contamination, critical dimension loss and etching defects. Therefore, it is necessary to regularly clean the parts exposed to the process environment inside the reaction chamber.
多晶刻蚀腔室中与工艺气体接触的陶瓷材料零件包括静电卡盘(ESC:ElectrostaticChucks),所述的陶瓷材料零件一般只是在零件的表面形成很薄的陶瓷层。通常的清洗手段是采用HNO3+HF浸泡方法进行清洗。清洗过程中,由于零件表面本身的特性与其他金属零件(刻蚀工艺腔体内部直接与等离子接触的零部件一般有三种,石英件,陶瓷件(整体全部是陶瓷),表面处理后的铝件:表面阳极氧化,等离子喷涂。ESC的受过喷涂处理)不同,这种方法在清除聚合物的同时,不仅清除过程耗时耗力,而且容易损伤零件表面,而且对于聚合物清洗效果不甚理想。The ceramic material parts in contact with the process gas in the polycrystalline etching chamber include electrostatic chucks (ESC: Electrostatic Chucks), and the ceramic material parts generally only form a very thin ceramic layer on the surface of the part. The usual cleaning method is to use HNO3+HF soaking method for cleaning. During the cleaning process, due to the characteristics of the surface of the part itself and other metal parts (the parts directly in contact with the plasma inside the etching process chamber, there are generally three types, quartz parts, ceramic parts (the whole is ceramic), aluminum parts after surface treatment : Surface anodic oxidation, plasma spraying. ESC has been subjected to spraying treatment) differently, this method is not only time-consuming and labor-intensive in the removal process, but also easy to damage the surface of the part, and the cleaning effect on the polymer is not ideal.
发明内容Contents of the invention
本发明的目的是提供一种多晶硅刻蚀腔室中陶瓷材料零件表面的清洗方法,可以实现对多晶硅刻蚀腔室中陶瓷材料零件表面的进行湿法清洗,对零件表面损伤小,且完全满足使用要求。The purpose of the present invention is to provide a method for cleaning the surface of ceramic material parts in a polysilicon etching chamber, which can realize wet cleaning of the surface of ceramic material parts in a polysilicon etching chamber, has little damage to the surface of the parts, and fully satisfies Requirements.
本发明的目的是通过以下技术方案实现的:The purpose of the present invention is achieved through the following technical solutions:
一种多晶硅刻蚀腔室中陶瓷材料零件表面的清洗方法,包括以下过程:A method for cleaning the surface of a ceramic material part in a polysilicon etching chamber, comprising the following processes:
A、用有机溶剂清洗零件表面;A. Clean the surface of the parts with organic solvents;
B、用碱性溶液与酸性溶液不分顺序依次清洗零件表面;B. Use alkaline solution and acid solution to clean the surface of parts in sequence;
C、将零件放入超声槽中,清洗设定的超声波清洗时间,进行超声波清洗。C. Put the parts into the ultrasonic tank, clean the set ultrasonic cleaning time, and perform ultrasonic cleaning.
所述过程B在清洗过程中包括下述过程至少一次:The process B includes the following processes at least once in the cleaning process:
用体积含量比为2%~20%的氢氧化四甲基氨TMAH水溶液擦拭、浸泡或喷淋零件表面,不超过设定的TMAH水溶液清洗时间。Wipe, soak or spray the surface of the part with a volume content ratio of 2% to 20% tetramethylammonium hydroxide TMAH aqueous solution, and do not exceed the set TMAH aqueous solution cleaning time.
所述的方法在每次更换溶液进行下一步清洗或用同一溶液进行下一次清洗过程之前和/或之后还包括下述过程:The described method also includes the following process before and/or after the solution is replaced for the next step of cleaning or the same solution is used for the next cleaning process:
用超纯水冲洗或喷淋零件表面;Rinse or spray the surface of the part with ultrapure water;
用洁净的擦拭物擦拭零件,直至擦拭物上无带色的污染物附着;和/或,用洁净的高压气体吹干零件的表面。Wipe the part with a clean wipe until the wipe is free of colored contamination; and/or, blow dry the surface of the part with clean, high-pressure air.
在进行清洗前对零件上无需清洗的表面设置保护层,并在过程C前去除保护层;或者,所述的过程C后,将零件在80℃~120℃环境下烘烤零件进行烘干处理。Before cleaning, set a protective layer on the surface of the part that does not need to be cleaned, and remove the protective layer before process C; or, after the above process C, bake the part at 80 ° C to 120 ° C for drying treatment .
所述的过程A前还包括用双氧水H2O2与水H2O的溶液浸泡零件,再用洁净的擦拭物擦拭零件。Before said process A, it also includes soaking the parts with a solution of hydrogen peroxide H 2 O 2 and water H 2 O, and then wiping the parts with a clean wipe.
所述的过程A包括用有机溶剂擦拭、浸泡或喷淋零件,再用洁净的擦拭物擦拭零件,直至擦拭物上无带色的污染物附着。Said process A includes wiping, soaking or spraying the part with an organic solvent, and then wiping the part with a clean wipe until no colored contaminants adhere to the wipe.
所述的过程B包括以下过程:Described process B comprises following process:
B1、用碱性溶液擦拭、浸泡或喷淋零件,并可重复多次;B1. Wipe, soak or spray parts with alkaline solution, and repeat many times;
B2、用酸性溶液擦拭零件,不超过设定的酸性溶液擦拭时间,并可重复多次。B2. Wipe the parts with an acidic solution, not exceeding the set acidic solution wiping time, and it can be repeated many times.
所述的有机溶剂包括:Described organic solvent comprises:
纯异丙醇,100%,符合SEMI标准C41-1101A的I级标准;或者,Pure isopropanol, 100%, conforming to Class I of SEMI Standard C41-1101A; or,
纯丙酮,满足电子纯级别要求。Pure acetone meets the requirements of electronic purity level.
所述的碱性溶液包括氢氧化氨NH4OH、双氧水H2O2与水H2O,其体积含量比为:NH4OH∶H2O2∶H2O为1~5∶3~10∶5~20。The alkaline solution includes ammonium hydroxide NH 4 OH, hydrogen peroxide H 2 O 2 and water H 2 O, the volume content ratio of which is: NH 4 OH: H 2 O 2 : H 2 O is 1-5:3- 10: 5-20.
