CN102517594A - Method for cleaning cerium-based polishing solution residues - Google Patents

Method for cleaning cerium-based polishing solution residues Download PDF

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CN102517594A
CN102517594A CN 201110430321 CN201110430321A CN102517594A CN 102517594 A CN102517594 A CN 102517594A CN 201110430321 CN201110430321 CN 201110430321 CN 201110430321 A CN201110430321 A CN 201110430321A CN 102517594 A CN102517594 A CN 102517594A
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cleaning
step
cerium
solution
part
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CN 201110430321
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CN102517594B (en )
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张艳
郭云飞
马瑾
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西安北方捷瑞光电科技有限公司
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Abstract

The invention discloses a method for cleaning cerium-based polishing solution residues, comprising the following steps of: 1) cleaning residual cerium-based polishing powder on the surface of a part by the use of an HNO3:H2O2:H2O acidic solution; 2) cleaning the part taken out from the step 1) by a pure water spraying mode; 3) measuring pure water, weighing ethylene diamine tetraacetic acid (EDTA) and sodium hydroxide, completely dissolving in pure water; 4) diluting the solution prepared in the step 3) in pure water and boiling on an electric furnace; 5) boiling the washed part obtained fromthe step 2) in the solution obtained from the step 4); and 6) cleaning the part taken out from the step 5) by the pure water spraying mode. According to the method, the acidic solution is used to dissolve most of the residual polishing powder; by the utilization of the EDTA reagent and cerium-based metal complex, the residual metal ions on the surface of the part are removed from the surface of the part after complexation and deposition; and then sodium hydroxide is used to remove organic matters in the polishing solution. By the adoption of the method provided by the invention, it is easy toclean the residual polishing powder on the surface of the part and the cleaning requires a short time and has little influence on micro-roughness of the part surface.

