CN111004579A - Alkaline polishing solution for reducing CMP defects of multilayer copper interconnection barrier layer and preparation method thereof - Google Patents
Alkaline polishing solution for reducing CMP defects of multilayer copper interconnection barrier layer and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of polishing solution, and particularly relates to alkaline polishing solution for reducing the CMP defects of a multilayer copper interconnection barrier layer and a preparation method thereof. The polishing solution consists of the following components in percentage by mass: 5-20% of silica sol, 0.1-5% of chelating agent, 0.001-5% of surfactant, 0.001-10% of oxidant and the balance of deionized water; wherein, the surfactant is obtained by compounding a nonionic active agent and an anionic active agent. The polishing solution of the invention is alkaline, has pH of 7.5-11, does not corrode equipment, and does not pollute the environment. The invention uses the nano SiO2 sol as the polishing liquid abrasive, and has high concentration, good dispersion degree and small hardness. The invention is composed of silica sol, chelating agent, surfactant, cosolvent, oxidant and deionized water, and has simple components, good stability and low price.
Description
Technical Field
The invention belongs to the field of polishing solution, and particularly relates to alkaline polishing solution for reducing the CMP defects of a multilayer copper interconnection barrier layer and a preparation method thereof.
Background
At present, the development trend of integrated circuit technology is as follows: increased wafer size, increased number of active devices, and reduced feature size. Planarization becomes more challenging and also places more stringent requirements on planarization, a flat surface, as little surface damage as possible, and a sufficiently small surface roughness. The role of Chemical Mechanical Planarization (CMP) is becoming more important as a key technology for global Planarization of large-size wafer chips.
CMP is used as a main planarization technology, which achieves planarization of a material surface through chemical reaction and mechanical friction, is applied to very large scale integrated circuits, and has local and global planarization effects. However, various defects may be formed on the surface of the workpiece during the CMP process. Including residues (organic residues and copper residues), particle adsorption, corrosion, scratch and the like, which all affect the reliability, electrical performance and other properties of the device, and more seriously may cause the functional failure of the device.
Scratch defects, which are the most common defects in the CMP process, are mainly generated in the mechanical rubbing process, which may reduce the thickness of the wiring metal, increase the resistance, and deteriorate the electromigration resistance. The micro-scratches are mainly caused by large particles (particle size >0.5 μm) in the polishing slurry. And the generation of the scratch defects is not irreversible, the generated scratch defects cannot be removed or reduced, and the scratch defects can be further reduced only by researching the generation reasons of the scratch defects. The formation of scratches is critical because they affect the yield and reliability of the device. It has been found that CMP scratches not only cause initial failure, but also long term reliability failure, and can lead to device failure, yield loss, and potential reliability problems. Previous researchers have mentioned reducing the amount of large particles and thus scratching by adding a slurry filtration system, but the abrasive particles in the slurry tend to stick to each other to form agglomerates when they come into contact due to brownian motion. Therefore, it is necessary to invent a polishing solution capable of effectively reducing scratch defects.
Disclosure of Invention
The invention aims to provide an alkaline polishing solution for reducing the CMP defects of a multi-layer copper interconnection barrier layer and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
an alkaline polishing solution for reducing the CMP defects of a multi-layer copper interconnection barrier layer comprises the following components in percentage by mass:
wherein, the surfactant is obtained by compounding a nonionic active agent and an anionic active agent.
The surfactant is one or a mixture of any nonionic surfactant and anionic surfactant selected from dodecyl dimethyl amine oxide OA, fatty alcohol-polyoxyethylene ether JFC, FA/O surfactant, fatty alcohol-polyoxyethylene ether AEO-7, polyvinylpyrrolidone PVP, fatty alcohol-polyoxyethylene ether ammonium sulfate AESA, sodium dodecyl sulfate SDS, sodium dodecyl benzene sulfonate SDBS, ammonium dodecyl sulfate ADS and dodecyl benzene sulfonate LABSA.
