TWI828146B - Cleaning method for ceramic parts - Google Patents

Cleaning method for ceramic parts Download PDF

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TWI828146B
TWI828146B TW111117910A TW111117910A TWI828146B TW I828146 B TWI828146 B TW I828146B TW 111117910 A TW111117910 A TW 111117910A TW 111117910 A TW111117910 A TW 111117910A TW I828146 B TWI828146 B TW I828146B
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equal
ceramic
cleaning
ceramic piece
solution
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TW111117910A
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TW202245924A (en
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王宏偉
張寶輝
符雅麗
鄭友山
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大陸商北京北方華創微電子裝備有限公司
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/02Cleaning by the force of jets or sprays
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B1/00Cleaning by methods involving the use of tools
    • B08B1/10Cleaning by methods involving the use of tools characterised by the type of cleaning tool
    • B08B1/14Wipes; Absorbent members, e.g. swabs or sponges
    • B08B1/143Wipes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B13/00Accessories or details of general applicability for machines or apparatus for cleaning
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/08Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/10Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/12Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations

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

Abstract

A cleaning method for ceramic parts, which comprises: a first cleaning process, using a chemical solution to dissolve particles on the ceramic parts; In the second cleaning process, the specified acidic solution is used to soften and corrode the particles on the ceramic parts and eliminate the damage layer on the ceramic parts; In the third cleaning process, the ceramic parts are cleaned by ultrasonic cleaning to remove the residual particles and solutions on the ceramic parts. The ceramic parts cleaning method provided by the embodiment of the invention can effectively remove the suspended particles and damage layer on the ceramic parts, so as to solve the problem that the number of ceramic particles exceeds the standard and improve the chip yield.

Description

陶瓷件清洗方法Ceramic parts cleaning method

本發明涉及半導體製造領域,具體地,涉及一種陶瓷件清洗方法。The present invention relates to the field of semiconductor manufacturing, and in particular, to a method for cleaning ceramic parts.

集成電路作為信息產業的基礎和核心,是關係著國民經濟和社會發展的全域戰略性產業。由於集成電路中溝槽和線寬尺寸很小,微小的顆粒都能夠對晶圓(如矽片)的製程結果造成很大的損害,顆粒污染問題已經嚴重制約集成電路領域向更低技術節點的延伸。顆粒控制能力,也是集成電路製程中衡量設備穩定性和製程穩定性的一項重要指標,尤其是目前先進的製程制程中,對顆粒控制的要求越來越高,這就對集成電路設備提出了更大的挑戰。As the foundation and core of the information industry, integrated circuits are a global strategic industry related to the national economy and social development. Due to the small size of trenches and line widths in integrated circuits, tiny particles can cause great damage to the process results of wafers (such as silicon wafers). The problem of particle contamination has seriously restricted the extension of the integrated circuit field to lower technology nodes. . Particle control capability is also an important indicator to measure the stability of equipment and process in integrated circuit manufacturing. Especially in the current advanced manufacturing process, the requirements for particle control are getting higher and higher, which puts forward the requirements for integrated circuit equipment. A bigger challenge.

氧化鋁陶瓷是一種以氧化鋁(Al2O3)為主體的陶瓷材料,是氧化物中最穩定的物質,具有耐高溫、耐腐蝕、耐磨、機械強度高、硬度大、電絕緣性高與介電損耗低等的優勢,這使得氧化鋁陶瓷材料越來越多地應用在半導體設備中。但是,這種材料在造粒、燒結和機加工等的成型過程中不可避免地會在表面產生一些粉末狀的顆粒,這些顆粒一旦在半導體製備製程過程中掉落在晶圓上,可能會影響製程結果,例如,不同導線的導通、同一導線的斷連、形成空穴而造成更大能耗和發熱等。這些顆粒如果不去除,會嚴重影響到製程結果和晶片良率。Alumina ceramics is a ceramic material based on aluminum oxide (Al2O3). It is the most stable substance among oxides and has high temperature resistance, corrosion resistance, wear resistance, high mechanical strength, high hardness, high electrical insulation and dielectric properties. The advantages of low loss make alumina ceramic materials increasingly used in semiconductor equipment. However, during the molding process of granulation, sintering and machining, this material will inevitably produce some powdery particles on the surface. Once these particles fall on the wafer during the semiconductor preparation process, they may affect Process results, such as conduction of different wires, disconnection of the same wire, formation of holes, resulting in greater energy consumption and heat generation, etc. If these particles are not removed, they will seriously affect the process results and wafer yield.

為了去除陶瓷件上的顆粒,就需要對陶瓷件進行清洗,但是,現有的陶瓷件清洗方法難以將陶瓷件清洗乾淨,在清洗後陶瓷件上的損傷層及懸浮顆粒依舊存在,無法滿足半導體製備製程對陶瓷件上顆粒數量的要求。In order to remove particles on ceramic parts, the ceramic parts need to be cleaned. However, the existing ceramic parts cleaning methods are difficult to clean the ceramic parts. After cleaning, the damaged layer and suspended particles on the ceramic parts still exist, which cannot meet the needs of semiconductor manufacturing. The manufacturing process requires the number of particles on ceramic parts.

本發明旨在至少解決現有技術中存在的技術問題之一,提出了一種陶瓷件清洗方法,其可以有效去除陶瓷件上的懸浮顆粒和損傷層,從而可以解決陶瓷顆粒數量超標的問題,提高晶片良率。The present invention aims to solve at least one of the technical problems existing in the prior art. It proposes a method for cleaning ceramic parts, which can effectively remove suspended particles and damaged layers on ceramic parts, thereby solving the problem of excessive number of ceramic particles and improving wafer quality. Yield.

為實現本發明的目的而提供一種陶瓷件清洗方法,包括:第一清洗過程,採用化學溶液溶解陶瓷件上的顆粒;第二清洗過程,採用指定酸性溶液軟化腐蝕所述陶瓷件上的顆粒以及消弭所述陶瓷件上的損傷層;第三清洗過程,採用超聲波清洗的方式清洗所述陶瓷件,以去除所述陶瓷件上殘留的顆粒和溶液。In order to achieve the purpose of the present invention, a method for cleaning ceramic parts is provided, which includes: a first cleaning process, using a chemical solution to dissolve particles on the ceramic parts; a second cleaning process, using a designated acidic solution to soften and corrode the particles on the ceramic parts; Eliminate the damaged layer on the ceramic piece; in the third cleaning process, use ultrasonic cleaning to clean the ceramic piece to remove residual particles and solution on the ceramic piece.

可選的,所述指定酸性溶液包括氟硝酸溶液,所述氟硝酸溶液由氫氟酸溶液、硝酸溶液和純水混合而成。Optionally, the specified acidic solution includes a fluorine nitric acid solution, which is a mixture of hydrofluoric acid solution, nitric acid solution and pure water.

可選的,所述氫氟酸溶液、硝酸溶液和電阻率為18MΩ•cm的純水的配比為1:1:1;其中,所述氫氟酸溶液包含的氫氟酸的質量分數的範圍為大於等於5% ,且小於等於15%;所述硝酸溶液包含的硝酸的質量分數的範圍為大於等於25%,且小於等於35%。Optionally, the ratio of the hydrofluoric acid solution, nitric acid solution and pure water with a resistivity of 18 MΩ·cm is 1:1:1; wherein the hydrofluoric acid solution contains a mass fraction of hydrofluoric acid The range 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%.

可選的,在進行第三清洗過程之前,所述第二清洗過程執行至少4次。Optionally, before performing the third cleaning process, the second cleaning process is performed at least 4 times.

