WO2018120808A1 - Chem-mechanical polishing liquid for barrier layer - Google Patents

Chem-mechanical polishing liquid for barrier layer Download PDF

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WO2018120808A1
WO2018120808A1 PCT/CN2017/094309 CN2017094309W WO2018120808A1 WO 2018120808 A1 WO2018120808 A1 WO 2018120808A1 CN 2017094309 W CN2017094309 W CN 2017094309W WO 2018120808 A1 WO2018120808 A1 WO 2018120808A1
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polishing liquid
mechanical polishing
chemical mechanical
liquid according
acid
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PCT/CN2017/094309
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French (fr)
Chinese (zh)
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姚颖
潘依君
荆建芬
杜玲曦
蔡鑫元
宋凯
杨俊雅
张建
王春梅
王雨春
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安集微电子科技（上海）股份有限公司
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Publication of WO2018120808A1 publication Critical patent/WO2018120808A1/en

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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
    • C23F3/04—Heavy metals
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/08—Etching
    • C30B33/10—Etching in solutions or melts
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/30604—Chemical etching

Definitions

  • the invention relates to the field of semiconductor manufacturing, and in particular to a chemical mechanical polishing liquid which can be applied to the planarization of a barrier layer.
  • CMP chemical mechanical polishing
  • the CMP process uses an abrasive-containing mixture and a polishing pad to polish the surface of the integrated circuit.
  • the substrate is placed in direct contact with a rotating polishing pad and a load is applied to the backside of the substrate with a load.
  • 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
  • CN1400266 discloses an alkaline barrier polishing liquid comprising a silica abrasive, an amine compound and a nonionic surfactant.
  • CN101372089A discloses an alkaline barrier polishing liquid containing silica abrasive, corrosion inhibitor, oxidant, nonionic fluorosurfactant, aromatic sulfonic acid oxidant compound , the polishing rate of the barrier layer is low, and the polishing efficiency is low;
  • CN101012356A discloses an acidic barrier polishing liquid comprising an oxidizing agent, a silica particle partially covered with aluminum, an inhibitor and a complexing agent, and a copper metal layer There is severe corrosion
  • CN101747843A discloses a copper chemical mechanical polishing liquid containing abrasive particles, a complexing agent, an oxidizing agent, a block polyether surfactant and water, wherein the function of the block polyether is to inhibit copper removal. The rate does not involve the polishing effect of low dielectric materials.
  • a barrier polishing capable of being suitable for a low dielectric material-copper interconnection process is sought, and a high barrier removal rate and a low dielectric can be achieved under milder conditions.
  • the process stop characteristics of the electrical material interface, and the chemical mechanical polishing liquid which can well control the dishing, metal corrosion and surface contaminants are urgently solved in the industry.
  • the present invention provides a barrier chemical mechanical polishing liquid having high barrier material, dielectric layer material removal rate and adjustable low dielectric layer material, and copper removal under milder conditions. Rate, and can well control the dishing, Erosion, metal corrosion, and surface contamination during polishing.
  • the present invention provides a chemical mechanical polishing liquid for barrier layer planarization comprising abrasive particles, an azole compound, a complexing agent, a nonionic surfactant, and an oxidizing agent, wherein the nonionic surface active agent
  • the agent is a block polyether compound.
  • the abrasive particles are silica particles; the mass percentage of the abrasive particles is preferably from 2 to 20%, more preferably from 5 to 15%; and the particle size of the abrasive particles is preferably from 10 to 250nm, More preferably, it is 50 to 200 nm.
  • the azole compound is preferably selected from one or more of the group consisting of benzotriazole, methylbenzotriazole, 5-phenyltetrazolium, 5-amino-tetrazene Oxazole, nonylphenyltetrazolium, benzimidazole, naphthotriazole and 2-mercapto-benzothiazole.
  • the mass percentage concentration of the azole compound is preferably 0.001 to 1%, more preferably 0.01 to 0.5%.
  • the complexing agent is selected from one or more of an organic carboxylic acid, an organic phosphonic acid, an amino acid and an organic amine, preferably selected from one or more of the following: acetic acid, propionic acid, oxalic acid, Malonic acid, succinic acid, citric acid, ethylenediaminetetraacetic acid, 2-phosphonic acid butane-1,2,4-tricarboxylic acid, aminotrimethylenephosphonic acid, hydroxyethylidene diphosphonic acid, ethylene
  • concentration of the above-mentioned complexing agent is preferably 0.001 to 2%, more preferably 0.01 to 1%, based on the amine tetramethylene phosphonic acid, glycine and ethylenediamine.
  • the block polyether compound is a polyoxyethylene-polyoxypropylene-polyoxyethylene triblock polyether.
  • the block polyether compound has the following chemical formula: (CH 2 CH 2 O)x-(CH(CH 3 )CH 2 O)y-(CH 2 CH 2 O)z-OH, which can also be expressed as (EO X-(PO)y-(EO)z wherein 10 ⁇ x, y, z ⁇ 150.