The pH value of the alkaline polishing solution is 7.5-11.
The mass percent of the surfactant is 0.26-0.75%, and the non-surfactant in the surfactant contains fatty alcohol polyoxyethylene ether.
The surfactant is a compound of fatty alcohol-polyoxyethylene ether, ammonium lauryl sulfate and dodecyl dimethyl amine oxide, and the mass ratio of the surfactant is 4 parts of fatty alcohol-polyoxyethylene ether; 2 parts of ammonium dodecyl sulfate; 1.5 parts of dodecyl dimethyl amine oxide.
Preferably, the alkaline polishing solution for reducing the CMP defects of the multilayer copper interconnection barrier layer comprises the following components in parts by mass:
more preferably, the alkaline polishing solution for reducing the CMP defects of the multilayer copper interconnection barrier layer comprises the following components in parts by mass:
the particle size of the silica sol is 50nm-90nm, and the dispersion degree is +/-3%; the chelating agent is one or any mixture of FA/O chelating agent, tetrahydroxyethyl ethylenediamine, ethylenediamine and triethanolamine;
the cosolvent is one or any mixture of potassium nitrate, potassium citrate, potassium tartrate, ammonium citrate and ammonium sulfate; the oxidant is one or any mixture of hydrogen peroxide, peroxyacetic acid, ammonium persulfate, potassium persulfate and potassium periodate.
The invention also comprises a preparation method of the alkaline polishing solution for reducing the CMP defects of the multilayer copper interconnection barrier layer, which comprises the following specific steps:
solution A: adding a chelating agent, a surfactant, a cosolvent and an oxidant into a proper amount of deionized water in sequence according to the component amounts, and uniformly stirring in a step-by-step mixing manner;
and B, liquid B: weighing silica sol according to the components, and adding the silica sol into a proper amount of deionized water;
and adding the solution A into the solution B in a mode of stirring while pouring, and finally complementing the solution A with deionized water.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts the compounding of the nonionic active agent and the anionic active agent, and can reduce the number of large particles in the polishing solution through the steric hindrance effect. The addition of the composite active agent in the polishing solution obviously reduces the number of large particles in the polishing solution. Due to the surface effect of the nano material, the surface of the SiO2 particle has a plurality of charges or functional groups and high surface energy, and the characteristics determine that the surface energy of the SiO2 particle tends to be small and agglomeration phenomenon occurs. After the composite active agent is added into the polishing solution, the hydrophilic group of the anionic active agent is fully extended in the aqueous solution, and the lipophilic group is adsorbed on the surface of the particles to form a layer of film. When the particles are close to each other, the repulsion energy exists in the boundary area, so that the particles can keep enough safe distance to generate steric hindrance effect, further the molecular reaction activity is reduced, and the collision focus and gravity sedimentation of the particles are hindered. The active agent adsorbed on the surface of the particle not only repels surrounding particles by its own charge, but also prevents particles moving brownian from approaching by hydrophobic groups and steric resistance effect, thereby generating a composite stabilization effect. The nonionic surfactant has the functions of penetration, infiltration and dispersion, is introduced into the polishing solution to reduce the contact angle and the surface tension, greatly enhances the infiltration and the permeability, and is better spread on the polished surface. The synergistic effect of the surfactants reduces the agglomeration capacity of the particles, so that the abrasive particles keep a stable state with the lowest energy, and finally the stability of the whole system is achieved, so that the number of large particles in the polishing solution is reduced, and the number of surface defects in the barrier layer CMP is reduced.
The polishing solution of the invention is alkaline, has pH of 7.5-11, does not corrode equipment, and does not pollute the environment.
The invention uses the nano SiO2 sol as the polishing liquid abrasive, and has high concentration, good dispersion degree and small hardness.
The invention is composed of silica sol, chelating agent, surfactant, cosolvent, oxidant and deionized water, and has simple components, good stability and low price.
