CN110813891B - Cleaning solution and cleaning method for cleaning abrasive particles after copper CMP - Google Patents

Cleaning solution and cleaning method for cleaning abrasive particles after copper CMP Download PDF

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Publication number
CN110813891B
CN110813891B CN201911116905.4A CN201911116905A CN110813891B CN 110813891 B CN110813891 B CN 110813891B CN 201911116905 A CN201911116905 A CN 201911116905A CN 110813891 B CN110813891 B CN 110813891B
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cleaning
cleaning solution
chelating agent
deionized water
copper
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CN110813891A (en
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檀柏梅
杨柳
殷达
何彦刚
王如
孙晓琴
张师浩
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Shenzhen Zhongwang Lihua Microelectronic Material Co ltd
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Hebei University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/0005—Other compounding ingredients characterised by their effect
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/044—Hydroxides or bases

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
  • Detergent Compositions (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

The invention relates to a cleaning solution and a cleaning method for cleaning abrasive particles after copper CMP. The cleaning solution comprises an active agent, a chelating agent, a pH regulator and deionized water; the cleaning solution comprises the following components in percentage by mass: 0.01-0.5% of active agent, 0.01-0.05% of chelating agent and the balance of deionized water; the pH value of the cleaning solution is 9-12; the active agent is an anionic surfactant and a nonionic surfactant, and the mass ratio of the anionic surfactant to the nonionic surfactant is 1: 1-3; the anionic surfactant is ADS; the nonionic surfactant is specifically AEO. The invention lays a foundation for realizing high-efficiency cleaning and low-cost cleaning of the sheet brushing machine of the composite active agent after copper CMP.