  • the mass percentage concentration of the block polyether surfactant is preferably 0.001 to 1.0%, more preferably 0.01 to 0.5%.
  • the oxidizing agent is selected from one or more of the group consisting of hydrogen peroxide, peracetic acid, potassium persulfate and ammonium persulfate, preferably hydrogen peroxide.
  • the mass percentage of the oxidizing agent is preferably from 0.01 to 5%, more preferably from 0.1 to 2%.
  • the chemical mechanical polishing liquid has a pH of 8.0 to 12.0, more preferably 9.0 to 11.0.
  • the chemical mechanical polishing liquid of the present invention may further contain other additives in the field such as a pH adjuster and a bactericide.
  • the chemical mechanical polishing liquid of the present invention can be prepared by concentration, diluted with deionized water in use, and added with an oxidizing agent to the concentration range of the present invention.
  • the technical advantage of the present invention is that it has a high barrier material, a removal rate of the dielectric layer material, and an adjustable low dielectric material, copper removal rate under milder conditions; It can well control dishing, Erosion, metal corrosion and reduce surface contamination during polishing. It can be concentrated and prepared for convenient storage. Storage and transportation and use.
  • Table 1 shows the comparative polishing liquids 1-2 and the polishing liquids 1 to 13 of the present invention, according to the formulation given in the table, the components other than the oxidizing agent are uniformly mixed, and adjusted to the desired pH with KOH or HNO3. value. Add oxidizing agent before use and mix well. Water is the balance.
  • the comparative polishing liquids 1 to 2 and the polishing liquids 1 to 9 of the present invention were used for copper (Cu), barrier material tantalum (Ta), dielectric material silicon dioxide (TEOS), and low dielectric material (BD) under the following conditions.
  • the polishing liquid of the present invention can obtain a higher removal rate of the barrier material Ta and the dielectric material silicon dioxide (TEOS) than the comparative polishing liquids 1 and 2, which can shorten the polishing time and increase the productivity.
  • the removal rate of the low dielectric material BD is controlled to be lower than that of TEOS, which is advantageous for controlling the polishing process of the graphic chip and the remaining thickness of the BD after polishing, and ensuring The surface uniformity of the chip.
  • the patterned copper wafer was polished using the comparative polishing liquid 2 and the polishing liquids 1 to 3 of the present invention under the following conditions.
  • the graphics chip is a commercially available 12-inch Sematech 754 graphics chip.
  • the film material is copper/germanium/tantalum nitride/TEOS/BD from top to bottom.
  • the polishing process is divided into three steps. The first step is to remove the commercially available copper polishing solution. Most of the copper, the second step uses a commercially available copper polishing solution to remove residual copper, and the third step uses the barrier polishing fluid of the present invention to remove the barrier layer (tantalum/niobium nitride), silicon dioxide TEOS, and partially low.
  • the dielectric material BD is removed and stopped on the BD layer.
  • the polishing machine is a 12" Reflexion LK machine
  • the polishing pad is Fujibo pad
  • the lower pressure is 1.5 psi
  • the polishing liquid flow rate is 300 ml/min. Polishing time is 70s.
  • Dishing mentioned above refers to a dish-shaped recess on a metal pad before the barrier layer is polished
  • Erosion refers to a dense-line region (50% copper/50% dielectric) having a barrier layer width of 0.18 ⁇ m and a density of 50%.
  • the dielectric layer on the layer is eroded, and ⁇ (Angstrom) refers to the corrected ability value after polishing.
  • the polishing liquid of the present invention can stop the polishing process of the graphic chip by suppressing the removal rate of the low dielectric material BD. And to ensure the remaining thickness of the polished BD, it can better correct the dishing and erosion generated on the wafer by the precursor (after copper polishing), and obtain a better crystal round appearance.
  • the patterned copper wafer was polished using the comparative polishing liquid 1 and the polishing liquid 1 under the following conditions.
  • the graphics chip is a commercially available 12-inch Sematech 754 graphics chip with film material from top to bottom
  • the following is copper / tantalum / tantalum nitride / TEOS / BD
  • the polishing process is divided into three steps, the first step to remove most of the copper with a commercially available copper polishing solution, the second step with a commercially available copper polishing solution to remove residual copper
  • the barrier layer yttrium/niobium nitride
  • the silicon dioxide TEOS silicon dioxide TEOS
  • a portion of the low dielectric material BD are removed and stopped on the BD layer by the barrier polishing liquid of the present invention.
  • Fig. 1 and Fig. 2 are SEM images of the surface topography of the Sematech 754 pattern test wafer after polishing of the polishing liquid 1 and the polishing liquid 1, respectively. It can be seen from the comparison that the polishing liquid of the invention effectively inhibits metal corrosion, especially the copper wire region, and the graphic test wafer is polished and polished, and the surface is still clear and sharp, no metal is found. Corrosion phenomenon, and no pollution particles remain.