可選的,所述第二清洗過程具體包括以下步驟:S21、採用所述指定酸性溶液對所述陶瓷件進行沖洗;S22、將採用所述指定酸性溶液沖洗後的所述陶瓷件浸泡在所述指定酸性溶液中;S23、採用純水對浸泡後的所述陶瓷件沖洗;S24、採用納米材料製作的打磨工具擦拭採用純水沖洗後的所述陶瓷件;S25、將擦拭後的所述陶瓷件浸泡在去離子水中,並進行超聲波清洗;S26、採用純水對超聲波清洗後的所述陶瓷件沖洗。Optionally, the second cleaning process specifically includes the following steps: S21. Rinse the ceramic piece with the specified acidic solution; S22. Soak the ceramic piece rinsed with the specified acidic solution in the specified acidic solution. in the specified acidic solution; S23. Use pure water to rinse the soaked ceramic pieces; S24. Use a grinding tool made of nanomaterials to wipe the ceramic pieces rinsed with pure water; S25. Clean the wiped ceramic pieces. The ceramic parts are soaked in deionized water and ultrasonic cleaned; S26, use pure water to rinse the ceramic parts after ultrasonic cleaning.

可選的,所述步驟S21中,採用所述指定酸性溶液對所述陶瓷件沖洗至少3次;所述步驟S22中,將採用所述指定酸性溶液沖洗後的所述陶瓷件浸泡在所述指定酸性溶液中的浸泡時間的範圍為大於等於10min,且小於等於20min;所述步驟S23中,採用純水對浸泡後的所述陶瓷件沖洗3次到5次;所述步驟S24中,採用納米材料製作的打磨工具擦拭採用純水沖洗後的所述陶瓷件3次到5次;所述步驟S25中,進行超聲波清洗的清洗時間的範圍為大於等於15min,且小於等於30min;所述步驟S26中,採用純水對超聲波清洗後的所述陶瓷件沖洗的時間的範圍為大於等於15min,且小於等於60min。Optionally, in step S21, the ceramic piece is rinsed with the designated acidic solution at least 3 times; in step S22, the ceramic piece rinsed with the designated acidic solution is soaked in the The range of the 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, use pure water to rinse the soaked ceramic piece 3 to 5 times; in the step S24, use The polishing tool made of nanomaterials wipes the ceramic piece washed with pure water 3 to 5 times; in the step S25, 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 steps In S26, the range of time for rinsing the ceramic piece after ultrasonic cleaning with pure water is greater than or equal to 15 minutes and less than or equal to 60 minutes.

可選的,所述第一清洗過程具體包括以下步驟:S11、採用沾有異丙酮溶液的無塵布擦拭所述陶瓷件;S12、將擦拭後的所述陶瓷件浸泡在鹼性溶液中,並進行超聲波清洗;S13、採用純水對超聲波清洗後的所述陶瓷件沖洗;S14、將沖洗後的所述陶瓷件浸泡在酸性溶液中;S15、採用純水對在所述酸性溶液浸泡後的所述陶瓷件沖洗;S16、將沖洗後的所述陶瓷件浸泡在鹼性溶液中。Optionally, the first cleaning process specifically includes the following steps: S11, wipe the ceramic piece with a lint-free cloth moistened with isopropyltone solution; S12, soak the wiped ceramic piece in an alkaline solution. And perform ultrasonic cleaning; S13, use pure water to rinse the ceramic parts after ultrasonic cleaning; S14, soak the rinsed ceramic parts in an acidic solution; S15, use pure water to rinse the ceramic parts after immersing in the acidic solution Rinse the ceramic piece; S16. Soak the rinsed ceramic piece in an alkaline solution.

可選的,所述異丙酮溶液的純度為99.7%;所述鹼性溶液為濃度百分比的範圍為大於等於15%,且小於等於20%的KOH溶液,所述鹼性溶液的溫度的範圍為大於等於75℃,且小於等於85℃;所述步驟S12中,進行超聲波清洗的時間的範圍為大於等於1h,且小於等於3h;所述步驟S13中,採用純水對超聲波清洗後的所述陶瓷件沖洗3次到5次;所述步驟S14中,將沖洗後的所述陶瓷件浸泡在酸性溶液中的浸泡時間的範圍為大於等於5min,且小於等於10min;所述步驟S15中,採用純水對在所述酸性溶液浸泡後的所述陶瓷件沖洗3次到5次;所述步驟S16中,沖洗後的所述陶瓷件浸泡在鹼性溶液中的浸泡時間的範圍為大於等於1h,且小於等於3h。Optionally, the purity of the isopropyl ketone solution is 99.7%; the alkaline solution is a KOH solution with a concentration percentage range of greater than or equal to 15% and less than or equal to 20%; the temperature range of the alkaline solution is Greater than or equal to 75°C and less than or equal to 85°C; in step S12, the time range for ultrasonic cleaning is greater than or equal to 1 hour and less than or equal to 3 hours; in step S13, pure water is used to clean the ultrasonic cleaning product Rinse the ceramic pieces 3 to 5 times; in the step S14, the soaking time of the rinsed ceramic pieces in the acidic solution ranges from 5 minutes to 10 minutes; in the step S15, use Pure water rinses the ceramic piece after being soaked in the acidic solution 3 to 5 times; in step S16, the range of the soaking time of the rinsed ceramic piece in the alkaline solution is greater than or equal to 1 hour , and less than or equal to 3h.

可選的,所述第三清洗過程具體包括以下步驟:S31、採用純水對所述陶瓷件沖洗;S32、將沖洗後的所述陶瓷件浸泡在去離子水中,並進行超聲波清洗;S33、將超聲波清洗後的所述陶瓷件浸泡在去離子水中,在浸泡過程中,始終向清洗槽中通入新的去離子水,並採用溢流的方式排出所述清洗槽中的去離子水;S34、對浸泡後的所述陶瓷件進行吹掃,並在吹掃後對所述陶瓷件進行烘烤。Optionally, the third cleaning process specifically includes the following steps: S31. Rinse the ceramic parts with pure water; S32. Soak the rinsed ceramic parts in deionized water and perform ultrasonic cleaning; S33. Soak the ultrasonically cleaned ceramic pieces in deionized water. During the soaking process, always introduce new deionized water into the cleaning tank, and use overflow to discharge the deionized water in the cleaning tank; S34. Purge the soaked ceramic piece, and bake the ceramic piece after purging.

可選的,所述步驟S31中,沖洗時間的範圍為大於等於45min,且小於等於60min;所述步驟S32中,進行超聲波清洗的時間的範圍為大於等於30min,且小於等於60min;所述步驟S33中,浸泡時間的範圍為大於等於30min,且小於等於60min;所述步驟S33中,所述去離子水的溫度維持的範圍為大於等於32℃,且小於等於42℃;所述步驟S34中,採用的吹掃氣體包括氮氣,所述氮氣的純度為99.999%;所述氮氣的吹掃方向與所述陶瓷件表面之間的夾角的範圍為大於等於30℃,且小於等於45℃。Optionally, in step S31, the range of flushing time is greater than or equal to 45 minutes and less than or equal to 60 minutes; in step S32, the range of ultrasonic cleaning time is greater than or equal to 30 minutes and less than or equal to 60 minutes; the steps In S33, the soaking time range is greater than or equal to 30 minutes and less than or equal to 60 minutes; in the step S33, the temperature maintenance range 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 purge gas used includes nitrogen, the purity of the nitrogen is 99.999%; the range of the angle between the purge direction of the nitrogen and the surface of the ceramic piece is greater than or equal to 30°C and less than or equal to 45°C.

可選的,所述陶瓷件包括用於半導體設備的陶瓷製程套件。Optionally, the ceramic part includes a ceramic process kit for semiconductor equipment.

