WO2015096630A1 - Chemical mechanical polishing liquid for polishing cobalt barrier layer - Google Patents
Chemical mechanical polishing liquid for polishing cobalt barrier layer Download PDFInfo
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- WO2015096630A1 WO2015096630A1 PCT/CN2014/093682 CN2014093682W WO2015096630A1 WO 2015096630 A1 WO2015096630 A1 WO 2015096630A1 CN 2014093682 W CN2014093682 W CN 2014093682W WO 2015096630 A1 WO2015096630 A1 WO 2015096630A1
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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
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- the present invention relates to a chemical mechanical polishing liquid, and more particularly to a chemical mechanical polishing liquid for a cobalt barrier layer.
- 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. Copper is widely used as a metal wire because of its good electrical conductivity, but copper has a rapid migration property and easily diffuses through the dielectric layer to cause leakage between adjacent metal lines, resulting in deterioration of device characteristics and may not be able to function. effect. Therefore, a diffusion barrier layer is typically applied to the substrate prior to deposition of copper. Tantalum and tantalum nitride have been widely accepted as barrier materials in the industry.
- the grain boundary and surface scattering effects will increase the resistance, which is likely to mean the traditional TaN/Ta.
- the /Cu structure will not continue.
- the TaN barrier layer can be scaled down to about 8 nm.
- TaN deposited by ALD does not form a good bond with copper.
- Metallic cobalt is a good binder, but because it does not inhibit the diffusion of copper, a barrier layer of TaN or TiN is also required.
- the industry has begun to develop an interconnect structure with Co as a barrier material.
- the copper interconnection can only be fabricated by a damascene process, that is, a trench is formed in the first layer, a copper barrier layer and copper are filled in the trench, and a metal wire is formed and overlaid on the dielectric layer. The excess copper/copper barrier on the dielectric layer is then removed by chemical mechanical polishing leaving a single interconnect in the trench.
- CMP chemical mechanical polishing
- Chemical mechanical polishing system is a chemical mechanical planarization technology that integrates cleaning, drying, on-line detection, and end point detection. It is an integrated circuit. It is an indispensable technology for miniaturization, multi-layering, flattening, and thinning, and integrated circuits to improve production efficiency, reduce cost, and flatten wafers globally.
- 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.
- the polished wafer film undergoes a chemical reaction to begin the polishing process.
- the chemical mechanical polishing process is generally divided into three steps. The first step is to remove a large amount of copper on the surface of the substrate with a high and low removal rate with a high downforce.
- Step 2 The pressure is lowered when the barrier layer is approaching, the remaining metal copper is polished at a lower removal rate and stopped at the barrier layer, and the barrier layer and a portion of the dielectric layer and the metal copper are removed by a barrier polishing solution to achieve planarization.
- the selection of the slurry composition is an important step in the CMP step.
- the active component of the polishing slurry reacts with the substrate to be polished to 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 purpose of planarization of the barrier layer is to remove the barrier metal and dielectric material from the surface of the wafer and to control the thickness of the metal copper and the interlayer dielectric to the extent required by the process to form an interconnect. Since the novel barrier material cobalt is prone to corrosion under acidic conditions, it is necessary to develop a barrier polishing liquid compatible with cobalt materials.
- This patent is intended to provide a polishing fluid suitable for a cobalt barrier layer having a high removal rate of silicon dioxide, cobalt and tantalum nitride, and an adjustable copper rate. Moreover, corrosion of metallic cobalt and copper does not occur.
- CN1400266 discloses an alkaline barrier polishing liquid comprising a silica abrasive, an amine compound and a nonionic surfactant, however, the amine-containing alkaline polishing liquid therein is susceptible to corrosion of copper.
- CN101372089A discloses an alkaline barrier polishing fluid comprising a silica abrasive, a corrosion inhibitor, an oxidizing agent, a nonionic fluorosurfactant, an aromatic sulfonic acid oxidizing agent compound. However, the polishing layer of the polishing liquid has a lower polishing rate and a lower yield.
- CN101012356A discloses an acidic barrier polishing fluid comprising an oxidizing agent, silica particles partially covered with aluminum, an inhibitor and a complexing agent, but the acidic polishing liquid does not in fact involve polishing of cobalt.
- the present invention provides a chemical mechanical polishing fluid suitable for polishing a cobalt barrier layer comprising at least one abrasive particle, an azole compound, a complexing agent, a polyalkoxide, and an oxidizing agent.
