CN111378378B - Chemical mechanical polishing solution and application thereof - Google Patents
Chemical mechanical polishing solution and application thereof Download PDFInfo
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- CN111378378B CN111378378B CN201811635515.3A CN201811635515A CN111378378B CN 111378378 B CN111378378 B CN 111378378B CN 201811635515 A CN201811635515 A CN 201811635515A CN 111378378 B CN111378378 B CN 111378378B
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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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- 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 potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table 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
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
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Abstract
The invention provides a chemical mechanical polishing solution, which comprises silicon dioxide abrasive particles, a corrosion inhibitor, a complexing agent, an oxidant, a hydrocarbon sulfonate anionic surfactant and a metal surface defect improver. The polishing solution has the advantages that: 1) The polishing solution has high copper polishing rate and low tantalum polishing rate, so that the polishing solution has higher copper/tantalum polishing rate selection ratio; 2) The polishing solution can improve dishing and dielectric layer erosion of the polished copper wire; 3) The polishing solution can improve the surface roughness of copper after polishing and reduce surface defects.
Description
Technical Field
The invention relates to the field of chemical mechanical polishing, in particular to a chemical mechanical polishing solution and application thereof.
Background
With the development of semiconductor technology, copper, which is a material having good conductivity, has been widely used in electronic element circuits as a material for miniaturization of electronic parts. The small resistance of copper can increase the signal transmission speed between transistors in a circuit, and can provide smaller parasitic capacitance capability and smaller electromigration sensitivity. These electrical advantages have led to copper having a good development prospect in the development of semiconductor technology.
However, during the fabrication of copper integrated circuits, it has been found that copper migrates or diffuses into the transistor regions of the integrated circuits, thereby adversely affecting the performance of the semiconductor transistors, and that copper interconnects can only be fabricated in a damascene process, namely: 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 covered on the dielectric layer. The excess copper/copper barrier layer on the dielectric layer is then removed by chemical mechanical polishing, leaving individual interconnect lines in the trenches. The copper chemical mechanical polishing process is generally divided into 3 steps: and 1, removing a large amount of copper on the surface of the substrate with high downward pressure at a high and efficient removal rate and leaving copper with a certain thickness, 2, removing the residual metallic copper with low removal rate and stopping on the barrier layer, 3, and removing the barrier layer, part of the dielectric layer and the metallic copper with a barrier layer polishing solution to realize planarization.
In the copper polishing process, on one hand, redundant copper on the barrier layer needs to be removed as soon as possible, and on the other hand, dishing of the polished copper wire needs to be reduced as much as possible. The metal layer has a partial recess over the copper lines prior to copper polishing. Copper on the dielectric material is easily removed at higher bulk pressures during polishing, while copper in the recess is polished at a lower pressure than the bulk pressure and at a lower copper removal rate. As polishing proceeds, the copper level difference gradually decreases to achieve planarization. However, if the chemical action of the copper polishing liquid is too strong and the static etching rate is too high during polishing, the passivation film of copper is easily removed even under a relatively low pressure (e.g., copper line dishing), resulting in a decrease in planarization efficiency and an increase in dishing after polishing.
With the development of integrated circuits, on the one hand, in the traditional IC industry, in order to improve the integration level, reduce the energy consumption, shorten the delay time, make the line width narrower and narrower, use the low dielectric (low-k) material with lower mechanical strength for the dielectric layer, the number of layers of the wiring is also increasing, and in order to ensure the performance and stability of the integrated circuit, the requirement on copper chemical mechanical polishing is also increasing. It is required to reduce polishing pressure, improve planarization of copper wire surface and control surface defects while ensuring copper removal rate. On the other hand, the line width cannot be scaled down indefinitely due to physical limitations, and the semiconductor industry is no longer solely dependent on integrating more devices on a single chip to improve performance, but is moving toward multi-chip packaging.