所述的酸性溶液包括:Described acid solution comprises:
配方X,包括氢氟酸HF、硝酸HNO3与水H2O,其体积含量比HF∶HNO3∶H2O为0.5~2∶3~10∶50~80;或者,Formula X, including hydrofluoric acid HF, nitric acid HNO 3 and water H 2 O, the volume content ratio of HF:HNO 3 : H 2 O is 0.5~2:3~10:50~80; or,
配方Y,包括盐酸HCl、双氧水H2O2与水H2O,其体积含量比HCl∶H2O2∶H2O为0.5-3∶1-5∶5-15。Formula Y includes hydrochloric acid HCl, hydrogen peroxide H 2 O 2 and water H 2 O, and the volume content ratio of HCl: H 2 O 2 : H 2 O is 0.5-3:1-5:5-15.
由上述本发明提供的技术方案可以看出,本发明所述的多晶硅刻蚀腔室中陶瓷材料零件表面的清洗方法,在清洗过程中采用有机溶剂、碱性溶液、酸性溶液和超纯水对零部件进行清洗,可以有效的去除附着于多晶硅刻蚀腔室中陶瓷材料零件表面的聚合物薄膜,且步骤简单方便,清洗效果理想,而且不会对多晶硅刻蚀腔室中陶瓷材料零件造成损伤。应用此方法对运行半导体多晶刻蚀工艺一定时间的腔室中零件清洗后,多晶硅刻蚀腔室中陶瓷材料零件表面的污染物完全被除去,且多晶硅刻蚀腔室中陶瓷材料零件表面没有遭到损伤,清洗后的多晶硅刻蚀腔室中陶瓷材料零件完全满足正常工艺的要求,达到清洗效果。As can be seen from the technical scheme provided by the above-mentioned invention, the method for cleaning the surface of ceramic material parts in the polysilicon etching chamber of the present invention adopts organic solvents, alkaline solutions, acid solutions and ultrapure water in the cleaning process. Cleaning the parts can effectively remove the polymer film attached to the surface of the ceramic material parts in the polysilicon etching chamber, and the steps are simple and convenient, the cleaning effect is ideal, and it will not cause damage to the ceramic material parts in the polysilicon etching chamber . After using this method to clean the parts in the chamber running the semiconductor polycrystalline etching process for a certain period of time, the pollutants on the surface of the ceramic material parts in the polysilicon etching chamber are completely removed, and the surface of the ceramic material parts in the polysilicon etching chamber is free of After being damaged, the cleaned ceramic material parts in the polysilicon etching chamber fully meet the requirements of the normal process and achieve the cleaning effect.
具体实施方式 Detailed ways
本发明所述的一种多晶硅刻蚀腔室中陶瓷材料零件表面的清洗方法,其核心是是先用有机溶剂清洗零件表面;再用碱性溶液与酸性溶液不分顺序依次清洗零件表面;最后,将零件放入超声槽中,清洗设定的超声波清洗时间,进行超声波清洗零件。达到去除零件表面的沉积物的目的。A method for cleaning the surface of ceramic material parts in a polysilicon etching chamber according to the present invention, the core of which is to first clean the surface of the part with an organic solvent; then use an alkaline solution and an acidic solution to clean the surface of the part in sequence; finally , Put the parts into the ultrasonic tank, clean the set ultrasonic cleaning time, and perform ultrasonic cleaning of the parts. To achieve the purpose of removing deposits on the surface of parts.
在采用此方法清洗之前,我们采用扫描电子显微镜(SEM)、能谱仪(EDS)、二次离子质谱仪(SMIC)对待清洗的零件表面进行分析,发现在使用过一段时间的多晶刻蚀腔室中的零部件的表面的沉积物(污染物)主要包括:有机杂质,金属杂质、电极杂质、硅类杂质、氟化物杂质、表面颗粒。详细来说的话,例如在污染中的氟化物杂质有AlF、TiF等;金属杂质包括Fe、Cr、Ni、Mo、V、Cu等;电极杂质包括W、P等;硅类颗粒包括Si、SiO2等。Before using this method to clean, we used scanning electron microscope (SEM), energy spectrometer (EDS), secondary ion mass spectrometer (SMIC) to analyze the surface of the parts to be cleaned, and found that the polycrystalline etching after using for a period of time The deposits (pollutants) on the surface of the components in the chamber mainly include: organic impurities, metal impurities, electrode impurities, silicon impurities, fluoride impurities, and surface particles. In detail, for example, fluoride impurities in pollution include AlF, TiF, etc.; metal impurities include Fe, Cr, Ni, Mo, V, Cu, etc.; electrode impurities include W, P, etc.; silicon particles include Si, SiO2 wait.
所述的清洗方法具体包括:Described cleaning method specifically comprises:
一、用有机溶剂清洗零件表面的过程1. The process of cleaning the surface of parts with organic solvents
可包含以下的方法或其组合:Can contain the following methods or combinations thereof:
1、用有机溶剂擦拭零件,直至擦拭物上无带色的污染物附着;通常采用无尘布蘸有机溶剂对零件进行擦拭,直至无尘布上无颜色为止。1. Wipe the parts with an organic solvent until no colored pollutants adhere to the wiped object; usually use a dust-free cloth dipped in an organic solvent to wipe the parts until there is no color on the dust-free cloth.
2、用有机溶剂喷淋零件设定的有机溶剂清洗时间(在此指的是喷淋时间,需要设定时间的目的是为了有机溶剂充分溶解零件表面的有机杂质),并可重复多次,且每次的喷淋时间与所用有机溶剂的可相同或不同;通常采用有机溶剂直接喷淋零件的表面,不少于设定的喷淋时间,然后用洁净的高压气体吹干零件的表面或用洁净的无尘布对零件进行擦拭直至无尘布上无颜色为止。2. Spray the part with organic solvent for the set organic solvent cleaning time (here refers to the spraying time, the purpose of setting the time is to fully dissolve the organic impurities on the surface of the part with the organic solvent), and it can be repeated many times, And the spraying time can be the same or different from that of the organic solvent used; usually, the organic solvent is used to directly spray the surface of the part, not less than the set spraying time, and then dry the surface of the part with clean high-pressure gas or Wipe the parts with a clean lint-free cloth until there is no color on the lint-free cloth.
3、用有机溶剂浸泡零件设定的有机溶剂清洗时间(在此指的是浸泡时间,需要设定时间的目的是为了有机溶剂充分溶解零件表面的有机杂质),并可重复多次,且每次的浸泡时间与所用有机溶剂的可相同或不同。通常采用有机溶剂直接浸泡零件,不少于设定的浸泡时间,然后,用洁净的无尘布对零件进行擦拭直至无尘布上无颜色为止或用洁净的高压气体吹干零件。3. Soak the parts with an organic solvent to set the organic solvent cleaning time (here refers to the soaking time, the purpose of setting the time is to fully dissolve the organic impurities on the surface of the parts with the organic solvent), and it can be repeated many times, and each time The soaking time for each time may be the same or different from that of the organic solvent used. Usually use organic solvent to directly soak the parts, not less than the set soaking time, and then wipe the parts with a clean dust-free cloth until there is no color on the dust-free cloth or dry the parts with clean high-pressure air.