The preparation method is simple, the raw materials are all made in China, and the method is suitable for the requirement of large-scale industrial production.
Drawings
FIG. 1 is a schematic illustration of the effect of different composite active agent concentrations of the present invention on the number of surface defects during barrier CMP.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and preferred embodiments.
Example one (Sample 1, S1) contains no surfactant:
taking 250g of silica sol with the abrasive mass fraction of 40%, wherein the grain diameter is 50nm-90nm, and the dispersion degree is +/-3%; 10g of FA/OII chelating agent which is used as a pH value regulator, a buffering agent and a chelating agent and does not contain metal ions; 0.05g of hydrogen peroxide. The preparation method comprises the following steps: sequentially adding the FA/O II chelating agent, hydrogen peroxide and silica sol into a proper amount of deionized water according to the component weight, uniformly stirring in a step-by-step mixing mode, finally supplementing the deionized water to 1000g, and continuously uniformly stirring.
And (3) test monitoring: the pH value of the polishing solution is 9.5, and the particle size is 80-120 nm.
Defect testing experiment: using the prepared polishing solution to an AMAT-LK CMP type polishing machine produced by Applied Materials; working pressure Z1：1psi、Z2：1.7psi、Z3：1.5psi、Z4：1.5psi、Z51.5 psi; the rotational speed of the throwing disc is 80 r/min; the head throwing speed is 78 r/min; the flow rate of the polishing solution was 300 ml/min. Polishing a 300mm pattern sheet, cleaning, detecting defects by using a Scanning Electron Microscope (SEM), and obtaining 30000+ particles of total defects. Defect map (as shown in S1 in fig. 1).
Example two (Sample 2, S2) surfactant contains only nonionic surfactant:
taking 250g of silica sol with the abrasive mass fraction of 40%, wherein the grain diameter is 50nm-90nm, and the dispersion degree is +/-3%; 10g of FA/OII chelating agent which is used as a pH value regulator, a buffering agent and a chelating agent and does not contain metal ions; 0.1g,0.5g,1g,1.5g and 3g of dodecyl dimethyl amine oxide and 0.05g of hydrogen peroxide are respectively taken. The preparation method comprises the following steps: sequentially adding an FA/O II chelating agent, dodecyl dimethyl amine Oxide (OA), hydrogen peroxide and silica sol into a proper amount of deionized water according to the component amount, uniformly stirring in a step-by-step mixing mode, finally supplementing the deionized water to 1000g, and continuously uniformly stirring. And (3) test monitoring: the pH value of the polishing solution is 9.5, and the particle size is 80-110 nm.
Defect testing experiment: using the prepared polishing solution to an AMAT-LK CMP type polishing machine produced by Applied Materials; working pressure Z1：1psi、Z2：1.7psi、Z3：1.5psi、Z4：1.5psi、Z51.5 psi; the rotational speed of the throwing disc is 80 r/min; throwing head rotating deviceSpeed 78 rpm; the flow rate of the polishing solution was 300 ml/min. Polishing a 300mm pattern sheet, cleaning, detecting defects by using a Scanning Electron Microscope (SEM), and obtaining 12000, 10000, 7863, 7900 and 7932 total defects respectively. Defect map (as shown in S2 in fig. 1).
In example three (Sample 3, S3), the surfactant is a combination of an anionic active agent and a nonionic active agent, the mass ratio of the anionic active agent to the nonionic active agent is 0.1-3:1, and the mass percentage of the surfactant in the polishing solution is 0.11-0.4%.