Through Silicon Via (TSV) technology is widely accepted in the industry as a latest technology for realizing interconnection between chips by making vertical conduction between chips and between wafers. TSVs enable the density of stacked chips in three dimensions to be maximized, the overall dimensions to be minimized, and chip speed and low power consumption performance to be greatly improved. The conventional TSV process is combined with the conventional IC process to form copper vias penetrating through the silicon substrate, i.e., copper is filled in the TSV opening to realize conduction, and the superfluous copper after filling also needs to be planarized by chemical mechanical polishing removal. Unlike the conventional IC industry, the excess copper filled back surface is typically several to tens of microns thick due to the deep through silicon vias. In order to quickly remove this excess copper. It is generally desirable to have a high copper polishing rate with good surface flatness after polishing. The existing polishing solution can generate dishing, dielectric layer erosion, copper residue, corrosion and other defects after polishing.
Disclosure of Invention
In order to solve the problems, the invention provides a chemical mechanical polishing solution and application thereof, wherein the polishing solution has higher copper polishing rate and lower polishing rate of a tantalum barrier layer, improves the polishing selection ratio of the polishing solution to the copper and tantalum barrier layer, improves dishing and dielectric erosion of a copper wire after polishing, and improves the surface roughness and surface defects of the copper wire after polishing by adding a corrosion inhibitor, a hydrocarbyl sulfonate anionic surfactant and a metal surface defect improver through using abrasive particles with larger particle size and wide distribution index range.
Specifically, the invention provides a chemical mechanical polishing solution, which comprises silicon dioxide grinding particles, a corrosion inhibitor, a complexing agent, an oxidant, a alkyl sulfonate anionic surfactant and a metal surface defect improver, wherein the average particle size of the silicon dioxide grinding particles is 60-140nm, the particle size distribution index is 0.1-0.6, and the pH value of the chemical mechanical polishing solution is 5-8.
Preferably, the silica abrasive particles have an average particle diameter of 80 to 120nm.
Preferably, the mass percentage content of the silicon dioxide abrasive particles is 0.05% -2%.
Preferably, the mass percentage content of the silicon dioxide abrasive particles is 0.1% -1%.
Preferably, the complexing agent comprises one or more of glycine, alanine, valine, leucine, proline, phenylalanine, tyrosine, tryptophan, lysine, arginine, histidine, serine, aspartic acid, glutamic acid, asparagine, glutamine, nitrilotriacetic acid, ethylenediamine tetraacetic acid, cyclohexane tetraacetic acid, ethylenediamine disuccinic acid, diethylenetriamine pentaacetic acid and triethylenetetramine hexaacetic acid.
Preferably, the mass percentage content of the complexing agent is 0.01% -10%.
Preferably, the mass percentage content of the complexing agent is 0.5% -3%.
Preferably, the alkyl sulfonate anionic surfactant is alkyl sulfonate with carbon number < 10.
Preferably, the alkyl sulfonate anionic surfactant is potassium salt or sodium salt.
Preferably, the mass percentage content of the alkyl sulfonate anionic surfactant is 0.0005-0.5%
Preferably, the mass percentage content of the alkyl sulfonate anionic surfactant is 0.005-0.1%
Preferably, the alkyl sulfonate anionic surfactant comprises one or more of methyl sulfonate, vinyl sulfonate, allyl sulfonate, p-methylbenzenesulfonate, p-ethylbenzene sulfonate and p-propylbenzene sulfonate.
Preferably, the corrosion inhibitor comprises one or more of 1,2, 4-triazole, 3-amino-1, 2, 4-triazole, 4-amino-1, 2, 4-triazole, 3, 5-diamino-1, 2, 4-triazole, 5-carboxy-3-amino-1, 2, 4-triazole, 3-amino-5-mercapto-1, 2, 4-triazole, 5-acetic acid-1H-tetrazole, 5-methyltetrazole, and 5-amino-1H-tetrazole.
Preferably, the corrosion inhibitor is present in an amount of 0.001% to 5% by mass.
Preferably, the corrosion inhibitor is present in an amount of 0.005% to 1% by mass.
Preferably, the oxidizing agent is hydrogen peroxide.
Preferably, the mass percentage content of the oxidant is 0.05% -5%.
Preferably, the mass percentage content of the oxidant is 0.1% -3%.
Preferably, the metal surface defect improving agent comprises one or more of a polyol, a hydrophilic polymer.
Preferably, the polyol comprises one or more of ethylene glycol, diethylene glycol, glycerol.