由于,目前有机溶液的成本往往较高,常用有机溶剂擦拭零件的方法;而有机溶液浸泡的效果要远远好于喷淋,故在有机溶液的成本允许的情况下,可采用有机溶液浸泡的方法。Because the cost of organic solutions is often high at present, the method of wiping parts with organic solvents is commonly used; and the effect of soaking in organic solutions is far better than spraying, so if the cost of organic solutions allows, the method of soaking in organic solutions can be used. method.
无尘布即为前文所述的擦拭物,其需满足超净室的使用标准。符合CL4(100级无尘室)要求,也可采用擦拭垫作为擦拭物,其需满足半导体行业标准。符合CL4(100级无尘室)要求。The dust-free cloth is the wiper mentioned above, which needs to meet the use standards of the ultra-clean room. Comply with CL4 (Class 100 clean room) requirements, and wipe pads can also be used as wipes, which must meet the semiconductor industry standards. Comply with CL4 (Class 100 clean room) requirements.
这里的有机溶剂为:The organic solvent here is:
纯异丙醇,100%,符合SEMI标准C41-1101A的I级标准;当然也可采用其它的有机溶剂。如纯丙酮,符合电子纯级别要求。Pure isopropanol, 100%, complies with Class I of SEMI standard C41-1101A; of course other organic solvents can also be used. Such as pure acetone, which meets the requirements of electronic purity level.
电子纯是国标中化学试剂的一种级别,简称MOS级,它的电性杂质含量极低。Electronic pure is a grade of chemical reagents in the national standard, referred to as MOS grade, and its content of electrical impurities is extremely low.
另外,需要说明的是在首次用有机溶剂清洗零件前,一般要用超纯水冲洗或喷淋零件表面设定的超纯水清洗时间;然后用洁净的擦拭物擦拭零件,直至擦拭物上无带色的污染物附着;和/或,用洁净的高压气体吹干零件的表面。In addition, it should be noted that before cleaning parts with organic solvents for the first time, it is generally necessary to rinse or spray the surface of the parts with ultrapure water for the set ultrapure water cleaning time; then wipe the parts with a clean wipe until there is no trace on the wipe. Attachment of colored contaminants; and/or, drying the surface of the part with clean, high-pressure air.
当然在每次用有机溶剂清洗零件前与清洗后也可用超纯水冲洗或喷淋零件表面设定的超纯水清洗时间;然后用洁净的擦拭物擦拭零件,直至擦拭物上无带色的污染物附着;和/或,用洁净的高压气体吹干零件的表面。Of course, before and after cleaning the parts with organic solvents, you can also use ultrapure water to rinse or spray the surface of the parts for the set ultrapure water cleaning time; then wipe the parts with a clean wipe until there is no colored stain on the wipe. Contaminants adhere; and/or, dry the surface of the part with clean, high-pressure air.
这里的超纯水UPW的参数要求为25℃下阻抗resistivity≥18Ω/cm。The parameter requirement of ultrapure water UPW here is impedance resistance ≥ 18Ω/cm at 25°C.
另外,在用有机溶剂清洗零件前还包括用双氧水H2O2与水H2O的溶液浸泡零件,再用洁净的擦拭物擦拭零件。In addition, before cleaning the parts with an organic solvent, it also includes soaking the parts with a solution of hydrogen peroxide H 2 O 2 and water H 2 O, and then wiping the parts with a clean wipe.
二、用碱性溶液与酸性溶液不分顺序依次清洗零件表面2. Use alkaline solution and acid solution to clean the surface of parts in sequence
这里需要明确的是,可以先用碱性溶液清洗后用酸性溶液清洗,也可以先用酸性溶液清洗后用碱性溶液清洗。What needs to be clear here is that it can be cleaned with an alkaline solution first and then with an acidic solution, or it can be cleaned with an acidic solution first and then with an alkaline solution.
1、酸性溶液的清洗方法为用无尘布(也可用擦拭垫)蘸酸性溶液擦拭零件不得超过酸性溶液擦拭时间;防止时间过长损伤零件表面。1. The cleaning method of the acid solution is to use a dust-free cloth (wiping pad can also be used) dipped in the acid solution to wipe the parts, and the time for wiping the acid solution should not exceed; prevent the surface of the parts from being damaged if the time is too long.
2、用碱性溶液浸泡或喷淋零件设定的碱性溶液清洗时间;通常采用碱性溶液直接浸泡零件,不少于设定的碱性溶液清洗时间,然后,用洁净的无尘布对零件进行擦拭直至无尘布上无颜色为止。2. Soak or spray parts with alkaline solution for the set alkaline solution cleaning time; usually use alkaline solution to directly soak the parts, not less than the set alkaline solution cleaning time, and then clean the parts with a clean dust-free cloth Wipe the parts until there is no color on the lint-free cloth.
这里的酸性溶液的配方有三种:There are three formulas for the acidic solution here:
第一种所述的碱性溶液包括氢氧化氨NH4OH、双氧水H2O2与水H2O,其体积含量比为:The first described alkaline solution includes ammonium hydroxide NH 4 OH, hydrogen peroxide H 2 O 2 and water H 2 O, the volume ratio of which is:
NH4OH∶H2O2∶H2O为1~5∶3~10∶5~20。The ratio of NH 4 OH: H 2 O 2 : H 2 O is 1-5:3-10:5-20.
所述的酸性溶液包括氢氟酸HF、硝酸HNO3与水H2O,其体积含量比HF∶HNO3∶H2O为0.5~2∶3~10∶50~80;较佳的含量比HF∶HNO3∶H2O为05~1.5∶4~8∶55~70;其优选含量比HF∶HNO3∶H2O为1∶5∶60。The acidic solution includes hydrofluoric acid HF, nitric acid HNO 3 and water H 2 O, the volume content ratio of HF:HNO 3 :H 2 O is 0.5~2:3~10:50~80; the preferred content ratio HF:HNO 3 : H 2 O is 05-1.5:4-8:55-70; the preferred content ratio of HF:HNO 3 :H 2 O is 1:5:60.
