CN115418623A - 治具保护下真空提拉泵辅助清洗喷淋头孔洞的方法 - Google Patents

治具保护下真空提拉泵辅助清洗喷淋头孔洞的方法 Download PDF

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CN115418623A
CN115418623A CN202210365872.2A CN202210365872A CN115418623A CN 115418623 A CN115418623 A CN 115418623A CN 202210365872 A CN202210365872 A CN 202210365872A CN 115418623 A CN115418623 A CN 115418623A
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shower head
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高敏刚
贺贤汉
陈日升
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Anhui Fullerde Technology Development Co ltd
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    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4401Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
    • C23C16/4407Cleaning of reactor or reactor parts by using wet or mechanical methods
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F3/00Brightening metals by chemical means
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/04Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
    • C23G1/06Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
    • C23G1/061Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors nitrogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/04Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
    • C23G1/06Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
    • C23G1/063Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors heterocyclic compounds
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    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45563Gas nozzles
    • C23C16/45565Shower nozzles

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Abstract

本发明公开了治具保护下真空提拉pump(泵)辅助清洗shower head(喷淋头孔洞),通过真空提拉pump(泵)反复抽吸药液对shower head(喷淋头孔洞)每个孔洞的均匀冲洗,真空提拉起到面板每个孔洞沉积物彻底去除,也使面板表面通过真空提拉的推动更加均匀,使面板孔径最小的变异改变,以来面板延长清洗次数,同时也大量的降低客户库存需求和买进新品的成本。

Description

治具保护下真空提拉泵辅助清洗喷淋头孔洞的方法
技术领域
本发明涉及治具保护下真空提拉pump(泵)辅助清洗shower head(喷淋头孔洞)的方法。
背景技术
CVD 制程把气体和气相材料引进反应器内,原材料扩散穿越边界层和接触基片的表面,随着吸附原材料的移动在基片的表面产生了化学反应,避免CVD制程在打入gas气体的时候产生不良反应或不均匀反应,shower head(喷淋头孔洞)起到关键性的作用,因此对shower head(喷淋头孔洞)的清洗要求非常的高,目前国内清洗行业清洗shower head(喷淋头孔洞),一般采用防酸胶带保护,再用一般的化学方法去除沉积物。
现有的清洗方法很容易造成shower head(喷淋头孔洞)孔径腐蚀,导致孔径之间大小偏差极大以及对面板损害,大大降低使用寿命。
发明内容
针对上述问题,本发明的提供一种方法:治具保护下真空提拉pump(泵)辅助清洗shower head(喷淋头孔洞)的方法,所述的治具包括子槽和真空提拉pump(泵),清洗步骤如下:
步骤1,测子槽平行度,将待清洗的shower head(喷淋头孔洞)放入子槽,加上盖子,用螺栓锁紧;
步骤2,子槽中加入混合酸,连接真空提拉pump(泵),反复抽吸30分钟;
步骤3,纯水反复抽吸后将shower head(喷淋头孔洞)放入超声波清洗槽,水温65℃,超声清洗12分钟;
步骤4,测量及数据收集。
作为本发明的进一步改进,所述步骤2的混合酸配比是,H3PO4为80ml/L,HCl为120ml/L,NaNO3为70g/L,NH4Cl为10g/L,草酸为5g/L,添加剂为25ml/L,其余为水;将各原料混合在65℃环境下搅拌8分钟。
作为本发明的进一步改进,添加剂的组成为:氯化钠3g/L, PEG10000 12.5g/L,尿素8g/L,乌洛托品5g/L,磺基水杨酸4g/L,氨基磺酸4g/L。
本发明的有益效果是:本方法通过真空提拉pump(泵)反复抽吸药液对showerhead(喷淋头孔洞)每个孔洞的均匀冲洗,真空提拉起到面板每个孔洞沉积物彻底去除,也使面板表面通过真空提拉的推动更加均匀,使面板孔径最小的变异改变,提高了孔洞的耐蚀性和表面平整度,同时也大量的降低客户库存需求和买进新品的成本。
附图说明:
图1为本方法清洗后选取30个孔测量孔径的数据表。
图2为添加剂正交试验表。
具体实施方式
治具保护下真空提拉pump(泵)辅助清洗shower head(喷淋头孔洞)的方法,所述的治具包括子槽和真空提拉pump(泵),清洗步骤如下:
步骤1,测子槽平行度,将待清洗的shower head(喷淋头孔洞)放入子槽,加上盖子,用螺栓锁紧;
步骤2,子槽中加入混合酸,连接真空提拉pump(泵),反复抽吸30分钟;
步骤3,纯水反复抽吸后将shower head(喷淋头孔洞)放入超声波清洗槽,水温65℃,超声清洗12分钟;
步骤4,测量及数据收集。
图1所示,清洗后选取30个孔进行测量的结果符合要求。
混合酸配比是,H3PO4为80ml/L,HCl为120ml/L,NaNO3为70g/L,NH4Cl为10g/L,草酸为5g/L,添加剂为25ml/L,其余为水;将各原料混合在65℃环境下搅拌8分钟。
混合酸去除氧化膜及抛光的配方中盐酸主要起浸蚀作用,磷酸表现为抛光作用,络合剂的添加有助于其与Cr3+, Fe3+络合,防止腐蚀产物沉积覆盖在部件表面,阻碍氧化膜去除以及抛光,氧化剂硝酸钠改变氧化膜结构,使其疏松,被剥落。与传统的铬酸配方和环保的双氧水配方相比较,本发明的配方去除速率快了几乎1000倍,而抛光效果通过失重分析、粗糙度分析和反射率分析,发现抛光效果基本得出的混合酸体系配方光洁度最好,粗糙度最小,去除氧化膜效率最快。
通过电化学测试分析,发现配方中盐酸的含量必须大于70m1/L,因为低浓度盐酸情况下,部件表面的活性低,氧化膜溶解较慢,并且实验过程中有气体不断生成,使体系动荡不稳定,只有盐酸浓度大于或等于70m1/L,才会稳定,部件表面保持活性,氧化膜持续溶解,盐酸的去除能力与浓度呈正比。双氧水体系和铬酸体系中氧化剂双氧水和铬酸有较强的钝化能力,有利于抛光但不利于去除氧化膜。
溶液中存在盐酸等酸性介质,很容易腐蚀金属基体,所以加入鸟洛托品,尿素作为缓蚀剂,降低金属基体的腐蚀,其中PEG 10000是表面活性剂,调节粘度,加快去除速率,尿素液可以起增溶作用,磺基水杨酸作为光亮剂,提高抛光效果,少量的氯化钠可以防止灰白;首先在前面各因素的基础体系中,选取一定范围的添加剂浓度做了各个添加成分浓度正交试验,选出最优组合,然后进行整体添加剂浓度筛选,各成分添加剂实验结果如图2所示。
通过正交优化实验得出各个添加剂组合使用去膜效率最高的浓度为实验2的浓度,添加剂的浓度为:氯化钠3g/L, PEG10000 12.5g/L,尿素8g/L,乌洛托品5g/L,磺基水杨酸4g/L,氨基磺酸4g/L。
以上对本发明的实施方式作了说明,但是本发明不限于上述实施方式,在所属技术领域普通技术人员所具备的知识范围内,还可以在不脱离本发明宗旨的前提下做出各种变化。