Taking 250g of silica sol with the abrasive mass fraction of 40%, wherein the grain diameter is 50nm-90nm, and the dispersion degree is +/-3%; 10g of FA/OII chelating agent which is used as a pH value regulator, a buffering agent and a chelating agent and does not contain metal ions; taking 0.1g,0.5g,1g,1.5g and 3g of ammonium dodecyl sulfate respectively; 1g of dodecyl dimethyl amine oxide and 0.05g of hydrogen peroxide. The preparation method comprises the following steps: adding the FA/O II chelating agent, ammonium dodecyl sulfate, dodecyl dimethyl amine oxide, hydrogen peroxide and silica sol into a proper amount of deionized water in turn according to the component amount, uniformly stirring in a step-by-step mixing mode, finally supplementing the deionized water to 1000g, and continuously uniformly stirring. And (3) test monitoring: the pH value of the polishing solution is 9.5, and the particle size is 80-105 nm.
Defect testing experiment: using the prepared polishing solution to an AMAT-LK CMP type polishing machine produced by Applied Materials; working pressure Z1：1psi、Z2：1.7psi、Z3：1.5psi、Z4：1.5psi、Z51.5 psi; the rotational speed of the throwing disc is 80 r/min; the head throwing speed is 78 r/min; the flow rate of the polishing solution was 300 ml/min. Polishing a 300mm pattern sheet, cleaning, and detecting defects by using a Scanning Electron Microscope (SEM), wherein 3500, 3210, 2500, 1899 and 1923 defects are obtained. Defect map (as shown in S3 in fig. 1).
Example four (Sample 4, S4), the surfactant is a combination of an anionic active agent and a nonionic active agent, and the mass ratio of the anionic active agent to the nonionic active agent is 1.5: 1.1-4, and the mass percentage in the polishing solution is 0.26-0.55%, and the surface active agent contains fatty alcohol polyoxyethylene ether.
Taking 250g of silica sol with the abrasive mass fraction of 40%, wherein the grain diameter is 50nm-90nm, and the dispersion degree is +/-3%; 10g of FA/OII chelating agent which is used as a pH value regulator, a buffering agent and a chelating agent and does not contain metal ions; respectively taking 0.1g,0.5g,1g,1.5g and 3g of fatty alcohol-polyoxyethylene ether; 1.5g of ammonium dodecyl sulfate, 1g of dodecyl dimethyl amine oxide and 0.05g of hydrogen peroxide. The preparation method comprises the following steps: sequentially adding an FA/O II chelating agent, fatty alcohol-polyoxyethylene ether, ammonium dodecyl sulfate, dodecyl dimethyl amine oxide, hydrogen peroxide and silica sol into a proper amount of deionized water according to the component amount, uniformly stirring in a step-by-step mixing manner, finally supplementing to 1000g with deionized water, and continuously uniformly stirring. And (3) test monitoring: the pH value of the polishing solution is 9.5, and the particle size is 80-105 nm. And (3) test monitoring: the pH value of the polishing solution is 9.5, and the particle size is 85-105 nm.
Defect testing experiment: using the prepared polishing solution to an AMAT-LK CMP type polishing machine produced by Applied Materials; working pressure Z1：1psi、Z2：1.7psi、Z3：1.5psi、Z4：1.5psi、Z51.5 psi; the rotational speed of the throwing disc is 80 r/min; the head throwing speed is 78 r/min; the flow rate of the polishing solution was 300 ml/min. The 300mm pattern piece was polished, cleaned, and then examined for defects by Scanning Electron Microscopy (SEM), and a defect map (shown as S4 in fig. 1) was obtained, in which the total number of defects was 1003, 700, 600, 450, and 312, respectively. Defect map (as shown in S4 in fig. 1).
Example five (Sample 5, S5): the surfactant is a compound of an anionic active agent and a nonionic active agent, and the mass ratio of the anionic active agent to the nonionic active agent is 2: 5.5, the mass percent of the polishing solution is 0.75%, and the surfactant contains fatty alcohol-polyoxyethylene ether.