第二种the second
所述的酸性溶液包括盐酸HCl、双氧水H2O2与水H2O,其体积含量比HCl∶H2O2∶H2O为05-3∶1-5∶5-15;或者,较佳的含量比HCl∶H2O2∶H2O为1-3∶2-5∶8-12;其优选含量比HCl∶H2O2∶H2O为1∶2∶5。The acidic solution includes hydrochloric acid HCl, hydrogen peroxide H 2 O 2 and water H 2 O, the volume content ratio of HCl: H 2 O 2 : H 2 O is 05-3:1-5:5-15; or, relatively The optimal content ratio of HCl: H 2 O 2 :H 2 O is 1-3:2-5:8-12; the preferred content ratio of HCl:H 2 O 2 : H 2 O is 1:2:5.
这里的碱性溶液的配方包括氢氧化氨NH4OH、双氧水H2O2与水H2O,其体积含量比为NH4OH∶H2O2∶H2O为1~5∶3~10∶5~20;较佳的含量比NH4OH∶H2O2∶H2O为2~4∶4~7∶8~15;其优选含量比NH4OH∶H2O2∶H2O为3∶6∶10。The formula of the alkaline solution here includes ammonium hydroxide NH 4 OH, hydrogen peroxide H 2 O 2 and water H 2 O, the volume ratio of which is NH 4 OH: H 2 O 2 : H 2 O is 1~5:3~ 10:5~20; the preferred content ratio NH 4 OH: H 2 O 2 :H 2 O is 2~4:4~7:8~15; the preferred content ratio NH 4 OH:H 2 O 2 : H 2 O is 3:6:10.
在此清洗过程中还包括下述过程至少一次:This cleaning process also includes at least one of the following procedures:
用体积含量比为2%~20%的氢氧化四甲基氨TMAH水溶液擦拭、浸泡或喷淋零件表面,不超过设定的TMAH水溶液清洗时间;防止时间过长损伤零件表面。Wipe, soak or spray the surface of parts with tetramethylammonium hydroxide TMAH aqueous solution with a volume content ratio of 2% to 20%, and do not exceed the set cleaning time of TMAH aqueous solution; prevent the surface of parts from being damaged if the time is too long.
另外,需要说明的是在每次用有机溶剂清洗零件前或清洗后,一般要用超纯水冲洗或喷淋零件表面设定的超纯水清洗时间;然后用洁净的擦拭物擦拭零件,直至擦拭物上无带色的污染物附着;和/或,用洁净的高压气体吹干零件的表面。In addition, it should be noted that before or after cleaning the parts with organic solvents, it is generally necessary to rinse or spray the surface of the parts with ultra-pure water for the set ultra-pure water cleaning time; then wipe the parts with a clean wipe until No colored contamination adheres to the wipe; and/or, dry the surface of the part with clean, high-pressure air.
这里的超纯水UPW的参数要求为25℃下阻抗resistivity≥18Ω/cm。The parameter requirement of ultrapure water UPW here is impedance resistance ≥ 18Ω/cm at 25°C.
三、用超声波清洗零件3. Use ultrasonic cleaning parts
将零件放入含有超纯水UPW的超声槽中,清洗设定的时间。超声清洗不但能去除零件表面的颗粒,而且能够去除零件内部的颗粒。例如括静电卡盘上的冷却槽、测温探头孔、针孔、He气孔以及相关的微槽。超声清洗后零件上的颗粒的密度少于017Particle/cm2是我们所希望的。Place the parts in an ultrasonic tank containing ultrapure water UPW and clean for the set time. Ultrasonic cleaning can not only remove particles on the surface of parts, but also remove particles inside the parts. For example, it includes cooling grooves, temperature measuring probe holes, pinholes, He gas holes and related microgrooves on the electrostatic chuck. It is our hope that the particle density on the parts after ultrasonic cleaning is less than 017Particle/cm2.
此外,为了保护零件的非氧化面,在进行清洗前需对零件无需清洗的表面(如静电卡盘的电极接触面)设置保护层,也就是粘贴抗化学文腐蚀的胶带;清洗结束后,需去除设置的保护层,也就是揭下抗化学文腐蚀的胶带。In addition, in order to protect the non-oxidized surface of the part, it is necessary to set a protective layer on the surface of the part that does not need to be cleaned (such as the electrode contact surface of the electrostatic chuck) before cleaning, that is, to paste the tape that resists chemical corrosion; after cleaning, it is necessary to Remove the installed protective layer, that is, peel off the tape that resists chemical corrosion.
另外,在进行超声波清洗零件后,需要将零件在80℃~120℃环境下进行烘干处埋。In addition, after ultrasonic cleaning of the parts, the parts need to be dried and buried in an environment of 80°C to 120°C.
可见,本发明的基本清洗方法为:Visible, basic cleaning method of the present invention is:
过程1、使用异丙醇(IPA:100%,符合SEMI标准C41-1101A,1级或更好)来去陶瓷材料零件表面的有机杂质,其他的有机溶剂(如丙酮)如果符合要求也可以使用,但前提是不能造成陶瓷材料零件的再次污染。不过ACE(丙酮)不是最佳有机溶剂,因为ACE对零件的粘结材料有损伤。Process 1. Use isopropanol (IPA: 100%, conforming to SEMI standard C41-1101A, grade 1 or better) to remove organic impurities on the surface of ceramic material parts. Other organic solvents (such as acetone) can also be used if they meet the requirements , but the premise is that it cannot cause re-contamination of ceramic material parts. However, ACE (acetone) is not the best organic solvent, because ACE will damage the bonding material of the parts.
过程2、使用碱性溶液NH4OH(氨水,29%,符合SEMI标准C21-0301,1级或更好)+H2O2(过氧化氢,29%或30%,符合SEMI标准C31-1101,1级或更好)来清洁零件表面。此种碱性溶液可以去除有机杂质、金属杂质和氟化物如TiF。H2O2是一种强氧化剂,具有很高的标准还原电位,它可以把H2O2+NH4OH组成的稀的溶液中金属杂质氧化成高价的金属离子,而金属离子可以和氨水形成较稳定的絡合离子,从而破除去。例如Cu被H2O2氧化成Cu+,之后Cu+和氨水形成Cu+(NH3)4 2+。此种碱性溶液在50℃以上时效果会很好。Process 2. Use alkaline solution NH 4 OH (ammonia water, 29%, meet SEMI standard C21-0301, grade 1 or better) + H 2 O 2 (hydrogen peroxide, 29% or 30%, meet SEMI standard C31- 1101, Class 1 or better) to clean part surfaces. This alkaline solution removes organic impurities, metal impurities and fluorides such as TiF. H 2 O 2 is a strong oxidant with a high standard reduction potential. It can oxidize metal impurities in a dilute solution composed of H 2 O 2 +NH 4 OH into high-priced metal ions, and the metal ions can be combined with ammonia Form a more stable complex ion, thereby breaking away. For example, Cu is oxidized by H 2 O 2 to Cu+, and then Cu+ and ammonia water form Cu+(NH 3 ) 4 2+ . This alkaline solution works well above 50°C.
