CN101972753B - Method for cleaning surface of magnesium aluminum alloy subjected to chemically mechanical polishing - Google Patents

Method for cleaning surface of magnesium aluminum alloy subjected to chemically mechanical polishing Download PDF

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CN101972753B
CN101972753B CN201010231659XA CN201010231659A CN101972753B CN 101972753 B CN101972753 B CN 101972753B CN 201010231659X A CN201010231659X A CN 201010231659XA CN 201010231659 A CN201010231659 A CN 201010231659A CN 101972753 B CN101972753 B CN 101972753B
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aluminum alloy
magnesium
mechanical polishing
water
surface cleaning
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CN101972753A (en
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刘玉岭
王如
檀柏梅
徐文忠
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Hebei University of Technology
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Abstract

本发明公开了一种镁铝合金化学机械抛光后表面清洗方法,旨在提供一种能够降低镁铝合金材料碱性化学机械抛光的后续加工成本,使用方法简单易行,能够提高晶片表面质量的清洗方法。取电阻为18MΩ以上的超纯水边搅拌边加入非离子表面活性剂和FA/O螯合剂;采用电阻为18MΩ以上的超纯水稀释阻蚀剂;将稀释后的阻蚀剂边搅拌边加入到上述液体中,搅拌均匀后得到水溶性表面清洗液,使用得到的水溶性表面清洗液迅速对碱性化学机械抛光后的镁铝合金材料采用大流量低压力条件下进行抛光清洗;用电阻为18MΩ以上的超纯水在零压力、大流量条件下冲洗。The invention discloses a surface cleaning method after magnesium-aluminum alloy chemical mechanical polishing, and aims to provide a method that can reduce the subsequent processing cost of magnesium-aluminum alloy material alkaline chemical mechanical polishing, is simple and easy to use, and can improve the surface quality of wafers cleaning method. Take ultrapure water with a resistance of 18MΩ or more and add nonionic surfactant and FA/O chelating agent while stirring; use ultrapure water with a resistance of 18MΩ or more to dilute the corrosion inhibitor; add the diluted corrosion inhibitor while stirring into the above liquid, stir evenly to obtain a water-soluble surface cleaning solution, use the obtained water-soluble surface cleaning solution to quickly polish and clean the magnesium-aluminum alloy material after alkaline chemical mechanical polishing under the condition of large flow and low pressure; The ultrapure water above 18MΩ is flushed under the condition of zero pressure and large flow.