Taking 250g of silica sol with the abrasive mass fraction of 40%, wherein the grain diameter is 50nm-90nm, and the dispersion degree is +/-3%; 10g of FA/OII chelating agent which is used as a pH value regulator, a buffering agent and a chelating agent and does not contain metal ions; taking 4g of fatty alcohol-polyoxyethylene ether; 2g of ammonium dodecyl sulfate; dodecyl dimethyl amine oxide 1.5 g; 0.05g of hydrogen peroxide. The preparation method comprises the following steps: sequentially adding an FA/OII chelating agent, dodecyl ammonium sulfate, dodecyl dimethyl amine oxide, fatty alcohol-polyoxyethylene ether, hydrogen peroxide and silica sol into a proper amount of deionized water according to the component amount, uniformly stirring in a step-by-step mixing manner, finally supplementing to 1000g with deionized water, and continuously uniformly stirring.
And (3) test monitoring: the pH value of the polishing solution is 9.5, and the particle size is 85-100 nm.
Defect testing experiment: using the prepared polishing solution to an AMAT-LK CMP type polishing machine produced by Applied Materials; working pressure Z1：1psi、Z2：1.7psi、Z3：1.5psi、Z4：1.5psi、Z51.5 psi; the rotational speed of the throwing disc is 80 r/min; the head throwing speed is 78 r/min; the flow rate of the polishing solution was 300 ml/min. The 300mm pattern piece was polished, then cleaned, and then examined for defects by Scanning Electron Microscopy (SEM), and a total number of defects of 29 were obtained. Defect map (as shown in S5 in fig. 1).
Example six (Sample 6, S6): the surfactant is a compound of an anionic active agent and a nonionic active agent, and the mass ratio of the anionic active agent to the nonionic active agent is 6: 15, and the mass percent of the polishing solution is 2.1%, and the surfactant contains fatty alcohol-polyoxyethylene ether.
Taking 250g of silica sol with the abrasive mass fraction of 40%, wherein the grain diameter is 50nm-90nm, and the dispersion degree is +/-3%; 10g of FA/OII chelating agent which is used as a pH value regulator, a buffering agent and a chelating agent and does not contain metal ions; 5g of dodecyl dimethyl amine oxide; 6g of dodecylamine sulfate (anion); 10g of fatty alcohol-polyoxyethylene ether; 0.05g of hydrogen peroxide. The preparation method comprises the following steps: sequentially adding an FA/O II chelating agent, dodecyl ammonium sulfate, dodecyl dimethyl amine oxide, fatty alcohol-polyoxyethylene ether, hydrogen peroxide and silica sol into a proper amount of deionized water according to the component weight, uniformly stirring in a step-by-step mixing manner, finally supplementing the deionized water to 1000g, and continuously uniformly stirring.
And (3) test monitoring: the pH value of the polishing solution is 9.5, and the particle size is 80-110 nm.
Defect testing experiment: using the prepared polishing solution to an AMAT-LK CMP type polishing machine produced by Applied Materials; working pressure Z1：1psi、Z2：1.7psi、Z3：1.5psi、Z4：1.5psi、Z51.5 psi; the rotational speed of the throwing disc is 80 r/min; the head throwing speed is 78 r/min; the flow rate of the polishing solution was 300 ml/min. Polishing a 300mm pattern piece, cleaning, detecting defects by using a Scanning Electron Microscope (SEM), and obtaining 1236 defects. Defect map (as shown in S6 in fig. 1).