此溶液一般在60-70℃下使用,H2O2的标准还原电位是:This solution is generally used at 60-70°C, and the standard reduction potential of H2O2 is:
H2O2+2H++2e-=2H2OH 2 O 2 +2H++2e - =2H 2 O
E0=1.776V(相对于H的标准还原电位)E 0 =1.776V (relative to the standard reduction potential of H)
H2O2在稀溶液中的标准还原电位:Standard reduction potential of H2O2 in dilute solution:
HO2 -+H2O+2e-=3OH- HO 2 − +H 2 O+2e − =3OH −
E0=0.878V(相对于H的标准还原电位)E 0 =0.878V (relative to the standard reduction potential of H)
NH4OH能够与金属杂质形成复合离子,例如Cu(NH3)4 2+和Ni(NH3)4 2+。NH4OH的使用能够增加被清洗零件表面的电位,从而能够减少金属离子的再沉积,还能减少化学清洗后被清洗零件表面对金属的吸附。例如Cu的标准还原电位是:NH 4 OH can form complex ions with metal impurities, such as Cu(NH 3 ) 4 2+ and Ni(NH 3 ) 4 2+ . The use of NH 4 OH can increase the potential of the surface of the cleaned parts, thereby reducing the redeposition of metal ions, and can also reduce the adsorption of metals on the surface of the cleaned parts after chemical cleaning. For example, the standard reduction potential of Cu is:
Gu2++2e-=CuGu 2+ +2e - =Cu
E0=0.337V(相对于H的标准还原电位)E 0 =0.337V (relative to the standard reduction potential of H)
过程3、使用酸性溶液HF(氢氟酸,49%,符合SEMI标准C28-0301,1级或更好)+HNO3(硝酸,67%,符合SEMI标准C35-0301,1级或更好)来清洗陶瓷材料零件表面由HF(49%,遵守SEMI标准C28-0301,Grade1或者更好)+HNO3(67%,遵守SEMI标准C41-1101A,Grade1或者更好)组成。此酸性溶液中的HNO3能够去除金属颗粒和电极杂质,HF能够去除硅颗粒,例如和二氧化硅SiO2反应如下:Process 3. Using acidic solution HF (hydrofluoric acid, 49%, conforming to SEMI standard C28-0301, grade 1 or better) + HNO 3 (nitric acid, 67%, conforming to SEMI standard C35-0301, grade 1 or better) To clean the surface of ceramic material parts is composed of HF (49%, comply with SEMI standard C28-0301, Grade1 or better) + HNO 3 (67%, comply with SEMI standard C41-1101A, Grade1 or better). HNO3 in this acidic solution can remove metal particles and electrode impurities, and HF can remove silicon particles, for example, react with silicon dioxide SiO2 as follows:
4HF+SiO2=SiF4+2H2O4HF+SiO 2 =SiF 4 +2H 2 O
6HF+SiO2=H2SiF6+2H2O6HF+SiO 2 =H 2 SiF 6 +2H 2 O
在此酸性溶液中H+和F-浓度较低,所以他有低的反应常数(K1=1.3×10-3mol/l),HNO3可以分解出H+,所以HNO3的含量可以导致甚至更低的F-浓度。因为HF能够侵蚀陶瓷晶界,所以在使用HF去处理陶瓷材料表面时,一定要格外的小心。在清洗过程中被认为HNO3浓度的增加能够提高金属和金属离子的去除。HNO3作为强氧化性酸可以和活跃的金属反应,例如Fe、Ni、Al、Zn,也可和不活跃的金属反应例如Cu。HNO3的标准反应电位:The concentration of H+ and F- in this acidic solution is low, so it has a low reaction constant (K 1 =1.3×10-3mol/l), HNO 3 can decompose H+, so the content of HNO 3 can lead to even lower The F-concentration. Because HF can attack ceramic grain boundaries, extra care must be taken when using HF to treat the surface of ceramic materials. An increase in the concentration of HNO3 during the cleaning process was considered to enhance the removal of metals and metal ions. As a strong oxidizing acid, HNO 3 can react with active metals, such as Fe, Ni, Al, Zn, and also react with inactive metals such as Cu. The standard reaction potential of HNO3:
NO3 -+4H++3e-=NO+2H2ONO 3 - +4H + +3e - =NO+2H 2 O
E0=0.957V(相对于H的标准还原电位)E 0 =0.957V (relative to the standard reduction potential of H)
因为HF与硅颗粒及含Si的杂质反应生成的氟硅酸(H2SiF6)会粘结在零件表面,可在此酸性溶液中加入硫酸铵,其作用是防止氟硅酸粘结在零件表面。Because the fluorosilicic acid (H2SiF6) generated by the reaction of HF with silicon particles and Si-containing impurities will stick to the surface of the part, ammonium sulfate can be added to the acidic solution to prevent the fluorosilicic acid from sticking to the surface of the part.
另一种酸性溶液:由HCl(遵守SEMI标准C28-0301,Grade2或者更好)+H2O2组成。这种酸性溶液被用来去除金属杂质和电极杂质。ESC陶瓷表面的金属杂质有Fe、Ni、Ti、Cu、Al和其他金属颗粒。为了从ESC陶瓷表面去除Cu污染物,对于Cu2+来说这种清洗溶液的PH值应该被控制在6.0左右,而且控制ESC陶瓷表面的反应电位在0.5v或者把标准还原电位控制在较高的值。Another acidic solution: composed of HCl (comply with SEMI standard C28-0301, Grade 2 or better) + H 2 O 2 . This acidic solution is used to remove metal impurities and electrode impurities. Metal impurities on the surface of ESC ceramics include Fe, Ni, Ti, Cu, Al and other metal particles. In order to remove Cu contamination from the ESC ceramic surface, the pH value of this cleaning solution should be controlled at about 6.0 for Cu 2+ , and the reaction potential of the ESC ceramic surface should be controlled at 0.5v or the standard reduction potential should be controlled at a higher level value.
在用以上提到的溶液去擦拭零件表面局部的污点的时候,使用擦拭垫(例如3MTMCE2200)能够帮助移出陶瓷材料零件表面的污染物。When using the above-mentioned solutions to wipe the local stains on the surface of the part, using a wiping pad (such as 3MTMCE2200) can help remove the contaminants on the surface of the ceramic material part.