本發明具有以下有益效果:The invention has the following beneficial effects:

本發明實施例提供的陶瓷件清洗方法,其將清洗分為三個清洗過程,其中,第一清洗過程採用化學溶液溶解陶瓷件上的顆粒,該過程可以有效對陶瓷件表面上尺寸較大的盲孔、褶皺及非焊接縫隙處的顆粒進行清洗;第二清洗過程採用指定酸性溶液軟化腐蝕陶瓷件上的顆粒以及消弭陶瓷件上的損傷層,由於該損傷層的存在是顆粒產生的重要源頭之一,上述第二清洗過程通過上述指定酸性溶液有針對性地消弭陶瓷件上的損傷層,可以有效在源頭上去除顆粒,這與現有技術相比,可以大大減少顆粒數量;第三清洗過程採用超聲波清洗的方式清洗陶瓷件,以去除陶瓷件上殘留的顆粒和溶液(酸性或鹼性溶液),從而可以對陶瓷件進行全面清洗,最終可以有效提高清洗效果,解決陶瓷顆粒數量超標的問題,提高晶片良率。The ceramic parts cleaning method provided by the embodiment of the present invention divides the cleaning into three cleaning processes. The first cleaning process uses a chemical solution to dissolve particles on the ceramic parts. This process can effectively remove larger particles on the surface of the ceramic parts. The particles in blind holes, wrinkles and non-welded gaps are cleaned; the second cleaning process uses designated acidic solutions to soften the particles on the corroded ceramic parts and eliminate the damaged layer on the ceramic parts, because the existence of this damaged layer is an important source of particle generation. One, the above-mentioned second cleaning process uses the above-mentioned designated acidic 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 the number of particles compared with the existing technology; the third cleaning process Ultrasonic cleaning is used to clean ceramic parts to remove residual particles and solutions (acidic or alkaline solutions) on the ceramic parts, so that the ceramic parts can be fully cleaned, which can ultimately effectively improve the cleaning effect and solve the problem of excessive number of ceramic particles. , improve wafer yield.

以下揭露提供用於實施本揭露之不同構件之許多不同實施例或實例。下文描述組件及配置之特定實例以簡化本揭露。當然,此等僅為實例且非意欲限制。舉例而言,在以下描述中之一第一構件形成於一第二構件上方或上可包含其中該第一構件及該第二構件經形成為直接接觸之實施例,且亦可包含其中額外構件可形成在該第一構件與該第二構件之間,使得該第一構件及該第二構件可不直接接觸之實施例。另外,本揭露可在各個實例中重複參考數字及/或字母。此重複出於簡化及清楚之目的且本身不指示所論述之各個實施例及/或組態之間的關係。The following disclosure provides many different embodiments or examples of different means for implementing the disclosure. Specific examples of components and configurations are described below to simplify the present disclosure. Of course, these are examples only and are not intended to be limiting. For example, the following description in which a first member is formed over or on a second member may include embodiments in which the first member and the second member are formed in direct contact, and may also include embodiments in which additional members Embodiments may be formed between the first member and the second member such that the first member and the second member may not be in direct contact. Additionally, the present disclosure may repeat reference numbers and/or letters in various instances. This repetition is for simplicity and clarity and does not inherently indicate a relationship between the various embodiments and/or configurations discussed.

此外,為便於描述,諸如「下面」、「下方」、「下」、「上方」、「上」及類似者之空間相對術語可在本文中用於描述一個元件或構件與另一(些)元件或構件之關係,如圖中圖解說明。空間相對術語意欲涵蓋除在圖中描繪之定向以外之使用或操作中之裝置之不同定向。設備可以其他方式定向(旋轉90度或按其他定向)且因此可同樣解釋本文中使用之空間相對描述詞。In addition, for ease of description, spatially relative terms such as “below,” “below,” “lower,” “above,” “upper,” and the like may be used herein to describe one element or component in relation to another(s). The relationship between components or components, as illustrated in the figure. Spatially relative terms are intended to cover different orientations of the device in use or operation other than the orientation depicted in the figures. The device may be otherwise oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.

儘管陳述本揭露之寬泛範疇之數值範圍及參數係近似值,然儘可能精確地報告特定實例中陳述之數值。然而,任何數值固有地含有必然由於見於各自測試量測中之標準偏差所致之某些誤差。再者,如本文中使用,術語「大約」通常意謂在一給定值或範圍之10%、5%、1%或0.5%內。替代地,術語「大約」意謂在由此項技術之一般技術者考量時處於平均值之一可接受標準誤差內。除在操作/工作實例中以外,或除非以其他方式明確指定,否則諸如針對本文中揭露之材料之數量、時間之持續時間、溫度、操作條件、數量之比率及其類似者之全部數值範圍、數量、值及百分比應被理解為在全部例項中由術語「大約」修飾。相應地,除非相反地指示,否則本揭露及隨附發明申請專利範圍中陳述之數值參數係可根據需要變化之近似值。至少,應至少鑑於所報告有效數位之數目且藉由應用普通捨入技術解釋各數值參數。範圍可在本文中表達為從一個端點至另一端點或在兩個端點之間。本文中揭露之全部範圍包含端點,除非另有指定。Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the disclosure are approximations, the values stated in the specific examples are reported as precisely as possible. Any numerical value, however, inherently contains certain errors necessarily resulting from the standard deviation found in their respective testing measurements. Furthermore, as used herein, the term "about" generally means within 10%, 5%, 1% or 0.5% of a given value or range. Alternatively, the term "approximately" means within one acceptable standard error of the mean when considered by one of ordinary skill in the art. Except in operating/working examples, or unless otherwise expressly specified, all numerical ranges such as quantities, durations of time, temperatures, operating conditions, ratios of quantities, and the like for materials disclosed herein, Quantities, values and percentages should be understood to be modified in all instances by the term "approximately". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the patent claims of this disclosure and accompanying invention claims are approximations that may vary as necessary. At a minimum, each numerical parameter should be interpreted in light of the number of reported significant digits and by applying ordinary rounding techniques. Ranges may be expressed herein as from one endpoint to the other endpoint or between two endpoints. All ranges disclosed herein include endpoints unless otherwise specified.

本發明實施例提供一種陶瓷件清洗方法,其可以應用於半導體設備中製程腔室的製程套件、陶瓷蓋和靜電卡盤的陶瓷層等的陶瓷件的清洗。Embodiments of the present invention provide a method for cleaning ceramic parts, which can be applied to cleaning ceramic parts such as process kits, ceramic covers, and ceramic layers of electrostatic chucks in process chambers in semiconductor equipment.

具體地,請參閱圖1,陶瓷件清洗方法包括:Specifically, please refer to Figure 1. Ceramic parts cleaning methods include:

第一清洗過程S1,採用化學溶液溶解陶瓷件上的顆粒;In the first cleaning process S1, a chemical solution is used to dissolve particles on the ceramic parts;

第一清洗過程S1可以有效對陶瓷件表面上的顆粒進行清洗,尤其是陶瓷件表面上尺寸較大的盲孔、褶皺及非焊接縫隙處的顆粒進行清洗。The first cleaning process S1 can effectively clean particles on the surface of ceramic parts, especially particles in large blind holes, wrinkles and non-welding gaps on the surface of ceramic parts.

第二清洗過程S2,採用指定酸性溶液軟化腐蝕陶瓷件上的顆粒以及消弭陶瓷件上的損傷層;The second cleaning process S2 uses a designated acidic solution to soften the particles on the corroded ceramic parts and eliminate the damaged layer on the ceramic parts;

由於該損傷層的存在是顆粒產生的重要源頭之一,上述第二清洗過程S2通過上述指定酸性溶液有針對性地消弭陶瓷件上的損傷層,可以有效在源頭上去除顆粒,這與現有技術相比,可以大大減少顆粒數量。Since the existence of this damaged layer is one of the important sources of particle generation, the above-mentioned second cleaning process S2 uses the above-mentioned specified acid solution to eliminate the damaged layer on the ceramic parts in a targeted manner, which can effectively remove particles at the source, which is consistent with the existing technology. In comparison, the number of particles can be greatly reduced.