Abstract

Provided is a chem-mechanical polishing liquid for planarization of a barrier layer, comprising abrasive particles, an azole compound, a complexing agent, a nonionic surfactant and an oxygenant, wherein the nonionic surfactant is a block polyether compound. The chem-mechanical polishing liquid has a high removal rate for barrier materials and dielectric materials, and a adjustable removal rate for low dielectric materials and copper under mild conditions, and can control well the generation of dish down, dielectric layer corrosion and metallic corrosion, and decrease surface pollutants, and the polished wafer is characterized by excellent morphology.

Description

一种用于阻挡层的化学机械抛光液Chemical mechanical polishing liquid for barrier layer 技术领域Technical field
本发明涉及半导体制造领域，尤其涉及一种可应用于阻挡层平坦化的化学机械抛光液。The invention relates to the field of semiconductor manufacturing, and in particular to a chemical mechanical polishing liquid which can be applied to the planarization of a barrier layer.
背景技术Background technique
目前，在集成电路制造中，随着互连技术的标准的不断提高、互连层数不断增加、工艺特征尺寸不断缩小，对硅片表面平整度的要求也越来越高。如果不能实现平坦化，在半导体晶圆上创建复杂和密集的结构就会是非常有限的。At present, in the manufacture of integrated circuits, as the standards of interconnect technology continue to increase, the number of interconnect layers continues to increase, and the size of process features continues to shrink, the requirements for the flatness of the surface of silicon wafers are also increasing. If flattening is not possible, creating complex and dense structures on semiconductor wafers can be very limited.
目前，化学机械抛光方法(CMP)是可实现整个硅片平坦化的最有效的方法。CMP工艺就是使用一种含磨料的混合物和抛光垫抛光集成电路表面。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，用一载重物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薄膜发生化学反应开始进行抛光过程。Currently, chemical mechanical polishing (CMP) is the most effective way to achieve planarization of the entire wafer. The CMP process uses an abrasive-containing mixture and a polishing pad to polish the surface of the integrated circuit. In a typical chemical mechanical polishing process, the substrate is placed in direct contact with a rotating polishing pad and a load is applied to the backside of the substrate with a load. During polishing, 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. The polished film undergoes a chemical reaction to begin the polishing process.
随着集成电路技术向超深亚微米(32、28nm)方向发展，因特征尺寸减小而导致的寄生电容愈加严重的影响着电路的性能，为减小这一影响，就必须采用低介电材料来降低相邻金属线之间的寄生电容，目前较多采用低介电材料为BD(Black Diamond)，在CMP过程中除了要严格控制表面污染物指标以及杜绝金属腐蚀外，还要具有较低的碟型凹陷和抛光均一性才能保证更加可靠的电性能，特别是阻挡层的平坦化过程中需要在更短的时间和更低的压力下快速移除阻挡层金属，封盖氧化物并能很好的停止在低介电材料表面，形成互连线，而且对小尺寸图形不敏感。这就对CMP提出了更高的挑 战，因为通常低介电材料为掺杂碳的二氧化硅，要控制停止层的残留厚度，就要有很强的选择比的调控能力，还要有很高的稳定性和易清洗等特征。As integrated circuit technology develops toward ultra-deep sub-micron (32, 28 nm), the parasitic capacitance caused by the reduced feature size is increasingly severely affecting the performance of the circuit. To reduce this effect, low dielectric must be used. Materials to reduce the parasitic capacitance between adjacent metal lines. Currently, low dielectric materials are used for BD (Black Diamond). In addition to strict control of surface pollutants and metal corrosion in the CMP process, Low dishing and polishing uniformity ensure more reliable electrical performance, especially in the planarization of the barrier layer, which requires quick removal of the barrier metal in a shorter time and lower pressure, capping the oxide and It can stop well on the surface of low dielectric materials, form interconnects, and is not sensitive to small size patterns. This raises a higher pick for CMP Battle, because the low dielectric material is usually carbon-doped silica, to control the residual thickness of the stop layer, it is necessary to have a strong selection ratio control ability, and also has high stability and easy cleaning characteristics. .
目前市场上已存在许多应用于阻挡层平坦化的化学机械抛光液，如，CN1400266公开一种碱性阻挡层抛光液，该抛光液包含二氧化硅磨料，胺类化合物和非离子表面活性剂，其在抛光后，会对铜金属层产生腐蚀；CN101372089A公开一种碱性阻挡层抛光液，其含有二氧化硅磨料，腐蚀抑制剂，氧化剂，非离子氟表面活性剂，芳族磺酸氧化剂化合物，其对阻挡层抛光速率较低，抛光效率低；CN101012356A公开一种酸性阻挡层抛光液，其包含氧化剂，部分被铝覆盖的二氧化硅颗粒，抑制剂和络合剂，其对铜金属层存在严重的腐蚀，CN101747843A公开了一种铜化学机械抛光液，其含有研磨颗粒，络合剂，氧化剂，嵌段聚醚类表面活性剂和水，其中嵌段聚醚的作用是抑制铜的去除速率，未涉及低介电材料的抛光效果。There are many chemical mechanical polishing liquids on the market that are used for the planarization of barrier layers. For example, CN1400266 discloses an alkaline barrier polishing liquid comprising a silica abrasive, an amine compound and a nonionic surfactant. After polishing, it will corrode the copper metal layer; CN101372089A discloses an alkaline barrier polishing liquid containing silica abrasive, corrosion inhibitor, oxidant, nonionic fluorosurfactant, aromatic sulfonic acid oxidant compound , the polishing rate of the barrier layer is low, and the polishing efficiency is low; CN101012356A discloses an acidic barrier polishing liquid comprising an oxidizing agent, a silica particle partially covered with aluminum, an inhibitor and a complexing agent, and a copper metal layer There is severe corrosion, CN101747843A discloses a copper chemical mechanical polishing liquid containing abrasive particles, a complexing agent, an oxidizing agent, a block polyether surfactant and water, wherein the function of the block polyether is to inhibit copper removal. The rate does not involve the polishing effect of low dielectric materials.