Description

一种铈基抛光液残留物的清洗方法技术领域[0001] 本发明涉及清洗技术领域,特别涉及一种抛光液残留物的新型清洗方法。 TECHNICAL FIELD The cleaning cerium-based polish residue was [0001] The present invention relates to a novel cleaning method technology, and particularly relates to a polishing liquid residue. 背景技术[0002] 目前用于超光滑表面加工的抛光液,因其具有高抛光效率和高表面质量等优点而备受加工者的青睐,但由于抛光液的成分多样化,组成复杂,配方比例呈保密状态,导致针对此类抛光液清洗的技术可靠性低,清洗后零件仍有少量抛光液的残留物,使得抛光后的零件表面清洗不干净,从而引起超精密器件产品合格率降低,占次品率的50%左右。 [0002] It was used for ultra-smooth polishing surface machining, because of its advantage of having a high polishing efficiency and high surface quality and much favored by the processors, but the diverse components of the polishing liquid, the composition of the complex, the formulation ratio was secrecy, resulting in a polishing liquid for cleaning such a low technical reliability, there is still a small amount of the part after cleaning the polishing liquid residue, such that parts of the surface cleaning after the polishing is not clean, resulting in reduced production yield ultra-precision devices, accounting 50% defective rate. 因此, 清洗质量的高低已严重影响到先进精密仪器的性能,超光滑表面的超精密清洗技术也随之成为超精密加工技术中急待解决的关键性难题之一。 Therefore, the level of cleaning quality has seriously affected the performance of advanced precision instruments, ultra-smooth surface of the ultra-precision cleaning technology also will become one of the key challenges in ultra-precision machining technology need to be solved. 发明内容[0003] 本发明的目的是提供一种针对抛光液残留物的清洗方法,与传统方法相比,该方法既可以有效的去除抛光液残留物,提高零件洁净度;又可以改善超光滑零件的表面质量, 避免清洗液对零件表面质量的损伤和腐蚀,对零件表面的微粗糙度影响甚小,从而提高了零件的良品率。 SUMMARY OF THE INVENTION [0003] The object of the present invention is to provide a method for cleaning a polishing liquid residue, in comparison with the conventional method, which can effectively remove not only a polishing liquid residue, to improve the cleanliness of the parts; ultra-smooth and can improve surface quality of the parts, to prevent the cleaning liquid on the surface quality and corrosion damage, micro-roughness of the surface of the part is very small, thereby increasing the yield of the parts. [0004] 为了实现上述目的,本发明采用如下技术方案:[0005] 一种铈基抛光液残留物的清洗方法,包括以下步骤:[0006] 1)采用体积比为HNO3 : H2O2 : H2O = 1 : 1 : 1的酸性溶液清洗零件表面残留的铈基抛光粉;[0007] 2)用纯水喷淋的方式清洗从步骤1)中取出的零件,清洗5min ;[0008] 3)量取纯水600ml,称取乙二胺四乙酸(EDTA) 8g和氢氧化钠3. 5_4g并完全溶解于所述600ml纯水中;[0009] 4)取步骤幻中已经配制好的溶液稀释至2-5倍纯水中,放置电炉上煮沸;[0010] 5)将步骤2)中洗好的零件放入步骤4)的溶液中煮沸;[0011] 6)用纯水喷淋的方式清洗从步骤幻中取出的零件,清洗5min,即完成铈基抛光液残留物的清洗。 [0004] To achieve the above object, the present invention adopts the following technical solution: [0005] A method for cleaning a cerium-based polishing liquid residues, comprising the steps of: [0006] 1) The volume ratio HNO3: H2O2: H2O = 1 : 1: 1 acid solution washing parts of surface residual cerium-based polishing powder; [0007] 2) withdrawn from the washing step 1) Part way with a pure water shower cleaning 5min; [0008] 3) amount of pure 600ml water, weighed ethylenediaminetetraacetic acid (EDTA) 8g 3. 5_4g and sodium hydroxide completely dissolved in the purified water 600ml; [0009] 4) the step of taking the diluted solution to the phantom has been formulated 2- boiled [0010] 5) in step 2) the washed parts into step 4) in solution;; 5-fold in purified water, placed in an electric furnace boiling [0011] 6) from the washing step with pure water shower manner magic parts removed, washed 5min, i.e., cerium-based polishing solution to complete the cleaning residue. [0012] 步骤1)中所述酸性溶液清洗的时间为1-1.证。 The [0012] Step 1) in an acidic solution is washed 1-1 times. Syndrome. [0013] 步骤2)中所述纯水的温度为40_50°C。 [0013] Step 2) in the temperature of pure water is 40_50 ° C. [0014] 步骤4)中所述溶液煮沸时间为3-5min。 [0014] Step 4) in the solution was boiled time 3-5min. [0015] 与传统清洗技术相比,本发明具有以下优点:本发明方法利用HNO3 : H2O2 : H2O的酸性溶液溶解大部分残余抛光粉;利用EDTA试剂可以与铈基金属铬合的特点,将零件表面残余金属离子经络合、沉淀后脱离零件表面;再利用氢氧化钠可以去除抛光液中有机物的特点,使得零件表面的残留抛光粉易清洗,清洗时间短,对零件表面的微粗糙度影响小。 [0015] Compared with the conventional washing techniques, the present invention has the following advantages: The method of the present invention using HNO3: H2O2: H2O in an acidic solution to dissolve most of the residual polishing powder; EDTA using a cerium reagent can be combined with the base characteristics of metallic chromium, the part residual metal ions meridian engagement surface, after precipitation from the surface of the part; reuse characteristics polishing liquid sodium can be removed organics, residual polishing powder so that parts of the surface to clean, the cleaning time is short, micro-roughness of the surface of the part small. 综上所述,本发明方法研制的铈基抛光液残留物的新型清洗方法能够有效去除顽固的抛光液残留物,从而获得表面高洁净度高的超光滑表面。 In summary, the novel method of the present invention, the cleaning method developed cerium-based polishing liquid can effectively remove residue stubborn polishing liquid residue, thereby obtaining an ultra-smooth surface of high surface cleanliness high. 具体实施方式[0016] 下面结合具体实施例对本发明做进一步详细描述。 DETAILED DESCRIPTION [0016] The following specific embodiments in conjunction with the present invention will be further described in detail. [0017] 实施例1:[0018] 1)采用体积比为HNO3 : H2O2 : H2O = 1 : 1 : 1的酸性溶液清洗零件表面残留的铈基抛光粉Ih ;[0019] 2)用纯水喷淋的方式清洗从步骤1)中取出的零件,清洗5min ;[0020] 3)向600ml、45°C的纯水中加入8克乙二胺四乙酸(EDTA)和3. 5g的氢氧化钠,搅拌至充分溶解;[0021] 4)将步骤3)中已经配制好的溶液稀释5倍,并煮沸^iin ;[0022] 5)将步骤2)中清洗的零件放入步骤4中煮%iin,即完成铈基抛光液残留物的清洗。 [0017] Example 1: [0018] 1) The volume ratio HNO3: H2O2: H2O = 1: 1: 1 acid solution washing parts of surface residual cerium-based polishing powder Ih; [0019] 2) with pure water spray shower cleaning manner withdrawn from step 1) parts, washing 5min; [0020] 3) to 600ml, 45 ° C water was added 8 g of ethylenediamine tetraacetic acid (EDTA) and sodium hydroxide 3. 5g of and stirred until fully dissolved; good solution was diluted 5-fold [0021] 4) the step 3) has been prepared and boiled ^ iin; [0022] 5) in the step 2) the step of washing parts into% boil 4 iin, i.e., cerium-based polishing solution to complete the cleaning residue. [0023] 清洗效果如下:[0024] 通过奥林巴斯工具显微镜和Talysurf CCI Lite白光三维形貌测量仪对采用不同溶液清洗的零件表面洁净度和粗糙度进行检测,采用本实施例清洗的零件表面无抛光粉残留物,且粗糙度相比清洗前零件的粗糙度增大了可达到0. lnm,传统方法清洗的零件表面存有抛光粉残留物,且粗糙度相比清洗前零件的粗糙度增大了0. 3nm。 [0023] Cleaning results are as follows: [0024] Olympus microscope and by Talysurf CCI Lite 3D white light topography sensor part embodiment of the present embodiment the cleaning solution to clean the different parts of the surface cleanliness and roughness detection using polishing powder residue-free surface, and the roughness of the front part of the washing is increased compared with the roughness of up to 0. lnm, the conventional method of cleaning the surface of the part there polishing powder residue, and the roughness of the rough parts before washing compared degree increased 0. 3nm. [0025] 实施例2[0026] 1)采用HNO3 : H2O2 : H2O = 1 : 1 : 1的酸性溶液清洗零件表面残留的铈基抛光粉1. 2h ;[0027] 2)用纯水喷淋的方式清洗从步骤1)中取出的零件,清洗时间5min ;[0028] 3)向600ml、40°C的纯水中加入8克乙二胺四乙酸(EDTA)和4g的氢氧化钠,搅拌至充分溶解;[0029] 4)将步骤3)中已经配制好的溶液稀释2倍,并煮沸;3min ;[0030] 5)将步骤2、中清洗的零件放入步骤4中煮3min,即完成铈基抛光液残留物的清洗。 [0025] Example 2 [0026] 1) HNO3: H2O2: H2O = 1: 1: 1 acid solution remaining on the surface of the cleaned part cerium-based polishing powder 1. 2h; [0027] 2) sprayed with purified water withdrawn from the cleaning mode in step 1) parts, cleaning time 5min; [0028] 3) to a 600ml, water of 40 ° C was added 8 g of ethylenediamine tetraacetic acid (EDTA) and 4g of sodium hydroxide, and stirred until fully dissolved; [0029] 4) the prepared solution was diluted 2-fold in step 3) has been prepared, and boiled; 3min; [0030] 5) the step 2, the step of cleaning parts placed in boiling 4 3min, complete cerium-based polishing cleaning fluid residue. [0031] 清洗效果如下:[0032] 通过奥林巴斯工具显微镜和Talysurf CCI Lite白光三维形貌测量仪对采用不同溶液清洗的零件表面洁净度和粗糙度进行检测,采用本实施例清洗的零件表面无抛光粉残留物,且粗糙度相比清洗前零件的粗糙度增大了可达到0. lnm,传统方法清洗的零件表面存有抛光粉残留物,且粗糙度相比清洗前零件的粗糙度增大了0. 2nm。 [0031] Cleaning results are as follows: [0032] Olympus microscope and by Talysurf CCI Lite 3D white light topography sensor part embodiment of the present embodiment the cleaning solution to clean the different parts of the surface cleanliness and roughness detection using polishing powder residue-free surface, and the roughness of the front part of the washing is increased compared with the roughness of up to 0. lnm, the conventional method of cleaning the surface of the part there polishing powder residue, and the roughness of the rough parts before washing compared degree increased 0. 2nm. [0033] 实施例3[0034] 1)采用HNO3 : H2O2 : H2O = 1 : 1 : 1的酸性溶液清洗零件表面残留的铈基抛光粉1. 5h ;[0035] 2)用纯水喷淋的方式清洗从步骤1)中取出的零件,清洗时间5min ;[0036] 3)向600ml、50°C的纯水中加入8克乙二胺四乙酸(EDTA)和4g的氢氧化钠,搅拌至充分溶解;[0037] 4)将步骤3)中已经配制好的溶液稀释3倍,并煮沸5min ;[0038] 5)将步骤2~)中清洗的零件放入步骤4中煮5min,即完成铈基抛光液残留物的清洗。 [0033] Example 3 [0034] 1) HNO3: H2O2: H2O = 1: 1: 1 acid solution remaining on the surface of the cleaned part cerium-based polishing powder 1. 5h; [0035] 2) sprayed with purified water withdrawn from the cleaning mode in step 1) parts, cleaning time 5min; [0036] 3) to a 600ml, purified water at 50 ° C was added 8 g of ethylenediamine tetraacetic acid (EDTA) and 4g of sodium hydroxide, and stirred until fully dissolved; in [0037] 4) the step 3) the prepared solution has been diluted 3-fold, and boiled for 5min; [0038] 5) in step 2 ~) in the washing step 4 parts into boiling 5min, complete cerium-based polishing cleaning fluid residue. [0039] 清洗效果如下:[0040] 通过奥林巴斯工具显微镜和Talysurf CCI Lite白光三维形貌测量仪对采用不同溶液清洗的零件表面洁净度和粗糙度进行检测,采用本实施例清洗的零件表面无抛光粉残留物,且粗糙度相比清洗前零件的粗糙度增大了可达到0. 2nm,传统方法清洗的零件表面存有抛光粉残留物,且粗糙度相比清洗前零件的粗糙度增大了0. 4nm。 [0039] Cleaning results are as follows: [0040] Olympus microscope and by Talysurf CCI Lite 3D white light topography sensor part embodiment of the present embodiment the cleaning solution to clean the different parts of the surface cleanliness and roughness detection using polishing powder residue-free surface, and the roughness of the front part of the washing is increased compared with the roughness of up to 0. 2nm, the conventional method of cleaning the surface of the part there polishing powder residue, and the roughness of the rough parts before washing compared degree increased 0. 4nm. [0041] 以上所述仅为本发明给出的有限的实施方式,不是全部或限定的实施方式,本领域普通技术人员通过阅读本发明说明书而对本发明技术方案采取的任何等效的变换,均为本发明的权利要求所涵盖。 [0041] The above are only limited embodiments of the present invention is given, not all embodiments or limitations, those of ordinary skill in the art of the present invention to take a reading of the description of the present invention, any equivalent transformations are claim encompassed by the present invention.