第三清洗過程S3,採用超聲波清洗的方式清洗陶瓷件,以去除陶瓷件上殘留的顆粒和溶液。In the third cleaning process S3, ultrasonic cleaning is used to clean the ceramic parts to remove residual particles and solution on the ceramic parts.

所謂超聲波清洗,是指通過超聲波震盪產生的水波清洗陶瓷件上的顆粒。第三清洗過程S3可以對陶瓷件進行全面清洗,以去除陶瓷件上殘留的顆粒和溶液(酸性或鹼性溶液),最終可以有效提高清洗效果。The so-called ultrasonic cleaning refers to cleaning particles on ceramic parts through water waves generated by ultrasonic vibration. The third cleaning process S3 can comprehensively clean the ceramic parts to remove residual particles and solutions (acidic or alkaline solutions) on the ceramic parts, which can ultimately effectively improve the cleaning effect.

具體地,在上述第二清洗過程S2中,指定酸性溶液包括氟硝酸溶液,該氟硝酸溶液由氫氟酸溶液、硝酸溶液和純水混合而成,能夠軟化腐蝕陶瓷件上的顆粒以及消弭陶瓷件上的損傷層。當然,在實際應用中,還可以採用其他任意可起到相同作用的酸性溶液。Specifically, in the above-mentioned second cleaning process S2, the designated acidic solution includes a fluorine nitric acid solution, which is a mixture of hydrofluoric acid solution, nitric acid solution and pure water, which can soften the particles on the corroded ceramic parts and eliminate the corrosion of the ceramics. Damage layer on the part. Of course, in practical applications, any other acidic solution that can play the same role can also be used.

為了強化上述氟硝酸溶液對陶瓷件上的損傷層的軟化和消弭作用,可選的,上述氫氟酸溶液、硝酸溶液和電阻率為18MΩ•cm的純水的配比為1:1:1;其中,氫氟酸溶液包含的氫氟酸的質量分數的範圍為大於等於5% ,且小於等於15%;硝酸溶液包含的硝酸的質量分數的範圍為大於等於25%,且小於等於35%。In order to strengthen the softening and elimination effect of the above-mentioned hydrofluoric acid solution on the damaged layer on the ceramic parts, optionally, the ratio of the above-mentioned hydrofluoric acid solution, nitric acid solution and pure water with a resistivity of 18MΩ·cm is 1:1:1 ; Among them, 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%. .

為了強化上述對陶瓷件上的損傷層的軟化和消弭作用,可選的,在進行第三清洗過程S3之前,上述第二清洗過程S2執行至少4次。In order to enhance the above-mentioned softening and elimination effect on the damaged layer on the ceramic piece, optionally, before performing the third cleaning process S3, the above-mentioned second cleaning process S2 is performed at least 4 times.

下面對上述第二清洗過程S2的具體實施方式進行詳細描述。具體地,如圖2所示,第二清洗過程S2具體包括以下步驟:The specific implementation of the above second cleaning process S2 will be described in detail below. Specifically, as shown in Figure 2, the second cleaning process S2 specifically includes the following steps:

S21、採用上述指定酸性溶液對陶瓷件進行沖洗;S21. Use the above specified acid solution to rinse the ceramic parts;

可選的,步驟S21中,採用指定酸性溶液對陶瓷件沖洗至少3次。Optionally, in step S21, use the specified acidic solution to rinse the ceramic piece at least 3 times.

S22、將採用上述指定酸性溶液沖洗後的陶瓷件浸泡在上述指定酸性溶液中;S22. Soak the ceramic pieces rinsed with the above specified acidic solution in the above specified acidic solution;

可選的,上述步驟S22中,將採用指定酸性溶液沖洗後的陶瓷件浸泡在指定酸性溶液中的浸泡時間的範圍為大於等於10min,且小於等於20min。Optionally, in the above step S22, the soaking time range of the ceramic piece rinsed with the designated acidic solution in the designated acidic solution is greater than or equal to 10 minutes and less than or equal to 20 minutes.

S23、採用純水對浸泡後的陶瓷件沖洗;S23. Use pure water to rinse the soaked ceramic parts;

可選的,上述步驟S23中,採用純水對浸泡後的陶瓷件沖洗3次到5次。Optionally, in the above step S23, pure water is used to rinse the soaked ceramic piece 3 to 5 times.

S24、採用納米材料製作的打磨工具擦拭採用純水沖洗後的陶瓷件;S24. Use a grinding tool made of nanomaterials to wipe the ceramic parts after being rinsed with pure water;

可選的,上述步驟S24中,採用納米材料製作的打磨工具擦拭採用純水沖洗後的陶瓷件3次到5次。Optionally, in the above step S24, a polishing tool made of nanomaterials is used to wipe the ceramic piece washed with pure water 3 to 5 times.

S25、將擦拭後的陶瓷件浸泡在去離子水中,並進行超聲波清洗;S25. Soak the wiped ceramic parts in deionized water and perform ultrasonic cleaning;

可選的,上述步驟S25中,進行超聲波清洗的清洗時間的範圍為大於等於15min,且小於等於30min。Optionally, in the above step S25, the range of cleaning time for ultrasonic cleaning is greater than or equal to 15 minutes and less than or equal to 30 minutes.

S26、採用純水對超聲波清洗後的陶瓷件沖洗。S26. Use pure water to rinse the ceramic parts after ultrasonic cleaning.

可選的,上述步驟S26中,採用純水對超聲波清洗後的所述陶瓷件沖洗的時間為大於等於15min,且小於等於60min。Optionally, in the above step S26, the time for rinsing the ceramic piece after ultrasonic cleaning with pure water is greater than or equal to 15 minutes and less than or equal to 60 minutes.

下面對上述第一清洗過程S1的具體實施方式進行詳細描述。具體地,如圖3所示,第一清洗過程S1具體包括以下步驟:The specific implementation of the above-mentioned first cleaning process S1 will be described in detail below. Specifically, as shown in Figure 3, the first cleaning process S1 specifically includes the following steps:

S11、採用沾有異丙酮(IPA)溶液的無塵布擦拭陶瓷件;S11. Wipe the ceramic parts with a lint-free cloth dipped in isopropyltone (IPA) solution;

上述步驟S11可以對陶瓷件進行導電,以中和陶瓷件上帶電的陶瓷顆粒。The above-mentioned step S11 can conduct electricity to the ceramic piece to neutralize the charged ceramic particles on the ceramic piece.

可選的,上述異丙酮溶液的純度為99.7%。Optionally, the purity of the above-mentioned isopropyl ketone solution is 99.7%.

應當注意的是,在擦拭過程中,若無塵布表面有污漬,需要重新清洗無塵布,以避免對陶瓷件表面的紋理和光滑表面造成損傷。It should be noted that during the wiping process, if there are stains on the surface of the lint-free cloth, the lint-free cloth needs to be cleaned again to avoid damage to the texture and smooth surface of the ceramic piece.

S12、將擦拭後的陶瓷件浸泡在鹼性溶液中,並進行超聲波清洗;S12. Soak the wiped ceramic parts in an alkaline solution and perform ultrasonic cleaning;

鹼性溶液(即用作上述第一清洗過程S1中的化學溶液)可以溶解陶瓷件上的顆粒,結合超聲波清洗,可以有效實現顆粒的去除。The alkaline solution (that is, the chemical solution used in the above-mentioned first cleaning process S1) can dissolve the particles on the ceramic piece, and combined with ultrasonic cleaning, the particles can be effectively removed.