因此，针对现有技术中存在的问题，寻求一种能够适合于低介电材料-铜互连制程中的阻挡层抛光，并可在较温和的条件下实现高的阻挡层去除速率和低介电材料界面的工艺停止特性，同时能很好的控制碟型凹陷、金属腐蚀和表面污染物的化学机械抛光液是本行业亟待解决解决的问题。Therefore, in view of the problems in the prior art, a barrier polishing capable of being suitable for a low dielectric material-copper interconnection process is sought, and a high barrier removal rate and a low dielectric can be achieved under milder conditions. The process stop characteristics of the electrical material interface, and the chemical mechanical polishing liquid which can well control the dishing, metal corrosion and surface contaminants are urgently solved in the industry.
发明内容Summary of the invention
为解决上述问题，本发明提供一种阻挡层化学机械抛光液，其在较温和的条件下具有高的阻挡层材料、介电层材料去除速率和可调的低介电层材料、铜的去除速率，并能在抛光过程中很好的控制碟型形凹陷(Dishing)、介质层侵蚀(Erosion)、金属腐蚀的产生，以及减少表面污染物。In order to solve the above problems, the present invention provides a barrier chemical mechanical polishing liquid having high barrier material, dielectric layer material removal rate and adjustable low dielectric layer material, and copper removal under milder conditions. Rate, and can well control the dishing, Erosion, metal corrosion, and surface contamination during polishing.
具体地，本发明提供了一种用于阻挡层平坦化的化学机械抛光液，其包含研磨颗粒、唑类化合物、络合剂、非离子表面活性剂和氧化剂，其中，所述非离子表面活性剂为嵌段聚醚类化合物。Specifically, the present invention provides a chemical mechanical polishing liquid for barrier layer planarization comprising abrasive particles, an azole compound, a complexing agent, a nonionic surfactant, and an oxidizing agent, wherein the nonionic surface active agent The agent is a block polyether compound.
其中，所述研磨颗粒为二氧化硅颗粒；研磨颗粒的质量百分比浓度较佳的为2～20％，更佳的为5～15％；所述的研磨颗粒的粒径较佳的为10～250nm， 更佳的为50～200nm。Wherein, the abrasive particles are silica particles; the mass percentage of the abrasive particles is preferably from 2 to 20%, more preferably from 5 to 15%; and the particle size of the abrasive particles is preferably from 10 to 250nm, More preferably, it is 50 to 200 nm.
其中，所述唑类化合物，较佳的选自下列中的一种或多种：苯并三氮唑、甲基苯并三氮唑、5-苯基四氮唑、5-氨基-四氮唑、巯基苯基四氮唑、苯并咪唑，萘并***和2-巯基-苯并噻唑。所述的唑类化合物的质量百分比浓度较佳的为0.001～1％，更佳的为0.01～0.5％。Wherein the azole compound is preferably selected from one or more of the group consisting of benzotriazole, methylbenzotriazole, 5-phenyltetrazolium, 5-amino-tetrazene Oxazole, nonylphenyltetrazolium, benzimidazole, naphthotriazole and 2-mercapto-benzothiazole. The mass percentage concentration of the azole compound is preferably 0.001 to 1%, more preferably 0.01 to 0.5%.
其中，所述络合剂选自有机羧酸、有机膦酸、氨基酸和有机胺中的一种或多种，较佳的选自下列中的一种或多种：乙酸、丙酸、草酸、丙二酸、丁二酸、柠檬酸、乙二胺四乙酸、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，甘氨酸和乙二胺，所述的络合剂的质量百分比的浓度较佳的为0.001～2％，更佳的为0.01～1％。Wherein the complexing agent is selected from one or more of an organic carboxylic acid, an organic phosphonic acid, an amino acid and an organic amine, preferably selected from one or more of the following: acetic acid, propionic acid, oxalic acid, Malonic acid, succinic acid, citric acid, ethylenediaminetetraacetic acid, 2-phosphonic acid butane-1,2,4-tricarboxylic acid, aminotrimethylenephosphonic acid, hydroxyethylidene diphosphonic acid, ethylene The concentration of the above-mentioned complexing agent is preferably 0.001 to 2%, more preferably 0.01 to 1%, based on the amine tetramethylene phosphonic acid, glycine and ethylenediamine.