前面已经提到步骤2与步骤3可以互换。As mentioned above, step 2 and step 3 can be interchanged.
步骤4、超声清洗,此过程不但能去除陶瓷材料零件表面的Particle,而且能够去除陶瓷材料零件零部件的一些孔内部的Particle。例如内衬上的抽气孔。超声清洗后零部件上的Particle的0.3μm的颗粒的密度少于5Particle/cm2是我们所希望的。Step 4, ultrasonic cleaning, this process can not only remove the Particle on the surface of the ceramic material part, but also remove the Particle inside some holes of the ceramic material part. For example, air extraction holes in the lining. After ultrasonic cleaning, it is our hope that the particle density of 0.3μm particles on the parts is less than 5Particle/cm2.
以上是基本步骤,此外在步骤2与步骤3中还包括:The above are the basic steps, and in addition, steps 2 and 3 also include:
步骤5、用TMAH水溶液清洗,此过程主要是用于去除零件表面的可见的污染物,其中TMAH具有较强的去除AlF3能力,而AlF3、AlF2-、AlF-等是刻蚀机中陶瓷材料零件部件与含有卤素元素特别是F等等离子体反应的副产物之一。刻蚀机中的零件表面经常具有较高的粗糙度如40uinch左右,是为了提高吸附刻蚀工艺时产生的颗粒,添加乙醇等有机溶剂,有利于改善此溶液的表面张力,使之能与微观的表面充分接触,去除零件里面的副产物。Step 5. Wash with TMAH aqueous solution. This process is mainly used to remove visible pollutants on the surface of parts. TMAH has a strong ability to remove AlF3, and AlF3, AlF 2- , AlF - , etc. are ceramic materials in the etching machine One of the by-products of the reaction of parts and components with plasma containing halogen elements, especially F. The surface of the parts in the etching machine often has a relatively high roughness, such as about 40uinch, in order to improve the adsorption of particles produced during the etching process. Adding organic solvents such as ethanol is beneficial to improve the surface tension of this solution, so that it can be compared with the microscopic Fully contact the surface to remove by-products inside the part.
此外在步骤4后还包括Also after step 4 include
步骤6、烘干处理,将零件放在80-120℃环境中烘烤30-60mins,之后让其缓慢冷却(随炉冷)到50-60℃。Step 6, drying treatment, put the parts in an environment of 80-120°C and bake for 30-60mins, and then allow them to cool slowly (cooling with the furnace) to 50-60°C.
采用此方法清洗零件表面有多种方案,以下举一例进行说明,但此方法并不局限于此例:There are many options for cleaning the surface of parts by this method, an example is given below to illustrate, but this method is not limited to this example:
在多晶刻蚀腔室中陶瓷表面零件具有代表性的是静电卡盘ESC,新制造的ESC或者是还在使用寿命中但被污染的ESC均需要清洗后才能使用。当刻蚀机台进行工艺时,刻蚀机台腔室内ESC表面会沉积刻蚀过程中的产物,进行一定RF小时后随着腔室内ESC表面沉积物量的增多会改变ESC的工艺状态,从而导关于ESC的问题出现,此时必须对腔室内破污染的ESC陶瓷表面进行处理,以去除其表面的污物恢复ESC正常的工艺条件,满足产品需求。In the polycrystalline etching chamber, the representative ceramic surface part is the electrostatic chuck ESC. The newly manufactured ESC or the contaminated ESC that is still in service life need to be cleaned before use. When the etching machine is performing the process, the surface of the ESC in the chamber of the etching machine will deposit products during the etching process. After a certain RF hour, the process state of the ESC will change as the amount of deposits on the ESC surface in the chamber increases, resulting in The problem about ESC arises. At this time, the decontaminated ESC ceramic surface in the chamber must be treated to remove the dirt on the surface and restore the normal process conditions of ESC to meet product requirements.
经过表面分析,沉积在ESC表面的污物改变了ESC表面的性质,从而导致了ESC在寿命期内提前产生了问题,因此ESC良好的运作是依靠ESC具有清洁的陶瓷表面。ESC表面污染物是来自新ESC的制造过程或者介电刻蚀的工艺过程。通过表面分析手段发现ESC陶瓷表面污染物包括有机物杂质、金属杂质(Fe,Cr,Ni,Mo,V)、氟化物杂质(ALF3,TiF)、电极材料杂质(W,P)、硅材质杂质和表面颗粒(Si,SiO2)。After surface analysis, the dirt deposited on the surface of the ESC changes the properties of the ESC surface, which causes problems in the ESC in advance of its life. Therefore, the good operation of the ESC depends on the ESC having a clean ceramic surface. ESC surface contamination is from the manufacturing process of the new ESC or the process of dielectric etching. Through surface analysis, it is found that the surface pollutants of ESC ceramics include organic impurities, metal impurities (Fe, Cr, Ni, Mo, V), fluoride impurities (ALF3, TiF), electrode material impurities (W, P), silicon material impurities and Surface particles (Si, SiO 2 ).
在多晶刻蚀工艺中所是用的ESC是由一个金属基座(经过阳极氧化处理,或没有经过阳极氧化处理的铝合金)和用来支撑半导体基板的陶瓷表面。这个陶瓷表面部分是碾压烧结成的,包含一个耐高温的电路图形电极层,此层在两个陶瓷层之间,厚度大约05mm(20mil)。这个碾压烧结的陶瓷部分通过粘结材料和ESC基座连接为一体,粘结材料一般为导电的金属(Si,Al等)。基座厚度大约为375mm(15inchs)主要包括RF和DC能量供给装备,支撑硅片的针孔,He背吹通道,控制ESC温度的冷却液循环通路以及测温探头。The ESC used in the poly etch process is composed of a metal base (anodized or not anodized aluminum alloy) and a ceramic surface to support the semiconductor substrate. The ceramic surface part is rolled and sintered and contains a high temperature resistant circuit pattern electrode layer, which is between two ceramic layers and has a thickness of about 0.5mm (20mil). The rolled and sintered ceramic part is integrated with the ESC base through a bonding material, which is generally a conductive metal (Si, Al, etc.). The thickness of the base is about 375mm (15 inches). It mainly includes RF and DC energy supply equipment, pinholes for supporting silicon wafers, He back blowing channels, coolant circulation channels for controlling ESC temperature, and temperature measuring probes.