為了有效溶解陶瓷件上的顆粒,提高清洗效果,可選的,上述鹼性溶液例如為濃度百分比的範圍為大於等於15%,且小於等於20%的KOH溶液,該鹼性溶液的溫度的範圍為大於等於75°,且小於等於85°;步驟S12中,進行超聲波清洗的時間的範圍為大於等於1h,且小於等於3h,該超聲波清洗的時間通過設定在上述範圍,既可以有效溶解陶瓷件上的顆粒,又可以避免陶瓷件在鹼性溶液中的浸泡時間過長而導致陶瓷件的密封面和孔邊緣處產生損傷,影響零件的密封性。In order to effectively dissolve the particles on the ceramic parts and improve the cleaning effect, optionally, the above-mentioned alkaline solution is, for example, a KOH solution with a concentration range of 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 range of ultrasonic cleaning time is greater than or equal to 1 hour and less than or equal to 3 hours. By setting the ultrasonic cleaning time in the above range, the ceramic parts can be effectively dissolved The particles on the ceramic parts can prevent the ceramic parts from being soaked in alkaline solution for too long, which will cause damage to the sealing surface and hole edges of the ceramic parts, affecting the sealing performance of the parts.

在實際應用中,可以利用濃度檢測儀檢測KOH溶液的濃度值,並根據檢測到的濃度值對溶液進行更換或者補充,以使其達到目標濃度值。In practical applications, 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 achieve the target concentration value.

S13、採用純水對超聲波清洗後的陶瓷件沖洗;S13. Use pure water to rinse the ceramic parts after ultrasonic cleaning;

可選的,上述步驟S13中,採用純水對超聲波清洗後的陶瓷件沖洗3次到5次。Optionally, in the above step S13, pure water is used to rinse the ultrasonic cleaned ceramic piece 3 to 5 times.

S14、將沖洗後的陶瓷件浸泡在酸性溶液中;S14. Soak the rinsed ceramic pieces in acidic solution;

上述步驟S14可以中和殘留在陶瓷件上的鹼性溶液,以減少鹼性溶液對陶瓷件的腐蝕,避免鹼性溶液對陶瓷件的密封面和孔邊緣處產生損傷。The above-mentioned step S14 can neutralize the alkaline solution remaining on the ceramic piece to reduce corrosion of the ceramic piece by the alkaline solution and avoid damage to the sealing surface and hole edge of the ceramic piece by the alkaline solution.

可選的,上述步驟S14中,將沖洗後的陶瓷件浸泡在酸性溶液中的浸泡時間的範圍為大於等於5min,且小於等於10min。Optionally, in the above step S14, the soaking time of 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.

可選的,上述酸性溶液為鹽酸或者氟硝酸溶液,其中,氟硝酸溶液與鹼性溶液(例如KOH溶液)的中和作用更優。Optionally, the above-mentioned acidic solution is hydrochloric acid or fluorine nitric acid solution, wherein the neutralization effect of fluorine nitric acid solution and an alkaline solution (such as KOH solution) is better.

另外,上述步驟S14可以不使用超聲波清洗。In addition, ultrasonic cleaning may not be used in the above step S14.

S15、採用純水對在所述酸性溶液浸泡後的陶瓷件沖洗;S15. Use pure water to rinse the ceramic parts after being soaked in the acidic solution;

S16、將沖洗後的陶瓷件浸泡在鹼性溶液中。S16. Soak the rinsed ceramic pieces in alkaline solution.

上述步驟S16可以進一步溶解陶瓷件上的顆粒。The above step S16 can further dissolve the particles on the ceramic piece.

可選的,上述步驟S16中,沖洗後的陶瓷件浸泡在鹼性溶液中的浸泡時間的範圍為大於等於1h,且小於等於3h,通過該浸泡時間設定在上述範圍,既可以有效溶解陶瓷件上的顆粒,又可以避免陶瓷件在鹼性溶液中的浸泡時間過長而導致陶瓷件的密封面和孔邊緣處產生損傷,影響零件的密封性。Optionally, in the above step S16, the range of the soaking time for immersing the rinsed ceramic pieces in the alkaline solution is greater than or equal to 1 hour and less than or equal to 3 hours. By setting the soaking time in the above range, the ceramic pieces can be effectively dissolved. The particles on the ceramic parts can prevent the ceramic parts from being soaked in alkaline solution for too long, which will cause damage to the sealing surface and hole edges of the ceramic parts, affecting the sealing performance of the parts.

下面對上述第三清洗過程S3的具體實施方式進行詳細描述。具體地,如圖4所示,第三清洗過程S3具體包括以下步驟:The specific implementation of the above third cleaning process S3 will be described in detail below. Specifically, as shown in Figure 4, the third cleaning process S3 specifically includes the following steps:

S31、採用純水對陶瓷件沖洗;S31. Use pure water to rinse the ceramic parts;

可選的,上述步驟S31中,沖洗時間的範圍為大於等於45min,且小於等於60min;Optionally, in the above step S31, the range of flushing time is greater than or equal to 45 minutes and less than or equal to 60 minutes;

S32、將沖洗後的陶瓷件浸泡在去離子水中,並進行超聲波清洗;S32. Soak the rinsed ceramic parts in deionized water and perform ultrasonic cleaning;

上述步驟S32可以對陶瓷件進行全面清洗,由於使用去離子水進行超聲波清洗的清洗效果最明顯,在完成超聲波清洗步驟之後,可以保證陶瓷件的清洗效果滿足製程要求。而且,利用前面的第一清洗過程S1和第二清洗過程S2已經實現了損傷層和懸浮顆粒的去除,從而可以彌補超聲波清洗無法完全去除損傷層和懸浮顆粒的不足。The above-mentioned step S32 can comprehensively clean the ceramic parts. Since ultrasonic cleaning using deionized water has the most obvious cleaning effect, after completing the ultrasonic cleaning step, it can be ensured that the cleaning effect of the ceramic parts meets the process requirements. Moreover, the damage layer and suspended particles have been removed using the previous 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.

可選的,上述步驟S32中,進行超聲波清洗的時間的範圍為大於等於30min,且小於等於60min。Optionally, in the above step S32, the time range for ultrasonic cleaning is greater than or equal to 30 minutes and less than or equal to 60 minutes.

可選的,上述去離子水的電阻率大於等於4MΩ•cm。Optionally, the resistivity of the above-mentioned deionized water is greater than or equal to 4MΩ·cm.

S33、將超聲波清洗後的陶瓷件浸泡在去離子水中,在浸泡過程中,始終向清洗槽中通入新的去離子水,並採用溢流的方式排出清洗槽中的去離子水;S33. Soak the ultrasonically cleaned ceramic parts in deionized water. During the soaking process, always introduce new deionized water into the cleaning tank, and use overflow to discharge the deionized water in the cleaning tank;

上述步驟S33中,通過在浸泡過程中,始終向清洗槽中通入新的去離子水,並採用溢流的方式排出該清洗槽中的去離子水,可以使去離子水處於循環流動狀態,從而可以進一步提高清洗效果。In the above step S33, by always introducing new deionized water into the cleaning tank during the soaking process, and using overflow to discharge the deionized water in the cleaning tank, the deionized water can be kept in a circulating flow state. This can further improve the cleaning effect.

可選的,上述步驟S33中,去離子水的溫度維持的範圍為大於等於32℃,且小於等於42℃。Optionally, in the above step S33, the temperature of the deionized water is maintained in a range of greater than or equal to 32°C and less than or equal to 42°C.

S34、對浸泡後的陶瓷件進行吹掃,並在吹掃後對陶瓷件進行烘烤。S34. Purge the soaked ceramic pieces, and bake the ceramic pieces after purging.

可選的,上述步驟S34採用的吹掃氣體包括氮氣,該氮氣的純度為99.999%;氮氣的吹掃方向與陶瓷件表面之間的夾角的範圍為大於等於30℃,且小於等於45℃,以避免顆粒重新掉落在陶瓷件表面。Optionally, the purge gas used in the above step S34 includes nitrogen, and the purity of the nitrogen is 99.999%; the angle between the purge direction of the nitrogen and the surface of the ceramic piece ranges from greater than or equal to 30°C to less than or equal to 45°C. To prevent particles from falling back onto the surface of the ceramic piece.