其中，所述嵌段聚醚类化合物为聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段聚醚。所述嵌段聚醚类化合物具有以下化学式：(CH2CH2O)x-(CH(CH3)CH2O)y-(CH2CH2O)z-OH，也可表示为(EO)x-(PO)y-(EO)z其中，10≤x，y，z≤150。所述嵌段聚醚类表面活性剂的质量百分比浓度较佳的为0.001～1.0％，更佳的为0.01～0.5％。Wherein the block polyether compound is a polyoxyethylene-polyoxypropylene-polyoxyethylene triblock polyether. The block polyether compound has the following chemical formula: (CH 2 CH 2 O)x-(CH(CH 3 )CH 2 O)y-(CH 2 CH 2 O)z-OH, which can also be expressed as (EO X-(PO)y-(EO)z wherein 10≤x, y, z≤150. The mass percentage concentration of the block polyether surfactant is preferably 0.001 to 1.0%, more preferably 0.01 to 0.5%.
其中，氧化剂选自下列中的一种或多种：过氧化氢、过氧乙酸，过硫酸钾和过硫酸铵，较佳地为过氧化氢。所述的氧化剂的质量百分比浓度较佳的为0.01～5％，更佳的为0.1～2％。Wherein the oxidizing agent is selected from one or more of the group consisting of hydrogen peroxide, peracetic acid, potassium persulfate and ammonium persulfate, preferably hydrogen peroxide. The mass percentage of the oxidizing agent is preferably from 0.01 to 5%, more preferably from 0.1 to 2%.
其中，所述的化学机械抛光液的pH值为8.0～12.0，更佳的为9.0～11.0。The chemical mechanical polishing liquid has a pH of 8.0 to 12.0, more preferably 9.0 to 11.0.
另外，本发明的化学机械抛光液还可以包含pH调节剂和杀菌剂等其他本领域添加剂。Further, the chemical mechanical polishing liquid of the present invention may further contain other additives in the field such as a pH adjuster and a bactericide.
且，本发明的化学机械抛光液可以浓缩制备，使用时用去离子水稀释并添加氧化剂至本发明的浓度范围使用。Further, the chemical mechanical polishing liquid of the present invention can be prepared by concentration, diluted with deionized water in use, and added with an oxidizing agent to the concentration range of the present invention.
与现有技术相比较，本发明的技术优势在于：其在较温和的条件下具有高的阻挡层材料、介电层材料的去除速率和可调的低介电材料、铜的去除速率；其能在抛光过程中很好的控制碟型形凹陷(Dishing)、介质层侵蚀(Erosion)、金属腐蚀的产生，以及减少表面污染物。其可浓缩制备，方便储 存以及运输和使用。Compared with the prior art, the technical advantage of the present invention is that it has a high barrier material, a removal rate of the dielectric layer material, and an adjustable low dielectric material, copper removal rate under milder conditions; It can well control dishing, Erosion, metal corrosion and reduce surface contamination during polishing. It can be concentrated and prepared for convenient storage. Storage and transportation and use.
具体实施方式detailed description
下面通过实施例的方式进一步说明本发明，但并不以此将本发明限制在所述的实施例范围之中。The invention is further illustrated by the following examples, which are not intended to limit the invention.
表1给出了对比抛光液1～2和本发明的抛光液1～13，按表中所给的配方，将除氧化剂以外的其他组分混合均匀，用KOH或HNO3调节到所需要的pH值。使用前加氧化剂，混合均匀即可。水为余量。Table 1 shows the comparative polishing liquids 1-2 and the polishing liquids 1 to 13 of the present invention, according to the formulation given in the table, the components other than the oxidizing agent are uniformly mixed, and adjusted to the desired pH with KOH or HNO3. value. Add oxidizing agent before use and mix well. Water is the balance.
表1对比抛光液1～2和本发明的抛光液1～13Table 1 Comparative polishing liquid 1 to 2 and polishing liquid 1 to 13 of the present invention
Figure PCTCN2017094309-appb-000001
Figure PCTCN2017094309-appb-000001
Figure PCTCN2017094309-appb-000002
Figure PCTCN2017094309-appb-000002
效果实施例1Effect Example 1
采用对比抛光液1～2和本发明的抛光液1～9按照下述条件对铜(Cu)、阻挡层材料钽(Ta)、介电材料二氧化硅(TEOS)和低介电材料(BD)进行抛光。抛光条件：抛光机台为12”Reflexion LK机台，抛光垫为Fujibo pad，下压力为1.5psi，转速为抛光盘/抛光头＝113/107rpm，抛光液流速为300ml/min，抛光时间为1min。The comparative polishing liquids 1 to 2 and the polishing liquids 1 to 9 of the present invention were used for copper (Cu), barrier material tantalum (Ta), dielectric material silicon dioxide (TEOS), and low dielectric material (BD) under the following conditions. ) Polishing. Polishing conditions: polishing machine is 12" Reflexion LK machine, polishing pad is Fujibo pad, lower pressure is 1.5 psi, rotation speed is polishing plate / polishing head = 113/107 rpm, polishing liquid flow rate is 300ml/min, polishing time is 1min .