Description

Magnadure chemically mechanical polishing rear surface cleaning method
Technical field
The present invention relates to a kind of magnadure chemically mechanical polishing rear surface cleaning method.
Background technology
Magnadure is the metal with its own strategic significance.Magnadure is widely used in the Aerospace Products, and for example gear box cover and helicopter rotor annex etc. are taken turns in landing aircraft.Along with magnadure melting and manufacturing technology improve constantly, aspect almags such as tank armor part-structure spare, missile case and empennage also are used widely in national defense industry.Especially in some plane devices,, need to realize very high degree of precision, nearly flawless ultraprecise planarization process as key or vitals such as film flying, samples.And these require to have reached the limit of present single machine cut or grinding and polishing working ability, become one of " bottleneck " that the restriction association area further develops day by day.
Chemically mechanical polishing (CMP) can really make magnadure realize leveling, thereby obtains surface and higher removal speed preferably.But magnesium and aluminium all are very active metals; do not take safeguard measure timely if finish the back at CMP; surface of magnesium aluminium alloy is easy to corrode; showing as pit increases sharply; thereby destroy the surface of magnesium aluminium alloy after the polishing; therefore study magnadure chemically mechanical polishing (Chemical-Mechanical Polishing is called for short CMP) technology and throw post-processing technology and become major issue anxious to be solved.
Surface of polished clean technology as one of process for treating surface is even more important.The clean water process of washing that adopts in the production of magnadure polishing at present rear surface, because wafer surface temperature height, the energy height, surface tension is big, though polishing has stopped, but the reaction of wafer surface has the process of a hysteresis, in air, can be easy to oxidized, simple water flushing can not be avoided the skewness of polishing fluid, stain phenomenons such as metal ion, make that cleaning the back wafer surface has inhomogeneous vaporific, the roughness height, corrode inhomogeneous etc., on 8 inches chips, particle diameter greater than 0.1 micron particle more than 1000, have a strong impact on wafer surface quality, thereby caused the raising of cost in the following process and the reduction of device accuracy.
Summary of the invention
The present invention is in order to overcome weak point of the prior art, a kind of subsequent machining cost that can reduce the magnesium-aluminium alloy material alkaline chemical mechanical polishing to be provided, and using method is simple, can improve the cleaning method of wafer surface quality.
The present invention is achieved through the following technical solutions:
A kind of magnadure chemically mechanical polishing rear surface cleaning method is characterized in that, comprises the steps:
(1) the power taking resistance adds non-ionic surface active agent and FA/O chelating agent while stirring for the above ultra-pure water of 18M Ω;
(2) adopting resistance is the above ultra-pure water dilution corrosion inhibitor of 18M Ω;
(3) corrosion inhibitor after will diluting joins in the liquid that step (1) obtains while stirring, obtain water-soluble surface cleaning liquid after stirring, in the water-soluble surface cleaning liquid that obtains, the percentage by weight of non-ionic surface active agent is 1-5%, the percentage by weight of FA/O chelating agent is 0.1-5%, corrosion inhibitor is 0.01-5%, and the resistance of surplus is the above ultra-pure water of 18M Ω;
(4) use the water-soluble surface cleaning liquid that obtains in the step (3) to adopt the big flow of 1000-5000ml/min to carry out polished and cleaned under 0-0.01 atmospheric low pressure conditions to the magnesium-aluminium alloy material behind the alkaline chemical mechanical polishing rapidly, the time of polished and cleaned is 30s-3min;
(5) be that the above ultra-pure water of 18M Ω is the magnesium-aluminium alloy material flushing 30s-3min after under the big flow condition of 1000-4000ml/min step (4) being cleaned at zero pressure, flow with resistance.
Wherein, zero pressure is meant that the pressure on the Pressure gauge is zero, has only the gravity pressure of polishing disk.0-0.01 0.01 atmospheric pressure in the individual atmospheric low-pressure is meant that the numerical value on the Pressure gauge is 0.01 atmospheric pressure, does not contain gravity pressure.The pressure condition that is equivalent to 2000Pa-12000Pa.
Described non-ionic surface active agent is FA/O I type surfactant, O π-7 ((C 10H 21-C 6H 4-O-CH 2CH 2O) 7-H), O π-10 ((C 10H 21-C 6H 4-O-CH 2CH 2O) 10-H), O-20 (C 12-18H 25-37-C 6H 4-O-CH 2CH 2O) 70-H), among the JFC any.Wherein, FA/OI type surfactant is Jingling Microelectric Material Co., Ltd., Tianjin commercially available prod.
Described FA/O chelating agent is Jingling Microelectric Material Co., Ltd., Tianjin commercially available prod, and name is called ethylenediamine tetra-acetic acid four (tetrahydroxyethyl-ethylene diamine), can be abbreviated as NH 2RNH 2, its structural formula is as follows,
Figure BDA0000023514890000031
Described corrosion inhibitor is phenylpropyl alcohol triazole or hexa (methenamine).
The present invention has following technique effect:
(1) cleaning method of the present invention is after alkaline polishing is just finished, use the water-soluble surface cleaning liquid that contains non-ionic surface active agent, chelating agent, corrosion inhibitor etc. to carry out big flow polishing cleans at once, can wash away by rapidly that wafer surface is residual polishing fluid, can obtain cleaning, perfect polished surface, and, the heat that the cleaning of big flow is taken out of makes wafer each several part Temperature Distribution unanimity, the temperature high conformity, stop non-uniform corrosion, improve uniformity, thereby reduce the cost of following process, improve device yield, easy to use, simple.And the cost of water-soluble surface cleaning liquid is low, free from environmental pollution and etching apparatus.
2. clean with water-soluble surface cleaning liquid in the cleaning method of the present invention, wherein, selected non-ionic surface active agent can make the high surface tension of chip surface after polishing reduce rapidly, reduces the damage layer, improves the uniformity of wafer surface quality; Chelating agent can with wafer surface metal remained ion is reacted, generate the big molecule chelate of solubility, under big flow aqueous solution effect, breaking away from wafer surface; Corrosion inhibitor can form the unimolecule passivating film at chip surface after polishing, stops the polishing fluid of wafer surface uneven distribution to continue to form non-uniform corrosion with the matrix reaction, improves the perfection of chip surface after polishing.Use method of the present invention can improve wafer surface quality, reduce the cost of following process, improve device yield.
3, method of the present invention is carried out under low-pressure, and water-soluble surface cleaning liquid is fully contacted with clean surface, effectively takes away the pollutant under the surface clean simultaneously under the effect of the big water-soluble surface cleaning liquid of flow, improves the surface clean quality; If pressure is excessive, then can friction be arranged, the surface quality after the influence polishing to the surface.
The specific embodiment
The present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1:
(1) the power taking resistance is put into FA/O I type surfactant 100g and FA/O chelating agent 50g while stirring for the above ultra-pure water 3645g of 18M Ω.
(2) claim that 5g phenylpropyl alcohol triazole is to pour into while stirring in the liquid of step (1) after the above ultra-pure water of 18M Ω dilutes with 200g resistance, gets the water-soluble surface cleaning liquid of magnadure after stirring.
(3) the water-soluble surface cleaning liquid that uses step (2) to obtain adopt 1000ml/min flow under the condition of zero pressure (gravity pressure) to the polished and cleaned 2 minutes immediately of the magnesium-aluminium alloy material behind the alkaline chemical mechanical polishing.
(4) be that the above ultra-pure water of 18M Ω is the magnesium-aluminium alloy material flushing 30s after under the condition of 1000ml/min step (3) being cleaned at zero pressure (gravity pressure), flow with resistance, the bright and clean no corrosion figure of the magnadure wafer surface that obtains, surface roughness can reach the 3nm rank, on 8 inches chips, particle diameter greater than 0.1 micron particle less than 10.
Embodiment 2:
(1) the power taking resistance is put into JFC 100g and FA/O chelating agent 50g while stirring for the above ultra-pure water 3400g of 18M Ω.
(2) claim that the 250g hexa is to be poured into while stirring in the liquid of step (1) after the above ultra-pure water of 18M Ω dilutes with 200g resistance, gets the water-soluble surface cleaning liquid of magnadure after stirring.
(3) the water-soluble surface cleaning liquid that uses step (2) to obtain adopt 4000ml/min flow under 0.01 atmospheric pressure condition of (not containing gravity pressure) to the polished and cleaned 30s immediately of the magnesium-aluminium alloy material behind the alkaline chemical mechanical polishing.
(4) be that the above ultra-pure water of 18M Ω is the magnesium-aluminium alloy material flushing 30s after under the condition of 4000ml/min step (3) being cleaned at zero pressure (gravity pressure), flow with resistance, the bright and clean no corrosion figure of the magnadure wafer surface that obtains, surface roughness reaches the 3.2nm rank.On 8 inches chips, particle diameter greater than 0.1 micron particle less than 10.