可選的,首先使用乾燥氮氣對陶瓷件進行全面吹掃;然後使用乾燥氮氣吹掃淨化爐(或烘箱),以烘乾其內部;最後,將陶瓷件放入吹掃後的淨化爐(或烘箱)中進行烘烤。Optionally, first use dry nitrogen to comprehensively purge the ceramic parts; then use dry nitrogen to purge the purification furnace (or oven) to dry the inside; finally, place the ceramic parts into the purged purification furnace (or oven). Bake in oven).

下面將採用現有技術中的陶瓷件清洗方法和本發明實施例提供的陶瓷件清洗方法分別獲得的陶瓷件進行對比實驗。具體地,現有技術中的陶瓷件清洗方法的流程為:首先將陶瓷件浸入鹼性脫脂劑中浸泡50min-80min,再將陶瓷件放入去離子水中漂洗(使用加壓去離子水噴淋陶瓷件表面各處);之後,將陶瓷件浸入酸性溶液中浸泡5min-10min,然後將陶瓷件從溶液中取出,並再次浸入去離子水中進行上述漂洗,之後浸入電阻率≥4MΩ•cm、常溫的去離子水中進行超聲波清洗10min-15min,之後將陶瓷件浸入電阻率≥8MΩ•cm的去離子水中進行熱水浸洗,最後使用氮氣吹幹陶瓷件,並烘乾陶瓷件,完成整個清洗流程。In the following, a comparative experiment will be conducted on ceramic pieces obtained by using the ceramic piece cleaning method in the prior art and the ceramic piece cleaning method provided by the embodiment of the present invention. Specifically, the process of the ceramic parts cleaning method in the prior art is: first, immerse the ceramic parts in an alkaline degreasing agent for 50min-80min, and then rinse the ceramic parts in deionized water (use pressurized deionized water to spray the ceramics (everywhere on the surface of the piece); after that, immerse the ceramic piece in the acidic solution for 5min-10min, then take the ceramic piece out of the solution and immerse it again in deionized water for the above rinse, and then immerse it in a solution with a resistivity of ≥4MΩ·cm and room temperature. Carry out ultrasonic cleaning in deionized water for 10min-15min, then immerse the ceramic parts in deionized water with a resistivity of ≥8 MΩ·cm and perform hot water soaking. Finally, use nitrogen to blow dry the ceramic parts and dry the ceramic parts to complete the entire cleaning process.

本發明實施例提供的陶瓷件清洗方法包括上述三個清洗過程S1-S3,其中,第一清洗過程S1包括上述步驟S11-S16;第二清洗過程S2包括上述步驟S21-S26;第三清洗過程S3包括上述步驟S31-S34。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; and the third cleaning process S3 includes the above steps S31-S34.

圖5為採用現有技術中的陶瓷件清洗方法和本發明實施例提供的陶瓷件清洗方法分別獲得的陶瓷件上的損傷層的對比圖。結合實驗數據和圖5所示,採用現有技術中的陶瓷件清洗方法獲得的陶瓷件,其表層仍然存在機加工損傷層,如圖5中的(a)圖所示,該損傷層的厚度為10μm-30μm,而該損傷層的存在是顆粒產生的重要源頭之一。與之相比,如圖5中的(b)圖可以看出,採用本發明實施例提供的陶瓷件清洗方法獲得的陶瓷件,該陶瓷件上的損傷層被顯著去除,從而可以避免陶瓷件在設備上使用過程中源源不斷地掉落顆粒。Figure 5 is a comparative view of the damaged layer on the ceramic piece obtained by using the ceramic piece cleaning method in the prior art and the ceramic piece cleaning method provided by the embodiment of the present invention. Based on the experimental data and shown in Figure 5, the ceramic parts obtained by using the ceramic parts cleaning method in the prior art still have a machining damage layer on the surface. As shown in (a) of Figure 5, the thickness of the damage layer is 10μm-30μm, and the existence of this damage layer is one of the important sources of particle generation. In contrast, as shown in (b) of Figure 5 , for ceramic parts obtained by using the ceramic parts cleaning method provided by the embodiment of the present invention, the damaged layer on the ceramic parts is significantly removed, thereby avoiding the possibility of damage to the ceramic parts. Particles continue to fall out during use on the device.

圖6為採用現有技術中的陶瓷件清洗方法和本發明實施例提供的陶瓷件清洗方法分別獲得的陶瓷件上的懸浮顆粒的對比圖。結合實驗數據和圖6所示,採用現有技術中的陶瓷件清洗方法獲得的陶瓷件,其陶瓷表面仍然存在0.2μm~1μm的懸浮顆粒,如圖6中的(a)圖所示,圖中黑色區域上的白色點狀物即為懸浮顆粒。此外,現有技術中的陶瓷件清洗方法獲得的陶瓷件,其在製程過程中落在晶圓上的每單位面積的顆粒數量≥500ea,遠高於顆粒指標(每單位面積的顆粒數量<2ea),另外,測量陶瓷件上的液體顆粒計數(即,LPC)獲取的檢測值為75856PA/cm2。與之相比,如圖6中的(b)圖可以看出,圖中黑色區域上的白色點狀物顯著減少,由此可知,採用本發明實施例提供的陶瓷件清洗方法獲得的陶瓷件,該陶瓷件上的懸浮顆粒顯著減少,該陶瓷件在製程過程中落在晶圓上的每單位面積的顆粒數量低於顆粒指標(每單位面積的顆粒數量<2ea),並且測量其LPC獲取的檢測值為729PA/cm2,遠遠小於現有技術的上述LPC檢測值。Figure 6 is a comparative diagram of suspended particles on ceramic parts obtained by using the ceramic parts cleaning method in the prior art and the ceramic parts cleaning method provided by the embodiment of the present invention. Combining the experimental data and shown in Figure 6, the ceramic parts obtained by using the ceramic parts cleaning method in the prior art still have suspended particles of 0.2 μm ~ 1 μm on the ceramic surface, as shown in (a) of Figure 6. In the figure The white dots on the black area are suspended particles. In addition, the number of particles per unit area that falls on the wafer during the manufacturing process of the ceramic parts obtained by the ceramic parts cleaning method in the prior art is ≥500ea, which is much higher than the particle index (the number of particles per unit area is <2ea). , In addition, the detection value obtained by measuring the liquid particle count (ie, LPC) on the ceramic piece is 75856PA/cm2. In comparison, as can be seen in (b) of Figure 6, the white dots in the black area in the figure are significantly reduced. From this, it can be seen that the ceramic parts obtained by using the ceramic parts 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 manufacturing process is lower than the particle index (the number of particles per unit area is <2ea), and its LPC is measured to obtain The detection value is 729PA/cm2, which is far smaller than the above-mentioned LPC detection value of the existing technology.

本發明實施例中的陶瓷件例如包括用於半導體設備的陶瓷製程套件。該陶瓷製程套件可以是諸如內襯、介質窗、噴嘴、篩管、立體感應線圈的主、副介質筒、觀察窗保護筒等採用陶瓷材料製備的部件。通過提高上述部件的清洗效果,可有效解決陶瓷顆粒數量超標的問題,提高晶片良率。The ceramic parts in embodiments of the present invention include, for example, ceramic process kits for semiconductor devices. The ceramic process kit can be components made of ceramic materials such as inner linings, media windows, nozzles, screen tubes, main and auxiliary media cylinders of the three-dimensional induction coil, and observation window protection cylinders. By improving the cleaning effect of the above components, the problem of excessive number of ceramic particles can be effectively solved and the wafer yield rate can be improved.

