WO2015096631A1 - 一种用于铝的化学机械抛光液及使用方法 - Google Patents

一种用于铝的化学机械抛光液及使用方法 Download PDF

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WO2015096631A1
WO2015096631A1 PCT/CN2014/093685 CN2014093685W WO2015096631A1 WO 2015096631 A1 WO2015096631 A1 WO 2015096631A1 CN 2014093685 W CN2014093685 W CN 2014093685W WO 2015096631 A1 WO2015096631 A1 WO 2015096631A1
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acid
polishing liquid
liquid according
aluminum
polishing
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PCT/CN2014/093685
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English (en)
French (fr)
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荆建芬
张建
蔡鑫元
宋凯
邱腾飞
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安集微电子（上海）有限公司
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09G—POLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00—Polishing compositions
    • C09G1/02—Polishing compositions containing abrasives or grinding agents
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23F—NON-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
    • C23F3/00—Brightening metals by chemical means
    • C23F3/02—Light metals
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23F—NON-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
    • C23F3/00—Brightening metals by chemical means
    • C23F3/02—Light metals
    • C23F3/03—Light metals with acidic solutions

Definitions

  • the present invention relates to a chemical mechanical polishing liquid, and more particularly to a polishing liquid for polishing metal aluminum.
  • Integrated circuits typically include millions of activated electronic components. These activating electronic components are mounted in a silicon substrate by a multi-layer metallized interconnect layer connector that is interconnected by metallized vias and contacts to form a complete functional circuit and component.
  • Metal interconnects or contacts are formed during the fabrication of the semiconductor by forming a pattern in the dielectric layer, forming trenches or holes by etching, depositing metal in the trenches, and then removing the dielectric layer by a planarization process Excess metal is applied and the deposited metal surface is flattened to form metal vias or contacts.
  • planarization technology has become one of the indispensable key technologies that are as important and interdependent as lithography and etching.
  • the chemical mechanical polishing (CMP) process is currently the most effective and mature planarization technology.
  • the chemical mechanical polishing system is a chemical mechanical planarization technology that integrates cleaning, drying, on-line detection, and endpoint detection technologies. It is the development of integrated circuits to be finer, multi-layered, flattened, and thinner, and integrated circuits to improve production efficiency. The necessary technology to reduce costs and global wafer flattening.
  • the CMP process uses an abrasive-containing mixture and a polishing pad to polish the wafer surface.
  • the substrate is brought into direct contact with a rotating polishing pad to apply pressure on the back side of the substrate.
  • the gasket and the table rotate while maintaining a downward force on the back of the substrate, applying abrasive and chemically active solutions (often referred to as polishing fluids or polishing slurries) to the gasket.
  • polishing fluids or polishing slurries abrasive and chemically active solutions
  • the selection of the slurry composition is an important step in the CMP step.
  • the active component of the slurry slurry reacts with the substrate to be polished, thereby changing Change the polishing effect.
  • the selection of a suitable polishing slurry not only accelerates the polishing rate of the substrate, but also effectively improves the surface flatness of the substrate, so that the integrated circuit has better operational performance. Therefore, different polishing pastes are required for different substrates to enhance the polishing effect of the substrate.
  • the silicon dioxide layer of the transistor has been reduced to only one tenth of the former, with only five oxygen atoms. It is.
  • the silicon dioxide layer can no longer be further reduced, otherwise the leakage current will make the transistor not work properly.
  • a transistor made of a high-k material plus a metal gate can reduce the source-to-drain leakage current by more than 5 times, the gate oxide dielectric leakage current by more than 10 times, and the transistor efficiency by 20%.
  • Chinese patent CN1238812A, US Pat. No. 7,186,654 B2, and US US20080200098A1 each provide a chemical mechanical polishing slurry for polishing aluminum.
  • the polishing slurry in the above patents contains a strong oxidizing agent such as ammonium persulfate, and alumina as abrasive particles.