As can be seen from the defect diagram in FIG. 1, the surface defects can be effectively reduced by compounding different active agents. Comparing S2 and S3 in fig. 1, it can be seen that the compounding of ammonium dodecyl sulfate and dodecyl dimethyl amine oxide can significantly reduce the number of defects, because ammonium dodecyl sulfate has good dispersing and wetting effects, and dodecyl dimethyl amine oxide improves the stability and dispersibility of silica nanoparticles, reduces particle aggregation, and further reduces defects, but the defect number is not as expected. Comparing S3, S4 and S5 in FIG. 1, it can be seen that fatty alcohol-polyoxyethylene ether is more effective in reducing surface defects, and fatty alcohol-polyoxyethylene ether has strong osmotic effect and can significantly reduce contact angles. The three active agents are compounded to obviously reduce the surface tension of the polishing solution, so that the wetting surface is improved and the uniformity is improved. The contact angle is small enough, improves the spreading behavior of polishing solution, reduces polishing friction, avoids the particle aggregation in the polishing process simultaneously, reduces the adsorption capacity of wafer surface, and then reduces the defect. Comparing S5 and S6 in fig. 1, it can be seen that as the mass fraction of the composite active agent continues to increase, the number of defects also increases, and the number of large particles in the polishing slurry also increases. This is because when the surfactant is excessive, free surfactant molecules bridge between particles to cause aggregation of particles, so that the number of large particles in the polishing slurry increases (more significantly, the particle diameter is greater than 5 μm); secondly, because the active agent has a foaming function, the foam in the polishing solution is increased along with the increase of the mass fraction of the active agent, and the foam floating on the surface of the polishing solution is easy to form crystals and scratch; the results of fig. 1 thus appear. The above description is only a preferred embodiment of the present invention, and for those skilled in the art, the present invention should not be limited by the description of the present invention, which should be interpreted as a limitation.
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| CN112322190A (en) * | 2020-11-05 | 2021-02-05 | 河北工业大学 | Multilayer copper interconnect barrier layer polishing solution and preparation method thereof |
| CN112355884A (en) * | 2020-11-05 | 2021-02-12 | 河北工业大学 | Control method for CMP rate selectivity of multi-layer copper interconnection barrier layer |
| CN114591684A (en) * | 2022-02-18 | 2022-06-07 | 浙江开化元通硅业有限公司 | An environmentally friendly chemical mechanical polishing liquid based on high-purity spherical silica sol and its preparation method and polishing method |
| CN115058198A (en) * | 2022-03-21 | 2022-09-16 | 康劲 | Novel polishing solution and preparation method and application thereof |
| CN115056117A (en) * | 2022-03-21 | 2022-09-16 | 康劲 | Polishing process for preventing scratches in CMP (chemical mechanical polishing) |
| CN116814166A (en) * | 2023-06-05 | 2023-09-29 | 深圳市众望丽华微电子材料有限公司 | Low-residue coarse polishing solution suitable for large-size silicon wafer and preparation method thereof |
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| CN112322190A (en) * | 2020-11-05 | 2021-02-05 | 河北工业大学 | Multilayer copper interconnect barrier layer polishing solution and preparation method thereof |
| CN112355884A (en) * | 2020-11-05 | 2021-02-12 | 河北工业大学 | Control method for CMP rate selectivity of multi-layer copper interconnection barrier layer |
| CN112355884B (en) * | 2020-11-05 | 2022-04-08 | 河北工业大学 | Control method for CMP rate selectivity of multi-layer copper interconnection barrier layer |
| CN114591684A (en) * | 2022-02-18 | 2022-06-07 | 浙江开化元通硅业有限公司 | An environmentally friendly chemical mechanical polishing liquid based on high-purity spherical silica sol and its preparation method and polishing method |
| CN114591684B (en) * | 2022-02-18 | 2024-01-30 | 浙江开化元通硅业有限公司 | Environment-friendly chemical mechanical polishing solution based on high-purity spherical silica sol, and preparation method and polishing method thereof |
| CN115058198A (en) * | 2022-03-21 | 2022-09-16 | 康劲 | Novel polishing solution and preparation method and application thereof |
| CN115056117A (en) * | 2022-03-21 | 2022-09-16 | 康劲 | Polishing process for preventing scratches in CMP (chemical mechanical polishing) |
| CN116814166A (en) * | 2023-06-05 | 2023-09-29 | 深圳市众望丽华微电子材料有限公司 | Low-residue coarse polishing solution suitable for large-size silicon wafer and preparation method thereof |
| CN119639353A (en) * | 2024-12-25 | 2025-03-18 | 河北工业大学创新研究院(石家庄) | Alkaline polishing liquid for TSV titanium barrier layer and preparation method thereof |
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