綜上所述,本發明實施例提供的陶瓷件清洗方法,其將清洗分為三個清洗過程,其中,第一清洗過程採用化學溶液溶解陶瓷件上的顆粒,該過程可以有效對陶瓷件表面上尺寸較大的盲孔、褶皺及非焊接縫隙處的顆粒進行清洗;第二清洗過程採用指定酸性溶液軟化腐蝕陶瓷件上的顆粒以及消弭陶瓷件上的損傷層,由於該損傷層的存在是顆粒產生的重要源頭之一,上述第二清洗過程通過上述指定酸性溶液有針對性地消弭陶瓷件上的損傷層,可以有效在源頭上去除顆粒,這與現有技術相比,可以大大減少顆粒數量;第三清洗過程採用超聲波清洗的方式清洗陶瓷件,以去除陶瓷件上殘留的顆粒和溶液(酸性或鹼性溶液),從而可以對陶瓷件進行全面清洗,最終可以有效提高清洗效果,解決陶瓷顆粒數量超標的問題,提高晶片良率。In summary, the ceramic parts cleaning method provided by the embodiment of the present invention divides the cleaning into three cleaning processes. In the first cleaning process, a chemical solution is used to dissolve the particles on the ceramic parts. This process can effectively clean the surface of the ceramic parts. Clean the particles in larger blind holes, wrinkles and non-welding gaps; the second cleaning process uses designated acidic solutions to soften the particles on the corroded ceramic parts and eliminate the damaged layer on the ceramic parts, because the existence of the damaged layer is One of the important sources of particle generation, the above-mentioned second cleaning process uses the above-mentioned designated acidic solution to eliminate the damaged layer on the ceramic parts in a targeted manner, which can effectively remove particles at the source. This can greatly reduce the number of particles compared with the existing technology. ; The third cleaning process uses ultrasonic cleaning to clean ceramic parts to remove residual particles and solutions (acidic or alkaline solutions) on the ceramic parts, so that the ceramic parts can be fully cleaned, which can ultimately effectively improve the cleaning effect and solve the problem of ceramic parts. To solve the problem of excessive number of particles and improve the wafer yield.

前述內容概括數項實施例之特徵,使得熟習此項技術者可更佳地理解本揭露之態樣。熟習此項技術者應瞭解,其等可容易地使用本揭露作為用於設計或修改用於實行本文中介紹之實施例之相同目的及/或達成相同優點之其他製程及結構之一基礎。熟習此項技術者亦應瞭解,此等等效構造不背離本揭露之精神及範疇,且其等可在不背離本揭露之精神及範疇之情況下在本文中作出各種改變、置換及更改。The foregoing content summarizes the features of several embodiments so that those skilled in the art may better understand the aspects of the present disclosure. Those skilled in the art should appreciate that they may readily use the present disclosure as a basis for designing or modifying other processes and structures for carrying out the same purposes and/or achieving the same advantages of the embodiments introduced herein. Those skilled in the art should also understand that such equivalent constructions do not depart from the spirit and scope of the present disclosure, and that they can be variously changed, replaced and modified herein without departing from the spirit and scope of the present disclosure.

S1-S3, S21-S26, S11-S16, S31-S34:步驟S1-S3, S21-S26, S11-S16, S31-S34: steps

當結合附圖閱讀時,從以下詳細描述最佳理解本揭露之態樣。應注意,根據產業中之標準實踐,各種構件未按比例繪製。事實上,為了論述的清楚起見可任意增大或減小各種構件之尺寸。 圖1為本發明實施例提供的陶瓷件清洗方法的流程框圖; 圖2為本發明實施例採用的第二清洗過程的流程框圖; 圖3為本發明實施例採用的第一清洗過程的流程框圖; 圖4為本發明實施例採用的第三清洗過程的流程框圖; 圖5為採用現有技術中的陶瓷件清洗方法和本發明實施例提供的陶瓷件清洗方法分別獲得的陶瓷件上的損傷層的對比圖; 圖6為採用現有技術中的陶瓷件清洗方法和本發明實施例提供的陶瓷件清洗方法分別獲得的陶瓷件上的懸浮顆粒的對比圖。 The present disclosure is best understood from the following detailed description when read in conjunction with the accompanying drawings. It should be noted that in accordance with standard practice in the industry, the various components are not drawn to scale. In fact, the dimensions of the various components may be arbitrarily increased or reduced for clarity of discussion. Figure 1 is a flow chart of a method for cleaning ceramic parts provided by an embodiment of the present invention; Figure 2 is a flow chart of the second cleaning process adopted in the embodiment of the present invention; Figure 3 is a flow chart of the first cleaning process adopted in the embodiment of the present invention; Figure 4 is a flow chart of the third cleaning process adopted in the embodiment of the present invention; Figure 5 is a comparative view of the damaged layer on the ceramic piece obtained by using the ceramic piece cleaning method in the prior art and the ceramic piece cleaning method provided by the embodiment of the present invention; Figure 6 is a comparative diagram of suspended particles on ceramic parts obtained by using the ceramic parts cleaning method in the prior art and the ceramic parts cleaning method provided by the embodiment of the present invention.

S1-S3:步驟 S1-S3: Steps

Claims (8)