Claims (4)

  1. 1. 一种铈基抛光液残留物的清洗方法,包括以下步骤:1)采用体积比为HNO3 : H2O2 : H2O = 1 : 1 : 1的酸性溶液清洗零件表面残留的铈基抛光粉;2)用纯水喷淋的方式清洗从步骤1)中取出的零件,清洗5min;3)量取纯水600ml,称取乙二胺四乙酸8g和氢氧化钠3. 5_4g,并完全溶解于所述600ml纯水中;4)取步骤幻中已经配制好的溶液稀释至2-5倍纯水中,放置电炉上煮沸;5)将步骤幻中洗好的零件放入步骤4)的溶液中煮沸;6)用纯水喷淋的方式清洗从步骤幻中取出的零件,清洗5min,即完成铈基抛光液残留物的清洗。 CLAIMS 1. A method of cleaning a cerium-based polishing liquid residues, comprising the following steps: 1) The volume ratio HNO3: H2O2: H2O = 1: 1: 1 acid solution washing parts of surface residual cerium-based polishing powder; 2) washed with pure water shower manner withdrawn from step 1) parts, washed 5min; 3) an amount of 600ml of pure water, weighed ethylenediamine tetraacetic acid and sodium hydroxide 8g 3. 5_4g, and completely dissolved in the 600ml of pure water; 4) have been prepared to take the step of magic to 2-5 times the diluted solution is purified water, placed in an electric furnace to boil; 5) step 4 Add the washed parts in phantom step) was boiled ; 6) withdrawn from the washing step with pure water shower parts in phantom way, cleaning 5min, i.e., cerium-based polishing solution to complete the cleaning residue.
  2. 2.如权利要求1所述一种铈基抛光液残留物的新型清洗方法,其特征在于:步骤1)中所述酸性溶液清洗的时间为1-1.证。 1 2. The novel method of cleaning residue cerium-based polishing solution as claimed in claim, wherein: said step 1) in an acidic solution washing time is 1-1 card.
  3. 3.如权利要求1所述一种铈基抛光液残留物的新型清洗方法,其特征在于:步骤2)中所述纯水的温度为40-50°C。 The cleaning method of a novel cerium-based polishing liquid residue claim, wherein: in step 2) the water temperature is 40-50 ° C.
  4. 4.如权利要求1所述一种铈基抛光液残留物的新型清洗方法,其特征在于:步骤4)中所述溶液煮沸时间为3-5min。 1 4. The method of cleaning a novel cerium-based polishing liquid residue claim, wherein: step 4), the solution was boiled time was 3-5min.
CN 201110430321 2011-12-15 2011-12-15 Method for cleaning cerium-based polishing solution residues CN102517594B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1603470A (en) * 2004-11-04 2005-04-06 上海华虹(集团)有限公司 Metal front contact hole cleaning process
US20050126588A1 (en) * 2003-11-04 2005-06-16 Carter Melvin K. Chemical mechanical polishing slurries and cleaners containing salicylic acid as a corrosion inhibitor
CN102044474A (en) * 2009-10-13 2011-05-04 中芯国际集成电路制造(上海)有限公司 Surface treatment method of copper metal layer subjected to chemically mechanical polishing
CN102179390A (en) * 2010-11-25 2011-09-14 西安北方捷瑞光电科技有限公司 Method for cleaning ultra-smooth surface

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050126588A1 (en) * 2003-11-04 2005-06-16 Carter Melvin K. Chemical mechanical polishing slurries and cleaners containing salicylic acid as a corrosion inhibitor
CN1603470A (en) * 2004-11-04 2005-04-06 上海华虹(集团)有限公司 Metal front contact hole cleaning process
CN102044474A (en) * 2009-10-13 2011-05-04 中芯国际集成电路制造(上海)有限公司 Surface treatment method of copper metal layer subjected to chemically mechanical polishing
CN102179390A (en) * 2010-11-25 2011-09-14 西安北方捷瑞光电科技有限公司 Method for cleaning ultra-smooth surface

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