Claims (3)

1.治具保护下真空提拉pump(泵)辅助清洗shower head(喷淋头孔洞)的方法,其特征是:所述的治具包括子槽和真空提拉pump(泵),清洗步骤如下:
步骤1,测子槽平行度,将待清洗的shower head(喷淋头孔洞)放入子槽,加上盖子,用螺栓锁紧;
步骤2,子槽中加入混合酸,连接真空提拉pump(泵),反复抽吸30分钟;
步骤3,纯水反复抽吸后将shower head(喷淋头孔洞)放入超声波清洗槽,水温65℃,超声清洗12分钟;
步骤4,测量及数据收集。
2.根据权利要求1所述的治具保护下真空提拉pump(泵)辅助清洗shower head(喷淋头孔洞)的方法,其特征是:所述步骤2的混合酸配比是,H3PO4为80ml/L,HCl为120ml/L,NaNO3为70g/L,NH4Cl为10g/L,草酸为5g/L,添加剂为25ml/L,其余为水;将各原料混合在65℃环境下搅拌8分钟。
3.根据权利要求2所述的治具保护下真空提拉pump(泵)辅助清洗shower head(喷淋头孔洞)的方法,其特征是:添加剂的组成为:氯化钠3g/L, PEG10000 12.5g/L,尿素8g/L,乌洛托品5g/L,磺基水杨酸4g/L,氨基磺酸4g/L。
CN202210365872.2A 2022-04-08 2022-04-08 治具保护下真空提拉泵辅助清洗喷淋头孔洞的方法 Pending CN115418623A (zh)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102513313A (zh) * 2011-12-29 2012-06-27 中微半导体设备(上海)有限公司 具有碳化硅包覆层的喷淋头的污染物处理方法
KR101455045B1 (ko) * 2013-07-29 2014-10-27 서문희 샤워 헤드의 페이스 플레이트 세정장치
CN107299348A (zh) * 2017-08-22 2017-10-27 无锡市恒利弘实业有限公司 一种环保型不锈钢抛光液及其制备方法和抛光工艺

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102513313A (zh) * 2011-12-29 2012-06-27 中微半导体设备(上海)有限公司 具有碳化硅包覆层的喷淋头的污染物处理方法
KR101455045B1 (ko) * 2013-07-29 2014-10-27 서문희 샤워 헤드의 페이스 플레이트 세정장치
CN107299348A (zh) * 2017-08-22 2017-10-27 无锡市恒利弘实业有限公司 一种环保型不锈钢抛光液及其制备方法和抛光工艺

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