Description

Cleaning solution and cleaning method for cleaning abrasive particles after copper CMP
Technical Field
The invention belongs to a CMP cleaning solution and a using method thereof, and particularly relates to a composite cleaning solution for removing silica sol abrasive particles and a cleaning method thereof.
Background
With the continuous development of semiconductor integrated circuits, the minimum line width of the integrated circuits is continuously reduced, and the surface defects are requiredThe demand is higher and higher, the cleaning difficulty is correspondingly increased, and the position of the cleaning process in the chip generation process is more and more important. Chemical Mechanical Polishing (CMP) is currently the most widely used global planarization technique. The cleanliness and surface condition of the polished surface are critical for manufacturing high-quality semiconductor devices. Quickly adsorbing abrasive SiO in polishing solution after CMP2Particles, single SiO2Scanning Electron Microscope (SEM) test images of particle contamination and horse honeycomb polar images. Due to SiO2The particles are adsorbed on the surface of the copper wire, and nail holes are easily formed during photoetching and ion implantation, so that short circuit and open circuit of the device are caused, the performance of the device is influenced, and the device is even failed, so that the quality and the quality rate of the semiconductor device are reduced. Therefore, the cleaning effect of post-CMP cleaning on the abrasive particles adsorbed and embedded on the wafer surface is a key factor related to the performance of semiconductor integrated circuits, and the research on the cleaning technology is more and more focused while the integrated circuits are rapidly developed.
After the semiconductor integrated circuit enters 28nm, the thickness of the barrier layer is required to be less than 2nm, and the barrier layer material generally adopts novel materials such as cobalt (Co) or ruthenium (Ru). Cobalt or ruthenium is easily vaporized in an acidic environment, and the product is toxic and pollutes the environment, and the acidic cleaning agent is easy to cause interface corrosion. The alkaline cleaner can solve these problems well, and therefore the research of the alkaline cleaner is of great significance. The currently used alkaline cleaning agent in the world is mainly ammonium hydroxide (NH)4OH) system, tetramethylammonium hydroxide (TMAH) system, etc., NH4OH can severely corrode copper surfaces, TMAH is easily decomposed and evaporated into the environment, and in addition, TMAH is toxic and can pose a series of health problems.
Disclosure of Invention
The invention aims to overcome the defects of the technology and provides a formula and a method for cleaning silica sol abrasive particles after copper CMP. The cleaning solution adopts a form of compounding a macromolecular nonionic surfactant and a micromolecular anionic surfactant, and the nonionic surfactant can effectively reduce the surface tension of the cleaning solution; the anionic surfactant can generate repulsion with the negatively charged copper surface after wrapping the adsorption particles, so that secondary deposition of the particles is not easy to occur, the removal of silica sol particles can be effectively improved, and the surface roughness is reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
a cleaning solution for cleaning abrasive particles after copper CMP comprises an active agent, a chelating agent, a pH regulator and deionized water; the cleaning solution comprises the following components in percentage by mass: 0.01-0.5% of active agent, 0.01-0.05% of chelating agent and the balance of deionized water; the pH value of the cleaning solution is 9-12;
the active agent is an anionic surfactant and a nonionic surfactant, and the mass ratio of the anionic surfactant to the nonionic surfactant is 1: 1-3;
the chelating agent is an FA/OII type chelating agent; the pH regulator is inorganic alkali solution with the concentration of 1-10 g/L;
the inorganic base is potassium hydroxide KOH or cesium hydroxide CsOH.
The anionic surfactant is Ammonium Dodecyl Sulfate (ADS); the nonionic surfactant is fatty alcohol polyoxyethylene ether (AEO).
The preparation method of the cleaning solution for cleaning the abrasive particles after copper CMP comprises the following steps:
adding the chelating agent and the active agent into deionized water according to the proportion under stirring, mixing, adding the pH regulator, and continuing stirring until the pH value reaches 9-12 to obtain the cleaning solution.
The use method of the cleaning solution for cleaning the abrasive particles after copper CMP comprises the following steps:
before a brushing machine is used for cleaning, a wafer copper sheet is soaked in 0.01-0.02% of FA/OII chelating agent for 2-3 minutes, then the wafer copper sheet is placed on the brushing machine, the rotating speed of the brushing machine is set to be 100 r/min-250 r/min, the brush interval is set to be 0-1.25mm, the flow rate of cleaning liquid is set to be 0.5L/min-1.5L/min, the cleaning time is 10 s-100 s, the deionized water flushing time is set to be 30 s-150 s, the ultrasonic time is set to be 10 s-100 s, the spin-drying time is set to be 20 s-150 s, and the nitrogen blow-drying time is set to be 20 s-150 s, so that the copper sheet is cleaned.
The invention has the substantive characteristics that:
in the cleaning solution for cleaning silica sol abrasive particles after copper CMP, the cleaning solution adopts a compound form of a macromolecular active agent and a micromolecular active agent, so that the spatial repulsion between the adsorbed abrasive particles is improved, the nonionic surfactant can effectively reduce the surface tension of the cleaning solution, the surface tension is low, the cleaning solution is easy to spread on the surface of a wafer, the more components are in gaps with the surface, and the better cleaning effect is. The anionic surfactant ADS has a hydrophilic group with negative charges, and generates repulsion with the copper surface with negative charges after the adsorption particles are wrapped, so that secondary deposition of the particles is less likely to occur, removal of silica sol particles can be effectively improved, and surface roughness can be reduced. The FA/OII type chelating agent is alkaline, under alkaline condition, the FA/OII type chelating agent is mixed with CuO and Cu (OH)XReacting to generate stable and soluble copper amine complex ions, so that SiO2The chemical adsorption bond of the particles is broken and separated from the surface of the copper wire, which is beneficial to the removal of the particles. The soaked copper sheet can effectively chelate copper ions generated in the polishing process, change the surface charged state, and enable the adsorption of particles on the surface to be in a physical adsorption state, and the particles cannot be changed into a bonding state due to the surface charging. The application of the cleaning machine enables the brushing efficiency to be higher, the brushing efficiency to be more uniform than manual brushing, the same cleaning conditions can be ensured every time, and the optimal technological parameters for removing the silica sol particles are further obtained.
The invention has the beneficial effects that: compared with the prior art, the invention lays a foundation for realizing high-efficiency cleaning and low-cost cleaning of the sheet brushing machine of the composite active agent after copper CMP. In particular:
1. the cleaning solution adopts a composite active agent, a chelating agent and an inorganic base pH regulator as main components, a brushing machine is used for cleaning, a macromolecular nonionic surfactant and a micromolecular anionic surfactant are used in a composite mode, the coverage area of the surfaces of silica sol particles is increased, the electrostatic repulsion among the particles is improved, the particles are favorably removed, the formula and the method are obviously superior to the commercially available cleaning solution, the cleaning efficiency is improved, the silica sol abrasive particles can be effectively removed, the surface roughness is improved, the roughness is reduced from the nanometer level to the Hermite level, the number of the surface residual particles is reduced by one order of magnitude, the equipment is not corroded, the components are simple, and the cost can be reduced.