  • ammonium persulfate is unstable, the on-line service life is short, and these strong oxidizing substances are difficult to control, causing excessive corrosion of aluminum or the substrate; and in order to remove the thick aluminum oxide layer produced by these strong oxidants.
  • U.S. Patent No. 5,209,816 A provides a polishing slurry for aluminum which effectively increases the polishing rate of aluminum. However, since the pH of the slurry is small, corrosion of aluminum is caused, and the surface flatness of the substrate is low.
  • the present invention discloses a chemical mechanical polishing for aluminum.
  • This polishing liquid contains at least one metal ion.
  • the addition of metal ions allows the polishing liquid of the present invention to have a higher removal rate of aluminum.
  • the polishing liquid in the present invention may further contain at least one complexing agent and one abrasive particle.
  • the complexing agent is an organic acid, an organic phosphonic acid and an aminocarboxylic acid compound
  • the organic acid is acetic acid, oxalic acid, citric acid, tartaric acid, malonic acid, succinic acid, malic acid, lactic acid, gallic acid and sulfosalicylic acid.
  • the organic phosphonic acid is 2-phosphonic acid butane-1,2,4-tricarboxylic acid, aminotrimethylene phosphonic acid, hydroxyethylidene diphosphonic acid, ethylenediamine tetramethyl
  • diphosphonic acid diethylenetriamine pentamethylphosphonic acid, 2-hydroxyphosphonic acid acetic acid, ethylenediaminetetramethylenephosphonic acid, and polyaminopolyether methylphosphonic acid
  • Aminocarboxylate selected from the group consisting of glycine, alanine, valine, leucine, valine, phenylalanine, tyrosine, tryptophan, lysine, arginine, histidine, serine , aspartic acid, threonine, glutamic acid, asparagine, glutamine, ammonia triacetic acid, ethylenediaminetetraacetic acid, cyclohexanetetraacetic acid, ethylenedi
  • the metal cation should include a standard electrochemical redox potential that is higher than the material to be polished. That is, the standard electrode potential of the metal cation in the present invention is greater than -1.66 V, preferably copper ion, silver ion, iron ion, etc., when the above metal cation is added to the polishing liquid in the form of a salt, the matching anion is Sulfate, nitric acid Salt, phosphate, carbonate, etc.
  • the concentration of the metal ions is from 1 to 1000 ppm. Preferably 5 to 500 ppm
  • the abrasive particles in the present invention are metal oxide particles commonly used in the art, and are silica, doped aluminum or aluminum-coated silica, alumina, ceria, titania and/or polymer abrasive particles. Silica is preferred.
  • the weight percentage of the abrasive particles is preferably from 0.1 to 20% by weight; more preferably from 0.2 to 5% by weight.
  • the abrasive particles have a particle diameter of 20 to 200 nm, preferably 20 to 120 nm.
  • the polishing liquid of the present invention preferably has a pH of from 3 to 10.
  • the metal cation in the polishing liquid according to the present invention is different from the metal cation in the prior art, it is not a catalyst as an oxidizing agent, and therefore, preferably, The polishing liquid of the present invention does not contain an oxidizing agent such as hydrogen peroxide.
  • the polishing liquid of the present invention can be prepared as a concentrated sample, and can be diluted with deionized water before use.
  • the positive progressive effect of the present invention is that the chemical mechanical polishing liquid of the present invention does not need to add an additional oxidizing agent, and only by adding a specific metal ion and a complexing agent to the silica abrasive particles, the aluminum can be made higher.
  • the polishing rate avoids problems such as surface scratching caused by alumina abrasive particles and oxidizing agents, and reduces production costs.
  • Table 1 shows Examples 1 to 46 of the chemical mechanical polishing liquid of the present invention. According to the formulation given in the table, all the components were uniformly mixed, and the mass percentage was made up to 100% with water. Adjust to the desired pH with KOH or HNO 3 . The percentages described below are all percentage by mass.
  • the chemical reagents used in the formulation are all commercially available.
  • Table 2 shows the chemical mechanical polishing liquid examples and comparative formulations of the present invention. According to the formula given in the table, mix all the components evenly and make up the mass percentage to 100% with water. Adjust to the desired pH with KOH or HNO3. The percentages described below are all percentage by mass. The chemical reagents used in the formulation are all commercially available.
  • Empty sheet polishing conditions 2 inch aluminum wafer, polishing machine for Logitech LP50, lower pressure 3 psi, polishing disc and polishing head speed 70/65 rpm, polishing pad IC1010, polishing liquid flow rate 50 ml/min, polishing time 1 min.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