- the abrasive particles may be abrasive particles commonly used in the art, such as silica, alumina, cerium oxide, aluminum-doped silica, and/or polymer particles; and the mass percentage of the abrasive particles is preferably 1 to 20%, more preferably 3 to 10%; the particle diameter of the abrasive particles is preferably from 20 to 200 nm, more preferably from 20 to 120 nm.
- the azole compound is preferably selected from one or more of the group consisting of benzotriazole, methylbenzotriazole, 1,2,4-triazole, 3-amino-1,2 , 4-triazole, 4-amino-1,2,4-triazole, 3,5-diamino-1,2,4-triazole, 1-hydroxy-benzotriazole, 5- Carboxy-3-amino-1,2,4-triazole, 3-amino-5-mercapto-1,2,4-triazole, 5-carboxy-benzotriazole, 5-phenyltetrazole Oxazole, 1-phenyl-5-mercapto-tetrazole, 5-acetic acid-1H-tetrazole, 5-methyl-tetrazole and 5-amino-tetrazole.
- the mass percentage concentration of the azole compound is preferably from 0.005 to 2%, more preferably from 0.01 to 1%.
- the complexing agent is one or more of an organic acid, an organic phosphoric acid and an aminocarboxylic acid compound.
- Preferred is one or more selected from the group consisting of acetic acid, propionic acid, oxalic acid, malonic acid, succinic acid, citric acid, tartaric acid, malic acid, 2-phosphonic acid butane-1, 2, 4- Tricarboxylic acid, aminotrimethylenephosphonic acid, hydroxyethylidene diphosphonic acid, ethylenediaminetetramethylenephosphonic acid, diethylenetriamine penta methylene phosphonic acid, 2-hydroxyphosphonic acid acetic acid, and more Amino polyether methylene phosphonic acid, ethylenediaminetetraacetic acid, cyclohexanetetraacetic acid, ethylenediamine disuccinic acid, diethylenetriaminepentaacetic acid and triethylenetetraamine hexaacetic acid, iminodiacetic acid, ammonia tris Acetic acid,
- the polyalkoxide is one or more of DISPERBYK-2090, DISPERBYK-2091.
- the concentration of the polyalkoxide is 0.005 to 1%, more preferably 0.01 to 0.5%.
- the oxidizing agent is preferably selected from one or more of the group consisting of hydrogen peroxide, peracetic acid, potassium persulfate and/or ammonium persulfate.
- 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 described therein has a pH of from 2.0 to 7.0, preferably from 3.0 to 5.0.
- the chemical mechanical polishing liquid of the present invention may further contain other additives in the field such as a pH adjuster, a viscosity modifier, an antifoaming agent and a bactericide to achieve a polishing effect.
- the chemical mechanical polishing liquid of the present invention can be prepared by uniformly mixing the components other than the oxidizing agent, adjusting the pH to a desired pH with a pH adjusting agent (such as KOH or HNO3), and adding an oxidizing agent before use. Mix well.
- a pH adjusting agent such as KOH or HNO3
- the polishing liquid of the present invention can prepare a concentrated sample which is diluted with deionized water to the concentration range of the present invention and added with an oxidizing agent before use.
- the reagents and starting materials used in the present invention are commercially available.
- the polishing liquid of the present invention has a high removal rate of cobalt, cerium and silicon dioxide, and the removal rate of metallic copper is adjustable.
- the polishing liquid of the present invention has a strong ability to control corrosion of metallic cobalt.
- Table 1 shows the formulation of the comparative polishing liquid and the polishing liquid of the present invention. According to the formula in the table, the components other than the oxidizing agent are simply and uniformly mixed, and the balance is water, and then adjusted to potassium hydroxide, ammonia water and nitric acid to The slurry of each example can be prepared by using a suitable pH value, and the oxidizing agent can be added before use, and the mixture can be uniformly mixed.
- polishing liquid Using a comparative polishing liquid and the polishing liquid of the present invention, copper (Cu, thickness: 15,000 angstroms), tantalum (Ta, thickness: 2,500 angstroms), silicon dioxide (TEOS, thickness: 15,000 angstroms), and cobalt (Co) were used under the following conditions.
- the polishing results are shown in Table 2.
- the cobalt wafer was vertically inserted into the comparative polishing liquid 1 and the polishing liquid 2, and the lower half 2 was immersed in the polishing liquid, and the upper half 1 was exposed outside the polishing liquid to investigate the influence of the polishing liquid on the wafer.
- the surface morphology of the wafer after being immersed was investigated using an optical microscope.