表2对比抛光液1～2和本发明抛光液1～9对铜(Cu)、钽(Ta)、二氧化硅(TEOS)和低介电材料(BD)的去除速率Table 2 Comparison of removal rates of copper (Cu), tantalum (Ta), silicon dioxide (TEOS) and low dielectric material (BD) by polishing liquid 1 to 2 and polishing liquid 1 to 9 of the present invention
Figure PCTCN2017094309-appb-000003
Figure PCTCN2017094309-appb-000003
由表2可见，与对比抛光液1与2相比，本发明的抛光液可以获得较高的阻挡层材料Ta和介电材料二氧化硅(TEOS)的去除速率，可以缩短抛光时间，提高产能，同时通过添加不同量的嵌段聚醚类化合物表面活性剂，将低介电材料BD的去除速率控制在比TEOS低，有利于控制图形芯片的抛光过程和抛光后的BD剩余厚度，并保证芯片的表面均一性。It can be seen from Table 2 that the polishing liquid of the present invention can obtain a higher removal rate of the barrier material Ta and the dielectric material silicon dioxide (TEOS) than the comparative polishing liquids 1 and 2, which can shorten the polishing time and increase the productivity. At the same time, by adding different amounts of block polyether compound surfactants, the removal rate of the low dielectric material BD is controlled to be lower than that of TEOS, which is advantageous for controlling the polishing process of the graphic chip and the remaining thickness of the BD after polishing, and ensuring The surface uniformity of the chip.
效果实施例2 Effect Example 2
采用对比抛光液2和本发明的抛光液1～3按照下述条件对带有图案的铜晶片进行抛光。该图形芯片为市售的12英寸Sematech754图形芯片，膜层材料从上至下为铜/钽/氮化钽/TEOS/BD，抛光过程分三步，第一步用市售的铜抛光液去除大部分的铜，第二步用市售的铜抛光液去除残留的铜，第三步用本发明的阻挡层抛光液将阻挡层(钽/氮化钽)、二氧化硅TEOS、和部分低介电材料BD去除并停在BD层上。阻挡层抛光液抛光条件：抛光机台为12”Reflexion LK机台，抛光垫为Fujibo pad，下压力为1.5psi，转速为抛光盘/抛光头＝113/107rpm，抛光液流速为300ml/min，抛光时间为70s。The patterned copper wafer was polished using the comparative polishing liquid 2 and the polishing liquids 1 to 3 of the present invention under the following conditions. The graphics chip is a commercially available 12-inch Sematech 754 graphics chip. The film material is copper/germanium/tantalum nitride/TEOS/BD from top to bottom. The polishing process is divided into three steps. The first step is to remove the commercially available copper polishing solution. Most of the copper, the second step uses a commercially available copper polishing solution to remove residual copper, and the third step uses the barrier polishing fluid of the present invention to remove the barrier layer (tantalum/niobium nitride), silicon dioxide TEOS, and partially low. The dielectric material BD is removed and stopped on the BD layer. Barrier polishing solution polishing conditions: the polishing machine is a 12" Reflexion LK machine, the polishing pad is Fujibo pad, the lower pressure is 1.5 psi, the rotation speed is polishing disk / polishing head = 113/107 rpm, and the polishing liquid flow rate is 300 ml/min. Polishing time is 70s.
表3对比抛光液2和本发明抛光液1～3对带有图案的铜晶片抛光后的矫正能力对比Table 3 Comparison of the correction ability of the polishing liquid 2 and the polishing liquid 1 to 3 of the present invention after polishing the patterned copper wafer
Figure PCTCN2017094309-appb-000004
Figure PCTCN2017094309-appb-000004
其中，上文中所述Dishing，是指阻挡层抛光前在金属垫上的碟型凹陷，Erosion是指阻挡层在线宽为0.18微米，密度为50％的密线区域(50％铜/50％介电层)上的介质层侵蚀，Δ(埃)是指抛光后的矫正能力值。Wherein, Dishing mentioned above refers to a dish-shaped recess on a metal pad before the barrier layer is polished, and Erosion refers to a dense-line region (50% copper/50% dielectric) having a barrier layer width of 0.18 μm and a density of 50%. The dielectric layer on the layer is eroded, and Δ (Angstrom) refers to the corrected ability value after polishing.
由表3可以看出，与对比抛光液2相比，本发明的抛光液由于抑制了低介电材料BD的去除速率，能很好地停止在BD上，有效的控制了图形芯片的抛光过程和保证了抛光后的BD剩余厚度，能较好的修正前程(铜抛光后)在晶圆上产生的碟型凹陷和侵蚀，获得了较好的晶圆形貌。As can be seen from Table 3, compared with the comparative polishing liquid 2, the polishing liquid of the present invention can stop the polishing process of the graphic chip by suppressing the removal rate of the low dielectric material BD. And to ensure the remaining thickness of the polished BD, it can better correct the dishing and erosion generated on the wafer by the precursor (after copper polishing), and obtain a better crystal round appearance.