Claims (3)

1.一种镁铝合金化学机械抛光后表面清洗方法,其特征在于,包括下述步骤:1. a surface cleaning method after magnesium-aluminum alloy chemical mechanical polishing, is characterized in that, comprises the following steps: (1)取电阻为18MΩ以上的超纯水边搅拌边加入非离子表面活性剂和FA/O螯合剂;(1) get resistance and add nonionic surfactant and FA/O chelating agent while stirring the ultrapure water more than 18MΩ; (2)采用电阻为18MΩ以上的超纯水稀释阻蚀剂;(2) Dilute the corrosion inhibitor with ultrapure water with a resistance of 18MΩ or more; (3)将稀释后的阻蚀剂边搅拌边加入到步骤(1)得到的液体中,搅拌均匀后得到水溶性表面清洗液,得到的水溶性表面清洗液中按重量百分比:非离子表面活性剂为1-5%,FA/O螯合剂为0.1-5%,阻蚀剂为0.01-5%,余量为电阻为18MΩ以上的超纯水;(3) Add the diluted corrosion inhibitor to the liquid obtained in step (1) while stirring, and stir to obtain a water-soluble surface cleaning solution. In the obtained water-soluble surface cleaning solution, by weight percentage: non-ionic surface active 1-5% of anti-corrosion agent, 0.1-5% of FA/O chelating agent, 0.01-5% of corrosion inhibitor, and the balance is ultra-pure water with resistance above 18MΩ; 所述FA/O螯合剂的结构式为:The structural formula of the FA/O chelating agent is:
Figure FDA0000072760620000011
Figure FDA0000072760620000011
(4)使用步骤(3)中得到的水溶性表面清洗液迅速对碱性化学机械抛光后的镁铝合金材料采用1000-5000ml/min的大流量在0-0.01个大气压的低压力条件下进行抛光清洗,抛光清洗的时间30s-3min;(4) Use the water-soluble surface cleaning solution obtained in step (3) to quickly perform alkaline chemical mechanical polishing on the magnesium-aluminum alloy material using a large flow rate of 1000-5000ml/min under a low pressure condition of 0-0.01 atmosphere. Polishing cleaning, polishing cleaning time 30s-3min; (5)用电阻为18MΩ以上的超纯水在零压力、流量为1000-4000ml/min的大流量条件下对步骤(4)清洗后的镁铝合金材料冲洗30s-3min。(5) Rinse the magnesium-aluminum alloy material cleaned in step (4) for 30s-3min with ultra-pure water with a resistance of 18MΩ or more under the condition of zero pressure and high flow rate of 1000-4000ml/min.
2.根据权利要求1所述的镁铝合金化学机械抛光后表面清洗方法,其特征在于,所述非离子表面活性剂为Oπ-7、Oπ-10、O-20、JFC中的任一种。2. surface cleaning method after magnesium-aluminum alloy chemical mechanical polishing according to claim 1, is characterized in that, described nonionic surfactant is any in 0 π- 7, 0 π -10, 0-20, JFC A sort of. 3.根据权利要求1所述的镁铝合金化学机械抛光后表面清洗方法,其特征在于,所述阻蚀剂为苯丙三氮唑或六亚甲基四胺。3. The method for cleaning the surface of magnesium-aluminum alloy after chemical mechanical polishing according to claim 1, wherein the corrosion inhibitor is benzotriazole or hexamethylenetetramine.
CN201010231659XA 2010-07-21 2010-07-21 Method for cleaning surface of magnesium aluminum alloy subjected to chemically mechanical polishing Expired - Fee Related CN101972753B (en)

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