- the surface optical micrograph of the cobalt wafer after immersion in the comparative polishing liquid 1 is as shown in Fig.
- the corrosion rate of cobalt was effectively inhibited by adding a certain amount of polyalkoxides DISPERBYK-2090 and DISPERBYK-2091 in the examples compared with the comparative examples. Very good protection, showing good corrosion resistance.
- the removal rate of cobalt is slightly decreased after the addition of the polyalkoxide, the removal rate is maintained, and the removal rates of silica, cerium and copper of the polishing liquid of the present invention can be carried out by the content of each component. Adjustment, can meet the requirements of different processes.
- wt% of the present invention refers to the mass percentage.
Abstract
Description
Claims (21)
- 一种用于钴阻挡层抛光的化学机械抛光液,其特征在于,所述化学机械抛光液含有研磨颗粒、唑类化合物、络合剂、聚烷氧化物和氧化剂。A chemical mechanical polishing liquid for polishing a cobalt barrier layer, characterized in that the chemical mechanical polishing liquid contains abrasive particles, an azole compound, a complexing agent, a polyalkoxide, and an oxidizing agent.
- 如权利要求1所述的化学机械抛光液,其特征在于,所述研磨颗粒选自二氧化硅、三氧化二铝、二氧化铈、掺杂铝的二氧化硅和/或聚合物颗粒。The chemical mechanical polishing liquid according to claim 1, wherein the abrasive particles are selected from the group consisting of silica, alumina, cerium oxide, aluminum-doped silica, and/or polymer particles.
- 如权利要求1所述的化学机械抛光液,其特征在于,所述研磨颗粒的浓度为质量百分比浓度1~20%。The chemical mechanical polishing liquid according to claim 1, wherein the abrasive particles have a concentration of 1 to 20% by mass.
- 如权利要求3所述的化学机械抛光液,其特征在于,所述研磨颗粒的浓度为质量百分比浓度3~10%。The chemical mechanical polishing liquid according to claim 3, wherein the abrasive particles have a concentration of 3 to 10% by mass.
- 如权利要求1所述的化学机械抛光液,其特征在于,所述研磨颗粒的粒径为20~200nm。The chemical mechanical polishing liquid according to claim 1, wherein the abrasive particles have a particle diameter of 20 to 200 nm.
- 如权利要求5所述的化学机械抛光液,其特征在于,所述研磨颗粒的粒径为20~120nm。The chemical mechanical polishing liquid according to claim 5, wherein the abrasive particles have a particle diameter of 20 to 120 nm.
- 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下列中的一种或多种:苯并三氮唑、甲基苯并三氮唑、1,2,4-三氮唑、3-氨基-1,2,4-三氮唑、4-氨基-1,2,4-三氮唑、3,5-二氨基-1,2,4-三氮唑、1-羟基-苯并三氮唑、5-羧基-3-氨基-1,2,4-三氮唑、3-氨基-5-巯基-1,2,4-三氮唑、5-羧基-苯并三氮唑、5-苯基四氮唑、1-苯基-5-巯基-四氮唑、5-乙酸-1H- 四氮唑、5-甲基-四氮唑和5-氨基-四氮唑。The chemical mechanical polishing liquid according to claim 1, wherein the azole compound is one or more selected from the group consisting of benzotriazole, methylbenzotriazole, 1,2, 4-triazole, 3-amino-1,2,4-triazole, 4-amino-1,2,4-triazole, 3,5-diamino-1,2,4-triazole , 1-hydroxy-benzotriazole, 5-carboxy-3-amino-1,2,4-triazole, 3-amino-5-mercapto-1,2,4-triazole, 5-carboxyl -benzotriazole, 5-phenyltetrazolium, 1-phenyl-5-mercapto-tetrazole, 5-acetic acid-1H- Tetrazolium, 5-methyl-tetrazole and 5-amino-tetrazole.
- 如权利要求1所述的化学机械抛光液,其特征在于,所述唑类化合物的浓度为质量百分比0.005~2%。The chemical mechanical polishing liquid according to claim 1, wherein the concentration of the azole compound is 0.005 to 2% by mass.
- 如权利要求8所述的化学机械抛光液,其特征在于,所述唑类化合物的浓度为质量百分比0.01~1%。The chemical mechanical polishing liquid according to claim 8, wherein the concentration of the azole compound is 0.01 to 1% by mass.