本发明揭示了一种用于铝的化学机械抛光。这种抛光液至少含有一种金属离子。金属离子的加入，使本发明的抛光液可以有较高的铝的去除速率。

Description

一种用于铝的化学机械抛光液及使用方法 技术领域
本发明涉及一种化学机械抛光液，尤其涉及一种用于抛光金属铝的抛光液。
技术背景
集成电路一般包括数百万个活化电子元件。这些活化电子元件通过多层金属化的互连层连接件安装在硅基材中，这些原本互相分离的活化电子元件通过金属化的通路和触点连接，从而形成完整的功能电路和部件。在半导体的制造过程中通过以下步骤形成金属互连线路或触点：在介电层中形成图案，通过蚀刻形成沟槽或孔，在沟槽中沉积金属，然后通过平坦化工艺去除介电层上多余的金属，并使得沉积的金属表面平整，从而形成金属通路或触点。
在整个半导体基材的抛光工艺中，平坦化技术已成为与光刻和刻蚀同等重要、且相互依赖的不可缺少的关键技术之一。而化学机械抛光(CMP)工艺便是目前最有效、最成熟的平坦化技术。化学机械抛光系统是集清洗、干燥、在线检测、终点检测等技术于一体的化学机械平坦化技术，是集成电路向微细化、多层化、平坦化、薄型化发展，和集成电路提高生产效率、降低成本、晶圆全局平坦化的必备技术。CMP工艺就是使用一种含磨料的混合物和抛光垫抛光晶圆表面。在典型的化学机械抛光方法中，将衬底直接与旋转抛光垫接触，在衬底背面施加压力。在抛光期间，垫片和操作台旋转，同时在衬底背面保持向下的力，将磨料和化学活性溶液(通常称为抛光液或抛光浆料)涂于垫片上，该抛光液与正在抛光的晶圆薄膜发生化学反应开始进行抛光过程。
而在化学机械抛光工艺中，浆料组合物的选择则是CMP步骤中一个重要步骤，使用时，抛光物浆料的有效成分会与被抛光基材发生反应，从而改 变抛光效果。选用合适的抛光浆料，不仅可以加速基材的抛光速率，还可有效提高基材表面平整度，使得集成电路拥有更好的运作性能。因而针对不同的基材，需要选用不同的抛光浆料，从而增强基材的抛光效果。
铝电阻率低，易于沉积和刻蚀，是最早被使用的生产线后端(back-end-of-the-line)的金属互连材料。而在生产线前端(front-end-of-the-line),随着集成电路工业的进一步发展，晶体管的二氧化硅层已经缩小到只有前者的十分之一，仅有5个氧原子的厚度了。作为阻隔栅极和下层的绝缘体，二氧化硅层已经不能再进一步缩小了，否则产生的漏电流会让晶体管无法正常工作。采用高-k材料加金属栅极制成的晶体管可以使源极到漏极的漏电流下降5倍以上，栅极氧化物介电质的漏电流降低10倍以上，晶体管的效能提高20％，这样的组合在45nm以下制程高度集成化的数以亿计的芯片上，每个晶体管单元都有如此幅度的提升，将突破物理效能提升的瓶颈。传统的多晶硅栅与高k材料不匹配，而铝金属栅可以和新的高k材料相兼容。因此需要开发适合这个前端铝金属栅抛光的抛光液和抛光工艺。
在对铝抛光过程中，因铝的硬度较小，为了获得良好的抛光效果，目前已有了一系列对于含有铝的基材适用的抛光液的研究。
如中国专利CN1238812A、美国专利US7186654B2、美国US20080200098A1均提供了用于抛光铝的化学机械抛光的浆料，然而上述专利中的抛光浆料均含有如过硫酸铵等强氧化剂，氧化铝作为研磨颗粒，在实际抛光过程中，过硫酸铵不稳定，在线使用寿命短，而且这些强氧化性物质难以控制，使得铝或是基材发生过度腐蚀；而为了去除由这些强氧化剂产生的厚的氧化铝层，必须使用氧化铝作为研磨颗粒，致使铝的表面出现凹陷使基材的表面出现刮痕等，严重影响基材的平整度，并且在抛光过程中，铝的抛光速率低。美国专利US5209816A提供了一种用于铝的抛光浆料，有效地提高了铝的抛光速率，然而因其浆料的pH值较小，造成铝的腐蚀，基材的表面平整度低。
同时，现有技术的化学机械抛光液中，经常会使用金属离子来促进例如铜或钨的抛光速率，例如US6541384中公开了一种用于抛光铜的抛光液，含有氧化剂，二价铜离子，有机酸及唑类化合物。然而，需要注意的是，二价铜离子作为氧化剂的催化剂，并不直接参与于金属材料的氧化还原反应。同时，现有技术中也存在使用金属离子来促进非金属材料抛光速率的先例，但是金属离子的加入，是为了改变研磨颗粒的zeta电位，避免研磨颗粒发生团聚，或者使之更容易与被抛光材料表面作用而促进抛光速率。在现有技术中，尚未有针对金属阳离子与抛光基材之间直接影响的研究。
发明概要