Preferably, the hydrophilic polymer comprises one or more of polyvinyl alcohol, polyvinylpyrrolidone, polyacrylamide, polyoxyethylene polyoxypropylene block polymers.
Preferably, the molecular weight of the hydrophilic polymer is 1000-10000.
Preferably, the metal surface defect improving agent is 0.001% -2% by mass.
In another aspect of the invention, there is provided the use of the chemical mechanical polishing solution described above for copper chemical mechanical polishing in metal copper interconnect and through silicon via processes.
The polishing liquid of the invention can also comprise additives commonly used in chemical mechanical polishing liquid, such as pH regulator, viscosity regulator, defoamer and the like.
Compared with the prior art, the invention has the advantages that: 1) The polishing solution has high copper polishing rate and low tantalum polishing rate, so that the polishing solution has higher copper/tantalum polishing rate selection ratio; 2) The polishing solution can improve dishing and medium layer erosion on the surface of the polished copper wire; 3) The polishing solution can improve the surface roughness of copper after polishing and reduce surface defects.
Detailed Description
The advantages of the present invention are further illustrated by the following specific examples, but the scope of the present invention is not limited to the following examples.
Table 1 shows the chemical mechanical polishing solution of the present inventionExamples 1-36, the components other than the oxidizing agent were mixed uniformly according to the formulations given in the table, with water to make up to 100% by mass. By KOH or HNO 3 Adjusted to the desired pH. Adding oxidant before use, and mixing. The polishing solution of the invention can also be prepared into a concentrated sample, and the concentrated sample is diluted to the concentration in the embodiment by deionized water when in use, and an oxidant is added for use.
TABLE 1 polishing liquid compositions of examples 1-36 of the present invention
Table 2 shows examples 37-48 and comparative examples 1-7 of the chemical mechanical polishing solutions of the present invention, and the components other than the oxidizing agent were uniformly mixed according to the formulations given in the table, with water being used to make up to 100% by mass. By KOH or HNO 3 Adjusted to the desired pH. Adding oxidant before use, and mixing. The polishing solution of the invention can also be prepared into a concentrated sample, and the concentrated sample is diluted to the concentration in the embodiment by deionized water when in use, and an oxidant is added for use.
Table 2 comparative examples 1-7 and examples 37-48
The polishing solutions of comparative examples 1 to 7 and inventive examples 37 to 48 were used to polish bare copper (Cu) and tantalum (Ta) under the following conditions. Specific polishing conditions: cu polishing pressures were 1.5psi and 2.0psi, tantalum polishing pressures were 1.5psi; the rotation speed of the polishing disk and the polishing head is 73/67rpm, the polishing pad IC1010 and the flow rate of the polishing liquid are 350mL/min, the polishing table is 12' reflexion LK, and the polishing time is 1min. The polishing rates for copper/tantalum for each example were measured separately and the polishing rate selection ratios for both were calculated and the results are set forth in table 3.
The patterned copper wafers were polished using the polishing solutions of comparative examples 1 to 7 and inventive examples 37 to 48 under the following conditions. Polishing conditions: the rotation speed of the polishing disk and the polishing head is 73/67rpm, the polishing pad IC1010 and the flow rate of the polishing liquid is 350mL/min, and the polishing table is 12' reflexion LK. Polishing the patterned copper wafer to about residual copper on polishing pad 1 with a downforce of 2.0psiThe residual copper was then removed on polishing pad 2 with a down force of 1.5 psi. Dishing (Dishing), dielectric Erosion (eroion), and copper surface Roughness (rouchness) of a copper line array region of 5um/1um (copper line/dielectric line width) on a patterned copper wafer were measured using an XE-300P atomic force microscope, and the number of surface defects of the polished copper blank wafer was measured using a surface defect scanner SP2, and the Dishing and dielectric Erosion values of the resulting copper line, and the copper surface Roughness and number of surface defects were as shown in table 3.