效果实施例3Effect Example 3
采用对比抛光液1和抛光液1按照下述条件对带有图案的铜晶片进行抛光。该图形芯片为市售的12英寸Sematech754图形芯片，膜层材料从上至 下为铜/钽/氮化钽/TEOS/BD，抛光过程分三步，第一步用市售的铜抛光液去除大部分的铜，第二步用市售的铜抛光液去除残留的铜，第三步用本发明的阻挡层抛光液将阻挡层(钽/氮化钽)、二氧化硅TEOS、和部分低介电材料BD去除并停在BD层上。The patterned copper wafer was polished using the comparative polishing liquid 1 and the polishing liquid 1 under the following conditions. The graphics chip is a commercially available 12-inch Sematech 754 graphics chip with film material from top to bottom The following is copper / tantalum / tantalum nitride / TEOS / BD, the polishing process is divided into three steps, the first step to remove most of the copper with a commercially available copper polishing solution, the second step with a commercially available copper polishing solution to remove residual copper In the third step, the barrier layer (yttrium/niobium nitride), the silicon dioxide TEOS, and a portion of the low dielectric material BD are removed and stopped on the BD layer by the barrier polishing liquid of the present invention.
图1和图2分别采用对比抛光液1和抛光液1抛光后Sematech 754图形测试晶圆的表面形貌的SEM图。对比可以看出，本发明的抛光液有效的抑制了金属腐蚀，特别是对铜线区域有很好的保护，图形测试晶圆经过本发明的抛光液抛光后，表面仍然清晰锐利，未发现金属腐蚀现象，且无污染颗粒残留。Fig. 1 and Fig. 2 are SEM images of the surface topography of the Sematech 754 pattern test wafer after polishing of the polishing liquid 1 and the polishing liquid 1, respectively. It can be seen from the comparison that the polishing liquid of the invention effectively inhibits metal corrosion, especially the copper wire region, and the graphic test wafer is polished and polished, and the surface is still clear and sharp, no metal is found. Corrosion phenomenon, and no pollution particles remain.
应当注意的是，本发明的实施例有较佳的实施性，且并非对本发明作任何形式的限制，任何熟悉该领域的技术人员可能利用上述揭示的技术内容变更或修饰为等同的有效实施例，但凡未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所作的任何修改或等同变化及修饰，均仍属于本发明技术方案的范围内。 It should be noted that the embodiments of the present invention are preferred embodiments, and are not intended to limit the scope of the present invention. Any one skilled in the art may use the above-disclosed technical contents to change or modify the equivalent embodiments. Any modification or equivalent changes and modifications of the above embodiments in accordance with the technical spirit of the present invention are still within the scope of the technical solutions of the present invention.

Claims (19)

  1. 一种用于阻挡层平坦化的化学机械抛光液，其特征在于，包括研磨颗粒、唑类化合物、络合剂、非离子表面活性剂和氧化剂，其中，所述非离子表面活性剂为嵌段聚醚类化合物。A chemical mechanical polishing liquid for barrier layer planarization, comprising: abrasive particles, an azole compound, a complexing agent, a nonionic surfactant, and an oxidizing agent, wherein the nonionic surfactant is a block Polyether compound.
  2. 如权利要求1所述的化学机械抛光液，其特征在于，所述研磨颗粒为二氧化硅颗粒，所述研磨颗粒的质量百分比浓度为2～20％，所述的研磨颗粒的粒径较佳的为10～250nm。The chemical mechanical polishing liquid according to claim 1, wherein said abrasive particles are silica particles, said abrasive particles have a mass percentage concentration of 2 to 20%, and said abrasive particles preferably have a particle diameter. It is 10 to 250 nm.
  3. 如权利要求2所述的化学机械抛光液，其特征在于，所述研磨颗粒的质量百分比浓度为5～15％，所述研磨颗粒的粒径为50～200nm。The chemical mechanical polishing liquid according to claim 2, wherein said abrasive particles have a mass percentage concentration of 5 to 15%, and said abrasive particles have a particle diameter of 50 to 200 nm.
  4. 如权利要求1所述的化学机械抛光液，其特征在于，所述唑类化合物选自苯并三氮唑、甲基苯并三氮唑、5-苯基四氮唑、5-氨基-四氮唑、巯基苯基四氮唑、苯并咪唑，萘并***和2-巯基-苯并噻唑中的一种或多种。The chemical mechanical polishing liquid according to claim 1, wherein the azole compound is selected from the group consisting of benzotriazole, methylbenzotriazole, 5-phenyltetrazolium, 5-amino-tetra One or more of azole, nonylphenyltetrazolium, benzimidazole, naphthotriazole and 2-mercapto-benzothiazole.