- 如权利要求1所述的化学机械抛光液,其特征在于,所述络合剂为有机酸、有机磷酸和氨羧化合物中的一种或多种。The chemical mechanical polishing liquid according to claim 1, wherein the complexing agent is one or more of an organic acid, an organic phosphoric acid, and an aminocarboxylic acid compound.
- 如权利要求10所述的化学机械抛光液,其特征在于,所述络合剂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、酒石酸、苹果酸、乳酸、2-膦酸丁烷-1,2,4-三羧酸、氨基三亚甲基膦酸、羟基亚乙基二膦酸,乙二胺四亚甲基膦酸、二乙烯三胺五亚甲基膦酸、2-羟基膦酸基乙酸、和多氨基多醚基亚甲基膦酸、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、亚氨基二乙酸、氨三乙酸、甘氨酸和/或脯氨酸。The chemical mechanical polishing liquid according to claim 10, wherein the complexing agent is selected from one or more of the group consisting of acetic acid, propionic acid, oxalic acid, malonic acid, succinic acid, citric acid, Tartaric acid, malic acid, lactic acid, 2-phosphonic acid butane-1,2,4-tricarboxylic acid, aminotrimethylenephosphonic acid, hydroxyethylidene diphosphonic acid, ethylenediaminetetramethylenephosphonic acid, two Ethylene triamine penta methylene phosphonic acid, 2-hydroxyphosphonic acid acetic acid, and polyamino polyether methylene phosphonic acid, ethylenediaminetetraacetic acid, cyclohexanetetraacetic acid, ethylenediamine disuccinic acid, two Ethylene triamine pentaacetic acid and triethylenetetramine hexaacetic acid, iminodiacetic acid, ammonia triacetic acid, glycine and/or valine.
- 如权利要求1所述的化学机械抛光液,其特征在于,所述络合剂的浓度为质量百分比0.01~3%。The chemical mechanical polishing liquid according to claim 1, wherein the concentration of the complexing agent is 0.01 to 3% by mass.
- 如权利要求12所述的化学机械抛光液,其特征在于,所述络合剂的浓度为质量百分比0.05~1%。 The chemical mechanical polishing liquid according to claim 12, wherein the concentration of the complexing agent is 0.05 to 1% by mass.
- 如权利要求1所述的化学机械抛光液,其特征在于,所述聚烷氧化物为DISPERBYK-2090,DISPERBYK-2091。The chemical mechanical polishing liquid according to claim 1, wherein the polyalkoxide is DISPERBYK-2090, DISPERBYK-2091.
- 如权利要求1所述的化学机械抛光液,其特征在于,所述聚烷氧化物浓度为质量百分比0.005~1%。The chemical mechanical polishing liquid according to claim 1, wherein the polyalkoxide concentration is 0.005 to 1% by mass.
- 如权利要求15所述的化学机械抛光液,其特征在于,所述聚烷氧化物浓度为质量百分比0.01~0.5%。The chemical mechanical polishing liquid according to claim 15, wherein the polyalkoxide concentration is 0.01 to 0.5% by mass.
- 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。The chemical mechanical polishing liquid according to claim 1, wherein the oxidizing agent is selected from one or more of the group consisting of hydrogen peroxide, peracetic acid, potassium persulfate and ammonium persulfate.
- 如权利要求1所述的化学机械抛光液,其特征在于,所述氧化剂的浓度为质量百分比0.01~5%。The chemical mechanical polishing liquid according to claim 1, wherein the concentration of the oxidizing agent is 0.01 to 5% by mass.
- 如权利要求18所述的化学机械抛光液,其特征在于,所述氧化剂的浓度为质量百分比0.1~2%。The chemical mechanical polishing liquid according to claim 18, wherein the concentration of the oxidizing agent is 0.1 to 2% by mass.
- 如权利要求1所述的化学机械抛光液,其特征在于,所述的化学机械抛光液的pH值2~7。The chemical mechanical polishing liquid according to claim 1, wherein said chemical mechanical polishing liquid has a pH of from 2 to 7.
- 如权利要求20所述的化学机械抛光液,其特征在于,所述的化学机械抛光液的pH值为3~5。 The chemical mechanical polishing liquid according to claim 20, wherein said chemical mechanical polishing liquid has a pH of from 3 to 5.
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CN109370439A (en) * | 2018-10-22 | 2019-02-22 | 河北工业大学 | For inhibiting the polishing slurries of copper cobalt barrier layer galvanic corrosion and cobalt surface pitting |
CN113278366B (en) * | 2019-12-31 | 2022-05-20 | 清华大学 | Copper interconnection cobalt barrier layer of substrate |
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