TABLE 3 polishing effects of comparative examples 1 to 7 and examples 37 to 48
As can be seen from Table 3, the polishing liquid of the present invention has not only a higher copper/tantalum polishing rate selection ratio than the comparative example, but also copper wires after polishing using the polishing liquid of the present inventionThe dishing and dielectric layer erosion, the copper surface roughness and the surface defects are less, and the copper surface morphology is greatly improved. The polishing solution of the comparative example 1 only contains grinding particles, complexing agent and oxidant, and the polishing rates of the polishing solution on copper and tantalum are high, so that the polishing rate selection on copper/tantalum is low, the polishing solution of the comparative example 2 is added with corrosion inhibitor on the basis of the comparative example 1, and the polishing solution of the comparative example 3 is further added with hydrocarbyl sulfonate surfactant on the basis of the comparative example 2, so that the polishing rate of tantalum is reduced, and the polishing rate selection ratio of the polishing solution on copper/tantalum is improved. However, copper dishing and dielectric erosion, and copper surface roughness and surface defect values were both high after polishing with the polishing solution of comparative example 2, and copper surface roughness and surface defects were high after polishing with the polishing solution of comparative example 3, failing to meet the polishing requirements. The polishing solutions of comparative examples 4 to 7 were used in combination with a corrosion inhibitor, a complexing agent, an oxidizing agent, a hydrocarbon sulfonate-based anionic surfactant, and a metal surface defect-improving agent, thereby having a high copper/tantalum polishing rate selection ratio. However, siO in the polishing liquid of comparative example 4 2 The abrasive has smaller particle size and wider particle size distribution, and the polishing solution of comparative example 5 contains SiO 2 The grain diameter of the abrasive is larger and the grain size distribution is narrower, and the removal rate of Cu by the two polishing solutions is smaller than that of CuAt a lower level; the pH of comparative example 6 was too low, resulting in a large dishing and dielectric erosion value of the copper wire after polishing; the pH of comparative example 7 was too high and the copper polishing rate was low, failing to remove copper effectively.
The polishing solutions of examples 37-48 of the present invention have a higher copper polishing rate and a lower tantalum polishing rate, and a higher copper/tantalum polishing rate selection ratio by selecting abrasive particles having a suitable particle size range and particle size distribution index, a suitable pH, and combining a corrosion inhibitor, a hydrocarbyl sulfonate anionic surfactant, and a metal surface defect-improving agent; meanwhile, the polished copper wire has less dishing, less erosion of a dielectric layer, less copper surface roughness and less surface defects and good surface morphology. Specifically, the polishing solution has higher copper polishing rate by selecting silicon dioxide grinding particles with average particle diameter of 60-140nm and particle diameter distribution index of 0.1-0.6; further using alkyl sulfonate anionic surfactant and corrosion inhibitor, the polishing rate of tantalum is reduced, thus improving the polishing rate selection ratio of polishing solution to copper/tantalum; further, a metal surface defect improver is added, and the pH value is controlled to be 5-8, so that dishing and medium layer erosion of the polished copper wire, copper surface roughness and surface defects are improved, and the copper surface morphology is greatly improved.
It should be noted that the embodiments of the present invention are preferred and not limited in any way, and any person skilled in the art may make use of the above-disclosed technical content to change or modify the same into equivalent effective embodiments without departing from the technical scope of the present invention, and any modification or equivalent change and modification of the above-described embodiments according to the technical substance of the present invention still falls within the scope of the technical scope of the present invention.
Claims (20)
1. A chemical mechanical polishing solution comprises silicon dioxide grinding particles, a corrosion inhibitor, a complexing agent, an oxidant, a alkyl sulfonate anionic surfactant and a metal surface defect improver, wherein the average particle size of the silicon dioxide grinding particles is 60-140nm, the particle size distribution index is 0.1-0.6, and the pH value of the chemical mechanical polishing solution is 5-7.5; the metal surface defect improver is polyalcohol; the corrosion inhibitor includes one or more of 1,2, 4-triazole, 3-amino-1, 2, 4-triazole, 4-amino-1, 2, 4-triazole, 3, 5-diamino-1, 2, 4-triazole, 5-carboxy-3-amino-1, 2, 4-triazole, 3-amino-5-mercapto-1, 2, 4-triazole, 5-acetic acid-1H-tetrazole, 5-methyltetrazole, and 5-amino-1H-tetrazole.
2. The chemical mechanical polishing liquid according to claim 1, wherein,
the average particle diameter of the silicon dioxide grinding particles is 80-120nm.