  5. 如权利要求1或4所述的化学机械抛光液，其特征在于，所述唑类化合物的质量百分比浓度为0.001～1％。The chemical mechanical polishing liquid according to claim 1 or 4, wherein the azole compound has a mass percentage concentration of 0.001 to 1%.
  6. 如权利要求5所述的化学机械抛光液，其特征在于，所述唑类化合物的质量百分比浓度为0.01～0.5％。The chemical mechanical polishing liquid according to claim 5, wherein the azole compound has a mass percentage concentration of 0.01 to 0.5%.
  7. 如权利要求1所述的化学机械抛光液，其特征在于，所述络合剂选自有机羧酸、有机膦酸、氨基酸和有机胺中的一种或多种。The chemical mechanical polishing liquid according to claim 1, wherein the complexing agent is selected from one or more of an organic carboxylic acid, an organic phosphonic acid, an amino acid, and an organic amine.
  8. 如权利要求7所述的化学机械抛光液，其特征在于，所述络合剂选自乙酸、丙酸、草酸、丙二酸、丁二酸、柠檬酸、乙二胺四乙酸、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，甘氨酸和乙二胺中的一种或多种。The chemical mechanical polishing liquid according to claim 7, wherein said complexing agent is selected from the group consisting of acetic acid, propionic acid, oxalic acid, malonic acid, succinic acid, citric acid, ethylenediaminetetraacetic acid, and 2-phosphine. One or more of butane-1,2,4-tricarboxylic acid, aminotrimethylenephosphonic acid, hydroxyethylidene diphosphonic acid, ethylenediaminetetramethylenephosphonic acid, glycine and ethylenediamine.
  9. 如权利要求1或7或8所述的化学机械抛光液，其特征在于，所述络合剂的质量百分比的浓度为0.001～2％。The chemical mechanical polishing liquid according to claim 1 or 7 or 8, wherein the concentration of the complexing agent is 0.001 to 2% by mass.
  10. 如权利要求9所述的化学机械抛光液，其特征在于，所述络合剂的质量百分比的浓度为0.01～1％。The chemical mechanical polishing liquid according to claim 9, wherein the concentration of the complexing agent is 0.01 to 1% by mass.
  11. 如权利要求1所述的化学机械抛光液，其特征在于，所述嵌段聚醚类化合 物为聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段聚醚。The chemical mechanical polishing liquid according to claim 1, wherein said block polyether compound The material is a polyoxyethylene-polyoxypropylene-polyoxyethylene triblock polyether.
  12. 如权利要求11所述的化学机械抛光液，其特征在于，所述嵌段聚醚类化合物具有以下化学式：(CH2CH2O)x-(CH(CH3)CH2O)y-(CH2CH2O)z-OH，其中，10≤x，y，z≤150。The chemical mechanical polishing liquid according to claim 11, wherein said block polyether compound has the following chemical formula: (CH 2 CH 2 O) x-(CH(CH 3 )CH 2 O)y-( CH 2 CH 2 O)z-OH, wherein 10≤x, y, z≤150.
  13. 如权利要求1或11或12所述的化学机械抛光液，其特征在于，所述嵌段聚醚类化合物的质量百分比浓度为0.001～1.0％。The chemical mechanical polishing liquid according to claim 1 or 11 or 12, wherein the block polyether compound has a mass percentage concentration of 0.001 to 1.0%.
  14. 如权利要求13所述的化学机械抛光液，其特征在于，所述嵌段聚醚类化合物的质量百分比浓度为0.01～0.5％。The chemical mechanical polishing liquid according to claim 13, wherein the block polyether compound has a mass percentage concentration of 0.01 to 0.5%.
  15. 如权利要求1所述的化学机械抛光液，其特征在于，所述氧化剂选自过氧化氢、过氧乙酸，过硫酸钾和过硫酸铵中的一种或多种。The chemical mechanical polishing liquid according to claim 1, wherein the oxidizing agent is selected from one or more of hydrogen peroxide, peracetic acid, potassium persulfate and ammonium persulfate.
  16. 如权利要求1或15所述的化学机械抛光液，其特征在于，所述氧化剂的质量百分比浓度为0.01～5％。The chemical mechanical polishing liquid according to claim 1 or 15, wherein the oxidizing agent has a mass percentage concentration of 0.01 to 5%.
  17. 如权利要求16所述的化学机械抛光液，其特征在于，所述氧化剂的质量百分比浓度为0.1～2％。The chemical mechanical polishing liquid according to claim 16, wherein the oxidizing agent has a mass percentage concentration of 0.1 to 2%.
  18. 如权利要求1所述的化学机械抛光液，其特征在于，所述化学机械抛光液的pH值为8.0～12.0。The chemical mechanical polishing liquid according to claim 1, wherein the chemical mechanical polishing liquid has a pH of from 8.0 to 12.0.
  19. 如权利要求18所述的化学机械抛光液，其特征在于，所述化学机械抛光液的pH值为9.0～11.0。 The chemical mechanical polishing liquid according to claim 18, wherein the chemical mechanical polishing liquid has a pH of 9.0 to 11.0.
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