本发明揭示了一种用于铝的化学机械抛光。这种抛光液至少含有一种金属离子。金属离子的加入，使本发明的抛光液可以有较高的铝的去除速率。
本发明中的抛光液，进一步还可含有至少一种络合剂和一种研磨颗粒。
其中，络合剂为有机酸、有机膦酸和氨羧化合物，有机酸为醋酸、草酸、柠檬酸、酒石酸、丙二酸、丁二酸、苹果酸、乳酸、没食子酸和磺基水杨酸中的一种或多种；所述的有机膦酸为2-膦酸丁烷-1，2，4-三羧酸、氨基三甲叉膦酸、羟基乙叉二膦酸、乙二胺四甲叉膦酸、二乙烯三胺五甲叉膦酸、2-羟基膦酸基乙酸、乙二胺四甲叉膦酸和多氨基多醚基甲叉膦酸中的一种或多种；所述的氨羧化合物选自甘氨酸、丙氨酸、缬氨酸、亮氨酸、脯氨酸、苯丙氨酸、酪氨酸、色氨酸、赖氨酸、精氨酸、组氨酸、丝氨酸、天冬氨酸、苏氨酸、谷氨酸、天冬酰胺、谷氨酰胺、氨三乙酸、乙二胺四乙酸、环己烷四乙酸、乙二胺二琥珀酸、二乙烯三胺五乙酸和三乙烯四胺六乙酸中的一种或多种；络合剂的含量为重量百分比0.05～10wt％，较佳为0.1～3wt％。
本领域技术人员可以轻易理解的是，金属阳离子应包括具有比待抛光的材料高的标准电化学氧化还原电位。即本发明中的金属阳离子的标准电极电位大于-1.66V，优选为铜离子、银离子、铁离子等，上述金属阳离子以盐的形式加入抛光液中时，针对相应金属阳离子，匹配的阴离子为硫酸盐、硝酸 盐、磷酸盐、碳酸盐等。所述的金属离子的浓度为1～1000ppm。优选为5～500ppm
本发明中研磨颗粒为本领域常用的金属氧化物颗粒，为二氧化硅、掺杂铝或覆盖铝的二氧化硅、氧化铝、二氧化铈、二氧化钛和/或高分子研磨颗粒。较佳为二氧化硅。研磨颗粒的重量百分比浓度较佳为0.1～20wt％；更佳为0.2～5wt％。研磨颗粒的粒径为20～200nm，较佳为20～120nm。
本发明的抛光液的pH值较佳为3～10。
本发明的浆料中还可以包括其他常用添加剂如pH调节剂，粘度调节剂，消泡剂等来达到抛光效果。
且需要说明的是，如之前在背景技术中所述，由于本发明所涉及的抛光液中的金属阳离子，与现有技术中金属阳离子的作用不同，并不是作为氧化剂的催化剂，因此优选地，本发明的抛光液中不含有例如双氧水等氧化剂。
本发明的抛光液可以制备浓缩样，使用前用去离子水稀释即可。
本发明的积极进步效果在于：本发明的化学机械抛光液中不需要添加额外氧化剂，仅需通过在二氧化硅研磨颗粒中加入特定的金属离子及络合剂，即可使铝具有较高的抛光速率，避免了采用氧化铝研磨颗粒和氧化剂带来的表面划伤等问题，并降低了生产成本。
发明内容
下面通过具体实施例进一步阐述本发明的优点，但本发明的保护范围不仅仅局限于下述实施例。
实施例1～46
表1给出了本发明的化学机械抛光液的实施例1～46，按表中所给配方，将所有组分混合均匀，用水补足质量百分比至100％。用KOH或HNO3调节到所需要的pH值。以下所述百分含量均为质量百分比含量。配方中所用化学试剂均为市面采购。
表1 抛光液实施例1～46
Figure PCTCN2014093685-appb-000001
Figure PCTCN2014093685-appb-000002
效果实施例
表2给出了本发明的化学机械抛光液实施例和对比例配方。按表中所给配方，将所有组分混合均匀，用水补足质量百分比至100％。用KOH或HNO3调节到所需要的pH值。以下所述百分含量均为质量百分比含量。配方中所用化学试剂均为市面采购。
采用对比抛光液和本发明的抛光液，对空片铝(Al)晶片进行抛光。所得的铝的抛光速率见表2。
空片抛光条件：2inch铝晶片，抛光机台为Logitech LP50,下压力3psi,抛光盘及抛光头转速70/65rpm，抛光垫IC1010，抛光液流速50ml/min，抛光时间1min。
表2 本发明的化学机械抛光液实施例与对比例的配方及铝去除速率
Figure PCTCN2014093685-appb-000003
由表2可知，与未加金属离子的对比例1和2相比，实施例47～60中添加了不同种类和浓度的金属离子后，铝的去除速率大大提高。
由对比例3与实施例48相比可知，在该体系中加入氧化剂双氧水后，将大大降低铝的去除速率。
应当理解的是，本发明所述wt％均指的是质量百分含量。
以上对本发明的具体实施例进行了详细描述，但其只是作为范例，本发明并不限制于以上描述的具体实施例。对于本领域技术人员而言，任何对本发明进行的等同修改和替代也都在本发明的范畴之中。因此，在不脱离本发明的精神和范围下所作的均等变换和修改，都应涵盖在本发明的范围内。