一種陶瓷件清洗方法,包括:一第一清洗過程,採用化學溶液溶解一陶瓷件上的顆粒;第二清洗過程,採用一指定酸性溶液軟化腐蝕該陶瓷件上的顆粒以及消弭該陶瓷件上的損傷層;第三清洗過程,採用超聲波清洗的方式清洗該陶瓷件,以去除該陶瓷件上殘留的顆粒和溶液;其中,該第一清洗過程、該第二清洗過程以及該第三清洗過程用以去除陶瓷件在成型過程中產生上的粉末狀顆粒;其中該第一清洗過程具體包括以下步驟:S11、採用沾有異丙酮溶液的無塵布擦拭該陶瓷件;S12、將擦拭後的該陶瓷件浸泡在鹼性溶液中,並進行超聲波清洗;S13、採用純水對超聲波清洗後的該陶瓷件沖洗;S14、將沖洗後的該陶瓷件浸泡在酸性溶液中;S15、採用純水對在該酸性溶液浸泡後的該陶瓷件沖洗;S16、將沖洗後的該陶瓷件浸泡在鹼性溶液中;其中該第二清洗過程具體包括以下步驟:S21、採用該指定酸性溶液對該陶瓷件進行沖洗;S22、將採用該指定酸性溶液沖洗後的該陶瓷件浸泡在該指定酸性溶液中;S23、採用純水對浸泡後的該陶瓷件沖洗;S24、採用奈米材料製作的打磨工具擦拭採用純水沖洗後的該陶瓷 件;S25、將擦拭後的該陶瓷件浸泡在去離子水中,並進行超聲波清洗;S26、採用純水對超聲波清洗後的該陶瓷件沖洗;其中該第三清洗過程具體包括以下步驟:S31、採用純水對該陶瓷件沖洗;S32、將沖洗後的該陶瓷件浸泡在去離子水中,並進行超聲波清洗;S33、將超聲波清洗後的該陶瓷件浸泡在去離子水中,在浸泡過程中,始終向清洗槽中通入新的去離子水,並採用溢流的方式排出該清洗槽中的去離子水;S34、對浸泡後的該陶瓷件進行吹掃,並在吹掃後對該陶瓷件進行烘烤。 A method for cleaning ceramic pieces, including: a first cleaning process, using a chemical solution to dissolve particles on a ceramic piece; a second cleaning process, using a designated acidic solution to soften and corrode the particles on the ceramic piece and eliminate the particles on the ceramic piece Damage layer; the third cleaning process uses ultrasonic cleaning to clean the ceramic piece to remove residual particles and solution on the ceramic piece; wherein, the first cleaning process, the second cleaning process and the third cleaning process use In order to remove the powdery particles produced on the ceramic parts during the molding process; the first cleaning process specifically includes the following steps: S11, wipe the ceramic parts with a lint-free cloth dipped in isopropyltone solution; S12, wipe the wiped ceramic parts The ceramic parts are soaked in an alkaline solution and subjected to ultrasonic cleaning; S13, use pure water to rinse the ceramic parts after ultrasonic cleaning; S14, soak the rinsed ceramic parts in an acidic solution; S15, use pure water to clean the ceramic parts. Rinse the ceramic piece after being soaked in the acidic solution; S16, soak the rinsed ceramic piece in an alkaline solution; wherein the second cleaning process specifically includes the following steps: S21, use the specified acidic solution to clean the ceramic piece Rinse; S22. Soak the ceramic piece rinsed with the specified acidic solution in the specified acidic solution; S23. Rinse the soaked ceramic piece with pure water; S24. Wipe it with a grinding tool made of nanomaterials. The ceramic after being rinsed with pure water piece; S25, soak the wiped ceramic piece in deionized water and perform ultrasonic cleaning; S26, use pure water to rinse the ultrasonic cleaned ceramic piece; wherein the third cleaning process specifically includes the following steps: S31. Use pure water to rinse the ceramic piece; S32. Soak the rinsed ceramic piece in deionized water and perform ultrasonic cleaning; S33. Soak the ultrasonic cleaned ceramic piece in deionized water. During the soaking process, Always introduce new deionized water into the cleaning tank, and use overflow to discharge the deionized water in the cleaning tank; S34, purge the soaked ceramic piece, and clean the ceramic piece after purging. pieces for baking. 如請求項1所述的陶瓷件清洗方法,其中該指定酸性溶液包括氟硝酸溶液,該氟硝酸溶液由氫氟酸溶液、硝酸溶液和純水混合而成。 The method for cleaning ceramic parts as described in claim 1, wherein the designated acidic solution includes a fluorine nitric acid solution, which is a mixture of hydrofluoric acid solution, nitric acid solution and pure water. 如請求項2所述的陶瓷件清洗方法,其中該氫氟酸溶液、硝酸溶液和電阻率為18MΩ.cm的純水的配比為1:1:1;其中,該氫氟酸溶液包含的氫氟酸的質量分數的範圍為大於等於5%,且小於等於15%;該硝酸溶液包含的硝酸的質量分數的範圍為大於等於25%,且小於等於35%。 The method for cleaning ceramic parts as described in claim 2, wherein the ratio of the hydrofluoric acid solution, nitric acid solution and pure water with a resistivity of 18MΩ.cm is 1:1:1; wherein, the hydrofluoric acid solution contains The mass fraction of hydrofluoric acid ranges from greater than or equal to 5% to less than or equal to 15%; the mass fraction of nitric acid contained in the nitric acid solution ranges from greater than or equal to 25% to less than or equal to 35%. 如請求項1至3任意一項所述的陶瓷件清洗方法,其中在進行第三清洗過程之前,該第二清洗過程執行至少4次。 The ceramic piece cleaning method according to any one of claims 1 to 3, wherein the second cleaning process is performed at least 4 times before the third cleaning process is performed. 如請求項1所述的陶瓷件清洗方法,其中該步驟S21中,採用該指定酸性溶液對該陶瓷件沖洗至少3次;該步驟S22中,將採用該指定酸性溶液沖洗後的該陶瓷件浸泡在該指定酸性溶液中的浸泡時間的範圍為大於等於10min,且小於等於20min;該步驟S23中,採用純水對浸泡後的該陶瓷件沖洗3次到5次;該步驟S24中,採用奈米材料製作的打磨工具擦拭採用純水沖洗後的該陶瓷件3次到5次;該步驟S25中,進行超聲波清洗的清洗時間的範圍為大於等於15min,且小於等於30min;該步驟S26中,採用純水對超聲波清洗後的該陶瓷件沖洗的時間的範圍為大於等於15min,且小於等於60min。 The ceramic piece cleaning method as described in claim 1, wherein in step S21, the ceramic piece is rinsed with the designated acidic solution at least 3 times; in step S22, the ceramic piece washed with the designated acidic solution is soaked The range of the soaking time in the designated acidic solution is greater than or equal to 10 minutes and less than or equal to 20 minutes; in step S23, pure water is used to rinse the soaked ceramic piece 3 to 5 times; in step S24, sodium chloride is used. The polishing tool made of rice material wipes the ceramic piece after being rinsed with pure water 3 to 5 times; in step S25, the cleaning time range of ultrasonic cleaning is greater than or equal to 15 minutes and less than or equal to 30 minutes; in step S26, The time range for rinsing the ceramic piece after ultrasonic cleaning with pure water is greater than or equal to 15 minutes and less than or equal to 60 minutes. 如請求項1所述的陶瓷件清洗方法,其中該異丙酮溶液的純度為99.7%;該鹼性溶液為濃度百分比的範圍為大於等於15%,且小於等於20%的KOH溶液,該鹼性溶液的溫度的範圍為大於等於75°,且小於等於85°;該步驟S12中,進行超聲波清洗的時間的範圍為大於等於1h,且小於等於3h;該步驟S13中,採用純水對超聲波清洗後的該陶瓷件沖洗3次到5次;該步驟S14中,將沖洗後的該陶瓷件浸泡在酸性溶液中的浸泡時間的範圍為大於等於5min,且小於等於10min;該步驟S15中,採用純水對在該酸性溶液浸泡後的該陶瓷件沖洗3次到5次;該步驟S16中,沖洗後的該陶瓷件浸泡在鹼性溶液中的浸泡時間的範圍為大於等於1h,且小於等於3h。 The method for cleaning ceramic parts as described in claim 1, wherein the purity of the isopropyl solution is 99.7%; the alkaline solution is a KOH solution with a concentration percentage range of greater than or equal to 15% and less than or equal to 20%, and the alkaline solution The temperature range of the 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; in step S13, pure water is used for ultrasonic cleaning The washed ceramic piece is rinsed 3 to 5 times; in step S14, the soaking time range of the rinsed ceramic piece in the acidic solution is greater than or equal to 5 minutes and less than or equal to 10 minutes; in step S15, use Pure water rinses the ceramic piece after being soaked in the acidic solution 3 to 5 times; in step S16, the soaking time of the rinsed ceramic piece in the alkaline solution ranges from greater than or equal to 1 hour to less than or equal to 3h. 如請求項1所述的陶瓷件清洗方法,其中該步驟S31中,沖洗時間的 範圍為大於等於45min,且小於等於60min;該步驟S32中,進行超聲波清洗的時間的範圍為大於等於30min,且小於等於60min;該步驟S33中,浸泡時間的範圍為大於等於30min,且小於等於60min;該步驟S33中,該去離子水的溫度維持的範圍為大於等於32℃,且小於等於42℃;該步驟S34中,採用的吹掃氣體包括氮氣,該氮氣的純度為99.999%;該氮氣的吹掃方向與該陶瓷件表面之間的夾角的範圍為大於等於30°,且小於等於45°。 The method for cleaning ceramic parts as described in claim 1, wherein in step S31, the rinsing time The range is greater than or equal to 45 minutes and less than or equal to 60 minutes; in step S32, the range of ultrasonic cleaning time is greater than or equal to 30 minutes and less than or equal to 60 minutes; in step S33, the range of soaking time is greater than or equal to 30 minutes and less than or equal to 60 minutes. 60 min; in step S33, the temperature of the deionized water is maintained in a range of greater than or equal to 32°C and less than or equal to 42°C; in step S34, the purge gas used includes nitrogen, and the purity of the nitrogen is 99.999%; The range of the angle between the purging direction of the nitrogen gas and the surface of the ceramic piece is greater than or equal to 30° and less than or equal to 45°. 如請求項1所述的陶瓷件清洗方法,其中該陶瓷件包括用於半導體設備的陶瓷製程套件。 The ceramic part cleaning method as claimed in claim 1, wherein the ceramic part includes a ceramic process kit for semiconductor equipment.
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