3. The chemical mechanical polishing liquid according to claim 1, wherein,
the mass percentage content of the silicon dioxide grinding particles is 0.05% -2%.
4. The chemical mechanical polishing liquid according to claim 3, wherein,
the mass percentage content of the silicon dioxide grinding particles is 0.1% -1%.
5. The chemical mechanical polishing liquid according to claim 1, wherein,
the complexing agent comprises one or more of glycine, alanine, valine, leucine, proline, phenylalanine, tyrosine, tryptophan, lysine, arginine, histidine, serine, aspartic acid, glutamic acid, asparagine, glutamine, nitrilotriacetic acid, ethylenediamine tetraacetic acid, cyclohexane tetraacetic acid, ethylenediamine disuccinic acid, diethylenetriamine pentaacetic acid and triethylenetetramine hexaacetic acid.
6. The chemical mechanical polishing liquid according to claim 1, wherein,
the mass percentage content of the complexing agent is 0.1% -5%.
7. The chemical mechanical polishing liquid as recited in claim 6, wherein,
the mass percentage content of the complexing agent is 0.5% -3%.
8. The chemical mechanical polishing liquid according to claim 1, wherein,
the alkyl sulfonate anionic surfactant is alkyl sulfonate with carbon number of < 10.
9. The chemical mechanical polishing liquid according to claim 1, wherein,
the alkyl sulfonate anionic surfactant is potassium salt or sodium salt.
10. The chemical mechanical polishing liquid according to claim 1, wherein,
the alkyl sulfonate anionic surfactant comprises one or more of methyl sulfonate, vinyl sulfonate, allyl sulfonate, p-methylbenzenesulfonate, p-ethylbenzene sulfonate and p-propyl benzene sulfonate.
11. The chemical mechanical polishing liquid according to claim 1, wherein,
the mass percentage content of the alkyl sulfonate anionic surfactant is 0.0005% -0.5%.
12. The chemical mechanical polishing liquid as recited in claim 11, wherein,
the mass percentage content of the alkyl sulfonate anionic surfactant is 0.005-0.1%.
13. The chemical mechanical polishing liquid according to claim 1, wherein,
the mass percentage content of the corrosion inhibitor is 0.001% -5%.
14. The chemical mechanical polishing liquid as recited in claim 13, wherein,
the mass percentage content of the corrosion inhibitor is 0.005% -1%.
15. The chemical mechanical polishing liquid according to claim 1, wherein,
the oxidizing agent is hydrogen peroxide.
16. The chemical mechanical polishing liquid according to claim 1, wherein,
the mass percentage content of the oxidant is 0.05% -5%.
17. The chemical mechanical polishing slurry of claim 16, wherein the slurry is a slurry,
the mass percentage content of the oxidant is 0.1% -3%.
18. The chemical mechanical polishing liquid according to claim 1, wherein,
the polyol comprises one or more of ethylene glycol, diethylene glycol and glycerol.
19. The chemical mechanical polishing liquid according to claim 1, wherein,
the content of the metal surface defect improver is 0.001% -2%.
20. Use of a chemical mechanical polishing solution according to any one of claims 1 to 19 in copper metal chemical mechanical polishing.
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| EP4189027A4 (en) * | 2020-07-28 | 2024-07-31 | CMC Materials LLC | CMP COMPOSITION WITH ANIONIC AND CATIONIC INHIBITORS |
| CN114958206B (en) * | 2021-02-22 | 2024-02-02 | 万华化学集团电子材料有限公司 | Copper chemical mechanical polishing solution and application thereof and chemical mechanical polishing method |
| CN113802122B (en) * | 2021-09-13 | 2024-02-27 | 万华化学集团电子材料有限公司 | Tungsten plug chemical mechanical polishing solution for reducing pitting corrosion and application thereof |
| CN114591686B (en) * | 2022-03-11 | 2023-05-26 | 万华化学集团电子材料有限公司 | Copper barrier layer chemical mechanical polishing solution and application thereof |
| CN119217158B (en) * | 2024-12-05 | 2025-03-18 | 中国人民解放军国防科技大学 | Ultra-smooth polishing method for NiP modified reflector |
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