Claims (17)

  1. 一种用于铝的化学机械抛光液，其特征在于，至少含有一种金属离子。
  2. 如权利要求1所述的抛光液，其特征在于，所述金属离子的标准电极电势大于-1.66V。
  3. 如权利要求2所述的抛光液，其特征在于，所述金属离子为铜离子、银离子、铁离子中的一种或多种。
  4. 如权利要求1所述的抛光液，其特征在于，所述金属离子的浓度为1～1000ppm。
  5. 如权利要求4所述的抛光液，其特征在于，所述金属离子的浓度为5～500ppm。
  6. 如权利要求1所述的抛光液，其特征在于，还至少含有一种研磨颗粒和一种络合剂。
  7. 如权利要求6所述的抛光液，其特征在于，所述络合剂选自有机酸、有机膦酸和氨羧化合物中的一种或多种。
  8. 如权利要求7所述的抛光液，其特征在于，所述有机酸为醋酸、草酸、柠檬酸、酒石酸、丙二酸、丁二酸、苹果酸、乳酸、没食子酸和磺基水杨酸中的一种或多种；所述有机膦酸为2-膦酸丁烷-1，2，4-三羧酸、氨基三甲叉膦酸、羟基乙叉二膦酸、乙二胺四甲叉膦酸、二乙烯三胺五甲叉膦酸、2-羟基膦酸基乙酸、乙二胺四甲叉膦酸和多氨基多醚基甲叉膦酸中的一种或多种；所述氨羧化合物选自甘氨酸、丙氨酸、缬氨酸、亮氨酸、脯氨酸、苯丙氨酸、酪氨酸、色氨酸、赖氨酸、精氨酸、组氨酸、丝氨酸、天冬氨酸、苏氨酸、谷氨酸、天冬酰胺、谷氨酰胺、氨三乙酸、乙二胺四乙酸、环己烷四乙酸、乙二胺二琥珀酸、二乙烯三胺五乙酸和三乙烯四胺六乙酸中的一种或多种。
  9. 如权利要求6所述的抛光液，其特征在于，所述络合剂的浓度为质量百分比0.05～10％。
  10. 如权利要求9所述的抛光液，其特征在于，所述络合剂的浓度为质量百分比0.1～3％
  11. 如权利要求6所述的抛光液，其特征在于，所述研磨颗粒为二氧化硅、掺杂铝或覆盖铝的二氧化硅、氧化铝、二氧化铈、二氧化钛和/或高分子研磨颗粒。
  12. 如权利要求11所述的抛光液，其特征在于，所述研磨颗粒为二氧化硅。
  13. 如权利要求6所述的抛光液，其特征在于，所述研磨颗粒的浓度为重量百分比0.1～20％。
  14. 如权利要求13所述的抛光液，其特征在于，所述研磨颗粒的浓度为重量百分比0.2～5％。
  15. 如权利要求6所述的抛光液，其特征在于，所述研磨颗粒的粒径为20～200nm。
  16. 如权利要求15所述的抛光液，其特征在于，所述研磨颗粒的粒径为20～120nm。
  17. 如权利要求1或6所述的抛光液，其特征在于，所述抛光液的pH值为3～10。
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