2. Compared with the traditional cleaning process, the method of soaking by using the chelating agent is adopted before the cleaning by using the brushing machine, so that the copper ions generated in the polishing process can be effectively chelated, the surface charge state is changed, the adsorption of the particles on the surface is in a physical adsorption state, and the particles cannot be changed into a bonding state due to the surface charge. With this cleaning method, the particle removal efficiency is improved by 5%.
3. Aiming at the silica sol abrasive particles remained on the surface of the copper after CMP, the cleaning solution and the cleaning method are optimized, the cleaning efficiency is finally improved, the particles are effectively removed, and the method has great guiding value for practical engineering application.
Drawings
FIG. 1AFM image of a copper surface after cleaning of example 1;
FIG. 2AFM image of copper surface after cleaning of example 2.
FIG. 3AFM image of copper surface after cleaning of example 3.
Detailed Description
The following detailed description of the preferred embodiments will be made in conjunction with the accompanying drawings.
The pH regulator is prepared by adding 10g of KOH into 1L of deionized water for dilution, and uniformly stirring the mixture to be used as the pH regulator, or adding 2g of CsOH into 1L of deionized water for dilution, and uniformly stirring the mixture to be used as the pH regulator.
Example 1
Preparing 5kg of composite cleaning solution for removing silica sol abrasive particles after copper CMP:
adding an FA/OII chelating agent (Tianjin Jingling microelectronic materials Co., Ltd.) into deionized water while stirring, then respectively adding a nonionic surfactant AEO and an anionic surfactant ADS while stirring, then adding a pH regulator CsOH solution, adjusting the pH value to 10.5, complementing the balance with deionized water, and uniformly stirring to obtain 5kg of composite cleaning solution; wherein the mass percentage of each component is as follows: 0.015% of chelating agent, 0.15% of nonionic surfactant AEO and 0.05% of ADS.
Soaking an 8-inch copper sheet for 3 minutes by using an FA/OII chelating agent with the mass concentration of 0.01%, then putting the wafer copper sheet on a sheet brushing machine, wherein the rotating speed of the sheet brushing machine is 200r/min, the brush interval is-0.75 mm, the flow of the obtained cleaning liquid is 1.2L/min, the cleaning time is 30s, the deionized water flushing time is 90s, the ultrasonic time is 30s, the spin-drying time is 50s, and the nitrogen blow-drying time is 40 s.
The results were: as can be seen from the AFM test chart of FIG. 1, the copper surface roughness after the brushing was 0.413nm, compared to 11.4nm before the cleaning, the silica sol particles were substantially removed to obtain a clean copper surface.
Example 2
5kg of composite cleaning solution for removing silica sol abrasive particles after copper CMP is prepared.
Adding an FA/OII chelating agent (Tianjin Jingling microelectronic materials Co., Ltd.) into deionized water while stirring, then respectively adding a nonionic surfactant AEO and an anionic surfactant ADS while stirring, then adding a pH regulator KOH solution, adjusting the pH value to 10.0, complementing the balance with deionized water, and uniformly stirring to obtain 5kg of composite cleaning solution; wherein the mass percentage of each component is as follows: 0.015% of chelating agent, 0.2% of nonionic surfactant AEO and 0.1% of ADS.
Soaking an 8-inch copper sheet for 2 minutes by using an FA/OII chelating agent with the mass concentration of 0.015%, then putting the wafer copper sheet on a sheet brushing machine, wherein the rotating speed of the sheet brushing machine is 100r/min, the brush interval is-0.25 mm, the flow of a cleaning solution is 1.0L/min, the cleaning time is 50s, the deionized water washing time is 50s, the ultrasonic time is 40s, the spin-drying time is 60s, and the nitrogen blow-drying time is 50 s.
The results were: as can be seen from the AFM test chart of FIG. 2, the copper surface roughness after the wafer brushing machine cleaning was 0.489nm, compared to 11.4nm before cleaning, the silica sol particles were substantially removed to obtain a clean copper surface.
Example 3
5kg of composite cleaning solution for removing silica sol abrasive particles after copper CMP is prepared.
Adding an FA/OII chelating agent (Tianjin Jingling microelectronic materials Co., Ltd.) into deionized water while stirring, then respectively adding a nonionic surfactant AEO and an anionic surfactant ADS while stirring, then adding a pH regulator KOH solution, adjusting the pH value to 11.0, complementing the balance with deionized water, and uniformly stirring to obtain 5kg of composite cleaning solution; wherein the mass percentage of each component is as follows: 0.05% of chelating agent, 0.25% of nonionic surfactant AEO and 0.25% of ADS.
Soaking an 8-inch copper sheet for 2 minutes by using an FA/OII chelating agent with the mass concentration of 0.02%, then placing a copper wafer on a sheet brushing machine, wherein the rotating speed of the sheet brushing machine is 250r/min, the brush interval is-1.25 mm, the flow of a cleaning solution is 1.2L/min, the cleaning time is 80s, the deionized water flushing time is 150s, the ultrasonic time is 80s, the spin-drying time is 100s, and the nitrogen blow-drying time is 80 s.
The results were: as can be seen from the AFM test chart of FIG. 3, the copper surface roughness after the brushing was 0.425nm, compared to 11.4nm before the cleaning, the silica sol particles were substantially removed to obtain a clean copper surface.
The nonionic surfactant and the FA/OII type chelating agent are commercially available from Tianjin Brilliant microelectronic materials Co. Other surfactants are commercially available anionic surfactants ADS and nonionic surfactants AEO.
The cleaning solution of the invention adopts a form of compounding a macromolecular nonionic surfactant and a micromolecular anionic surfactant, and the two surfactants are jointly adsorbed on the surface of silica sol particles to form mixed micelles. The covering coefficient of the surfaces of the colloidal particles is increased, so that the active agent and the silica sol particles are more fully wrapped, the spatial repulsion potential is improved due to the increase of the covering rate, the electrostatic repulsion among the colloidal particles is increased, the particles are less prone to agglomeration, and the dispersibility of the abrasive particles in the cleaning solution can be improved. The nonionic surfactant can effectively reduce the surface tension of the cleaning solution, the surface tension is low, the cleaning solution is easy to spread on the surface of the wafer, the contact with components in surface gaps is more, and the cleaning effect is better. The anionic surfactant ADS has a hydrophilic group with negative charges, and generates repulsion with the copper surface with negative charges after the adsorption particles are wrapped, so that secondary deposition of the particles is less likely to occur, removal of silica sol particles can be effectively improved, and surface roughness can be reduced.
The copper sheet is soaked in the FA/OII type chelating agent solution for 2-3 minutes, so that copper ions generated in the polishing process can be effectively chelated, the surface charge state is changed, the adsorption of particles on the surface is in a physical adsorption state, and the particles cannot be changed into a bonding state due to the surface charge. The application of the cleaning machine enables the brushing efficiency to be higher, the brushing efficiency to be more uniform than manual brushing, the same cleaning conditions can be ensured every time, and the optimal technological parameters for removing the silica sol particles are further obtained.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the structure of the present invention in any way. Any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention still fall within the scope of the technical solution of the present invention.
The invention is not the best known technology.