ESC主要包括Coulombic(库伦型)和Johnsen-Rahbek型两种。库伦型ESC表面是由介电材料组成的表面层,其有高的电阻抗(需要有高的)去产生库伦力。而Johnsen-Rahbek型ESC主要提供较低的电压就可以产生较大的静电吸附力,他的表面一般采用较低阻抗材料(例如掺杂TiO2的AL2O3)。详细来说的话,Johnsen-Rahbek型ESC的介电层表面材料是由Al2O3(94%)+SiO2(4%)+TiO2(1%)+CaO(1%)以及很微量的MgO、Si、Ti、Ca和Mg。因此在用湿法清洗ESC时,Si、Ti、Ca和Mg在一定范围内一般不被认为是污染物。ESC mainly includes Coulombic (Coulomb type) and Johnsen-Rahbek type. The Coulomb-type ESC surface is a surface layer composed of a dielectric material that has a high electrical resistance (needs to be high) to generate the Coulomb force. The Johnsen-Rahbek type ESC mainly provides a relatively low voltage to generate a large electrostatic adsorption force, and its surface generally uses a low-impedance material (such as AL 2 O 3 doped with TiO 2 ). In detail, the dielectric layer surface material of Johnsen-Rahbek type ESC is composed of Al 2 O 3 (94%)+SiO 2 (4%)+TiO 2 (1%)+CaO (1%) and a very small amount of MgO, Si, Ti, Ca and Mg. Therefore, Si, Ti, Ca, and Mg are generally not considered as pollutants within a certain range when cleaning ESCs with wet methods.
另外,当在清洗过程中,用一专用和支架(ESC支撑装置)把ESC支撑起来,同时保证ESC陶瓷表面向下,这样可以防止清洗液和TAMH不会进入ESC的内部通路和损害ESC的连接层。In addition, during the cleaning process, use a special bracket (ESC support device) to support the ESC, and at the same time ensure that the ESC ceramic surface is downward, so as to prevent the cleaning liquid and TAMH from entering the internal passage of the ESC and damaging the connection of the ESC. layer.
本例针对于陶瓷表面零件的具体方法为:The specific method for ceramic surface parts in this example is:
步骤11、首先用抗化学腐蚀胶带保护待清洗的ESC的电极接触面(塑料绝缘和银涂层电极接触面);和ESC边缘粘结层的表面,用IPA擦拭ESC陶瓷表面。Step 11, first protect the electrode contact surface (plastic insulation and silver coating electrode contact surface) of the ESC to be cleaned with an anti-chemical corrosion tape; and the surface of the ESC edge bonding layer, and wipe the ESC ceramic surface with IPA.
步骤12、把ESC浸泡在30%H2O2中20mins,然后用无尘布擦拭ESC表面。如果必要地话,用3MTM white scotch Brite擦拭ESC陶瓷表面上的局部污迹。Step 12. Soak the ESC in 30% H 2 O 2 for 20 minutes, and then wipe the surface of the ESC with a dust-free cloth. If necessary, use 3M™ white scotch Brite to wipe local stains on the ESC ceramic surface.
步骤13、用UPW(超纯水,电阻系数≥18Ω/cm,25℃)喷淋ESC至少5mins,然后用带有过滤器(0.05-0.1μm)的N2枪吹干ESC表面的水。Step 13. Spray the ESC with UPW (ultrapure water, resistivity ≥18Ω/cm, 25°C) for at least 5mins, and then dry the water on the surface of the ESC with a N2 gun with a filter (0.05-0.1μm).
步骤14、把ESC浸入IPA中浸泡20mins,然后用无尘布擦拭ESC用UPW(电阻系数≥18Ω/cm,25℃)喷淋ESC至少5mins,然后用带有过滤器(005-01μm)的N2枪吹干ESC表面的水。Step 14. Soak the ESC in IPA for 20mins, then wipe the ESC with a dust-free cloth, spray the ESC with UPW (resistivity ≥ 18Ω/cm, 25°C) for at least 5mins, and then use a N filter (005-01μm) 2 guns to dry the water on the surface of the ESC.
步骤15、把ESC放在预先准备好的架子上,陶瓷表面冲下。用蘸有HF∶HNO3∶H2O(05-2∶3-10∶50-80)的无尘布擦拭ESC陶瓷表面,控制擦拭时间,防止损毁ESC陶瓷表面。如果ESC陶瓷表面的污染物较难擦拭,也可以同时用3MTM white scotch Brite来擦拭ESC表面。Step 15. Place the ESC on the pre-prepared rack with the ceramic surface flushed down. Wipe the ESC ceramic surface with a dust-free cloth dipped in HF:HNO 3 :H 2 O (05-2:3-10:50-80), and control the wiping time to prevent damage to the ESC ceramic surface. If the pollutants on the ESC ceramic surface are difficult to wipe, you can also use 3MTM white scotch Brite to wipe the ESC surface at the same time.
步骤16、用UPW(电阻系数≥18Ω/cm,25℃)喷淋ESC至少10mins,喷淋时要注意He气孔和一些沟槽的清洗,然后用带有过滤器(005-0.1μm)的N2枪吹干ESC表面的水。Step 16. Spray the ESC with UPW (resistivity ≥ 18Ω/cm, 25°C) for at least 10mins. When spraying, pay attention to the cleaning of He pores and some grooves, and then use the N with filter (005-0.1μm) 2 guns to dry the water on the surface of the ESC.
步骤17、重新把ESC放在支架上,同样陶瓷表面冲下。用0.5-3%的TMAH擦拭ESC陶瓷表面5-10mins(时间长短依靠陶瓷表面氟化物的沉积程度),避免TMAH溶液与金属底座接触。Step 17. Put the ESC on the bracket again, and flush down the ceramic surface. Wipe the ESC ceramic surface with 0.5-3% TMAH for 5-10mins (the length of time depends on the degree of fluoride deposition on the ceramic surface), avoiding the contact of the TMAH solution with the metal base.
步骤18、用UPW(电阻系数≥18Ω/cm,25℃)喷淋ESC至少5mins,喷淋时要注意He气孔和一些沟槽的清洗,然后用带有过滤器(0.05-0.1μm)的N2枪吹干ESC表面的水。Step 18. Spray the ESC with UPW (resistivity ≥ 18Ω/cm, 25°C) for at least 5mins. When spraying, pay attention to the cleaning of He pores and some grooves, and then use a filter (0.05-0.1μm) with N 2 guns to dry the water on the surface of the ESC.
步骤19、把ESC从支架上拿下,浸泡入NH4OH∶H2O2∶H2O(1-53-105-20)中10-20mins,用无尘布或3MTM white scotch Brite擦拭ESC陶瓷表面。Step 19. Remove the ESC from the bracket, soak it in NH 4 OH:H 2 O 2 :H2O (1-53-105-20) for 10-20mins, and wipe the ESC ceramic surface with a dust-free cloth or 3MTM white scotch Brite .
步骤110、用UPW(电阻系数≥18Ω/cm,25℃)喷淋ESC至少5mins,喷淋时要注意He气孔和一些沟槽的清洗,然后用带有过滤器(0.05-0.1μm)的N2枪吹干ESC表面的水。Step 110. Spray the ESC with UPW (resistivity ≥ 18Ω/cm, 25°C) for at least 5mins. When spraying, pay attention to the cleaning of He pores and some grooves, and then use N with a filter (0.05-0.1μm) 2 guns to dry the water on the surface of the ESC.
步骤111、重新把ESC放在支架上,同样陶瓷表面冲下。然后用蘸有HCl∶H2O2∶H2O(0.5-3∶1-5∶5-15)的无尘布擦拭ESC陶瓷表面,控制擦拭时间,防止损毁ESC陶瓷表面。Step 111, put the ESC on the bracket again, and flush down the ceramic surface as well. Then wipe the ESC ceramic surface with a dust-free cloth dipped in HCl: H 2 O 2 :H 2 O (0.5-3:1-5:5-15), and control the wiping time to prevent damage to the ESC ceramic surface.
步骤112、用UPW(电阻系数≥18Ω/cm,25℃)喷淋ESC至少10mins,喷淋时要注意He气孔和一些沟槽的清洗,然后用带有过滤器(0.05-0.1μm)的N2枪吹干ESC表面的水。Step 112. Spray the ESC with UPW (resistivity ≥ 18Ω/cm, 25°C) for at least 10mins. When spraying, pay attention to the cleaning of He pores and some grooves, and then use N with a filter (0.05-0.1μm) 2 guns to dry the water on the surface of the ESC.
步骤113、用ACE和绵签去除ESC边缘的防化学胶带粘结物。Step 113 , use ACE and cotton swab to remove the chemical-proof adhesive tape on the edge of the ESC.
步骤114、然后把ESC移到1000级的洁净室并且测量ESC陶瓷表面的粗糙度。Step 114, then move the ESC to a class 1000 clean room and measure the roughness of the ceramic surface of the ESC.
步骤115、把ESC放入有UPW的超声槽中超声清洗60mins(室温)。ESC的陶瓷表面冲着超声槽底部,但是其的支撑面要高于超声槽的底部,在超声清洗的过程中ESC陶瓷表面绝对不要和超声槽底部接触Step 115, put the ESC into an ultrasonic tank with UPW and ultrasonically clean it for 60 mins (at room temperature). The ceramic surface of the ESC faces the bottom of the ultrasonic tank, but its supporting surface is higher than the bottom of the ultrasonic tank. During the ultrasonic cleaning process, the ceramic surface of the ESC must not touch the bottom of the ultrasonic tank.
步骤116、把ESC拿到100级的清洁间,然后把它放在一个加热灯或者烘箱中在80-120℃烘烤30-60mins,之后让ESC缓慢冷却(随炉冷)到50-60℃。然后检测ESC表面的颗粒度。Step 116. Take the ESC to a clean room of level 100, then put it in a heating lamp or an oven and bake it at 80-120°C for 30-60mins, and then let the ESC cool down slowly (cooling with the furnace) to 50-60°C . The particle size of the ESC surface was then detected.
另外在用以上提到的溶液去擦拭ESC陶瓷表面局部的污点的时候,使用擦拭垫(例如3MTM white scotch Brite)能够帮助移出ESC表面的污染物。In addition, when using the above-mentioned solutions to wipe the local stains on the ESC ceramic surface, using a wiping pad (such as 3MTM white scotch Brite) can help remove the pollutants on the ESC surface.
综上所述,本发明技术方案所述的清洗方法是一种无破坏性的、简易的清洗陶瓷零件表面的有效方法,它主要包括使用有机溶剂、碱性溶液、稀释的酸性溶液和超声清洗的方法去除零件的污染物,该方法不会使陶瓷材料零件的陶瓷层剥落,如果有损伤也是极为微量的,不会导致零部件需要重新进行涂陶瓷处理。In summary, the cleaning method described in the technical solution of the present invention is a non-destructive, simple and effective method for cleaning the surface of ceramic parts. It mainly includes the use of organic solvents, alkaline solutions, diluted acidic solutions and ultrasonic cleaning. This method will not cause the ceramic layer of the ceramic material parts to peel off, and if there is a small amount of damage, it will not cause the parts to need to be re-coated with ceramics.
此方法不但能满足低制程的工艺腔室中陶瓷材料零件的清洗要求,同时也可以满足高制程(0.25μm)工艺腔室的陶瓷材料零件的要求。This method can not only meet the cleaning requirements of ceramic material parts in low-process process chambers, but also meet the requirements of ceramic material parts in high-process (0.25 μm) process chambers.
传统的湿法清洗对零部件本身的损伤较大,而这种清洗方法对零部件本身损伤几乎为零,延长了零部件的使用寿命,节约了设备拥有者的零部件耗材成本。The traditional wet cleaning has a lot of damage to the parts themselves, but this cleaning method has almost zero damage to the parts themselves, which prolongs the service life of the parts and saves the cost of parts and consumables for the equipment owner.
这种湿法清洗方法比传统的多晶刻蚀陶瓷材料零件的清洗方法节约了近1个小时,节约了清洗者的人力成本。This wet cleaning method saves nearly one hour compared with the traditional cleaning method of polycrystalline etched ceramic material parts, and saves the labor cost of the cleaner.
这种湿法清洗方法比传统的多晶刻蚀陶瓷材料零件的清洗方法节约了近30%的药液(如果采用有机溶液喷林的方法,估计会增加药液的使用量),节约了清洗者的化学药液的成本。This wet cleaning method saves nearly 30% of the chemical solution compared with the traditional cleaning method of polycrystalline etched ceramic material parts (if the method of spraying the forest with organic solution is used, it is estimated that the amount of chemical solution used will be increased), saving cleaning The cost of the chemical solution for the operator.
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。The above is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed in the present invention can easily think of changes or Replacement should be covered within the protection scope of the present invention.
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Address after: 100176 Beijing economic and Technological Development Zone, Wenchang Road, No. 8, No. Patentee after: Beijing North China microelectronics equipment Co Ltd Address before: 100016, building 2, block M5, No. 1 East Jiuxianqiao Road, Beijing, Chaoyang District Patentee before: Beifang Microelectronic Base Equipment Proces Research Center Co., Ltd., Beijing |