Claims (1)

1. A cleaning solution for cleaning abrasive particles after copper CMP is characterized in that the cleaning solution comprises an active agent, a chelating agent, a pH regulator and deionized water; the cleaning solution comprises the following components in percentage by mass: 0.01-0.5% of active agent, 0.01-0.05% of chelating agent and the balance of deionized water; the pH value of the cleaning solution is 9-12;
the active agent is an anionic surfactant and a nonionic surfactant, and the mass ratio of the anionic surfactant to the nonionic surfactant is 1: 1-3;
the chelating agent is an FA/OII type chelating agent; the pH regulator is inorganic alkali solution; the concentration of the inorganic alkali solution is 1-10 g/L;
the anionic surfactant is Ammonium Dodecyl Sulfate (ADS); the nonionic surfactant is fatty alcohol polyoxyethylene ether (AEO);
the inorganic base is potassium hydroxide (KOH) or cesium hydroxide (CsOH);
the preparation method of the cleaning solution for cleaning the abrasive particles after copper CMP is characterized by comprising the following steps of:
adding an active agent and a chelating agent into deionized water according to the proportion under stirring, mixing, adding a pH regulator, and continuing stirring until the pH value reaches 9-12 to obtain the cleaning solution;
the using method of the cleaning solution for cleaning the abrasive particles after copper CMP is characterized by comprising the following steps of:
before a brushing machine is used for cleaning, a wafer copper sheet is soaked in an FA/OII type chelating agent with the mass concentration of 0.01-0.02% for 2-3 minutes, then the wafer copper sheet is placed on the brushing machine, the rotating speed of the brushing machine is set to be 100-250 r/min, the distance between brushes is set to be 0-1.25mm, the flow of the obtained cleaning liquid is 0.5L/min-1.5L/min, the cleaning time is 10-100 s, the deionized water flushing time is 30-150 s, the ultrasonic time is 10-100 s, the spin-drying time is 20-150 s, and the nitrogen blow-drying time is 20-150 s, so that the copper sheet is cleaned.
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CN112175756A (en) * 2020-11-05 2021-01-05 河北工业大学 Cleaning solution for removing surface residues after CMP of multi-layer copper interconnection barrier layer
CN115124983B (en) * 2021-03-29 2023-11-28 中国石油天然气股份有限公司 Water-based cleaning agent and preparation method and application thereof
CN115261152B (en) * 2022-08-05 2024-03-29 长鑫存储技术有限公司 Cleaning agent and application thereof

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