CN113215584A - Preparation method of cleaning solution after chemical mechanical polishing - Google Patents

Preparation method of cleaning solution after chemical mechanical polishing Download PDF

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CN113215584A
CN113215584A CN202110488661.3A CN202110488661A CN113215584A CN 113215584 A CN113215584 A CN 113215584A CN 202110488661 A CN202110488661 A CN 202110488661A CN 113215584 A CN113215584 A CN 113215584A
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percent
cleaning solution
mass
scheme
base
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CN113215584B (en
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王溯
马丽
史筱超
何加华
李健华
王真
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Shanghai Xinyang Semiconductor Material Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/16Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions using inhibitors
    • C23G1/18Organic inhibitors
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/20Other heavy metals
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/20Other heavy metals
    • C23G1/205Other heavy metals refractory metals

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Abstract

The invention discloses a preparation method of a cleaning solution after chemical mechanical polishing. The preparation method of the cleaning solution comprises the following steps: mixing the raw materials; the cleaning solution comprises the following raw materials in parts by mass: 0.01 to 25 percent of strong base, 0.01 to 30 percent of alcohol amine, 0.001 to 1 percent of antioxidant, 0.01 to 0.1 percent of copper complex shown as the formula A, 0.01 to 10 percent of corrosion inhibitor, 0.01 to 10 percent of chelating agent, 0.01 to 5 percent of surfactant and 14 to 75 percent of water, wherein the sum of the mass fractions of the components is 100 percent. The cleaning solution prepared by the invention has stronger cleaning capability, lower corrosion rate, stronger BTA removing capability and better stability, and can simultaneously realize the effects of cleaning, corrosion inhibition and BTA removing.

Description

Preparation method of cleaning solution after chemical mechanical polishing
Technical Field
The invention relates to a preparation method of a cleaning solution after chemical mechanical polishing.
Background
Metal materials such as copper, aluminum, tungsten, etc. are commonly used as conductive line materials in integrated circuits. Chemical Mechanical Polishing (CMP) is a major technique for wafer planarization in the fabrication of devices. The metal chemical mechanical polishing solution generally contains abrasive particles, a complexing agent, a metal corrosion inhibitor, an oxidizing agent, and the like. The abrasive particles are mainly silicon dioxide, aluminum oxide, aluminum-doped or aluminum-coated silicon dioxide, cerium dioxide, titanium dioxide, polymer abrasive particles, and the like. After the metal CMP process, the wafer surface is contaminated with metal ions and abrasive particles themselves in the slurry, which can affect the electrical characteristics of the semiconductor and the reliability of the device. The residues of these metal ions and abrasive particles can affect the flatness of the wafer surface, which can degrade device performance and affect subsequent processing or device operation. Therefore, it is very necessary to remove metal ions, metal corrosion inhibitors and abrasive particles remaining on the wafer surface after the metal CMP process, to improve the hydrophilicity of the cleaned wafer surface, and to reduce surface defects.
In the development process of the cleaning solution after CMP at present, how to consider cleaning, corrosion inhibition and Benzotriazole (BTA) removal is a great technical difficulty in the synergistic development of the cleaning solution, the corrosion inhibition and the Benzotriazole (BTA).
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to develop a brand-new product and improve the performance of CMP in all aspects, and provides a preparation method of a cleaning solution after chemical mechanical polishing. The cleaning solution prepared by the invention has stronger cleaning capability, lower corrosion rate, stronger BTA removing capability and better stability, and can simultaneously realize cleaning, corrosion inhibition and BTA removing.
The invention provides a preparation method of a cleaning solution, which comprises the following steps: mixing the raw materials; wherein the raw materials comprise the following components in percentage by mass: 0.01 to 25 percent of strong base, 0.01 to 30 percent of alcohol amine, 0.001 to 1 percent of antioxidant, 0.01 to 0.1 percent of copper complex shown as the formula A, 0.01 to 10 percent of corrosion inhibitor, 0.01 to 10 percent of chelating agent, 0.01 to 5 percent of surfactant and 14 to 75 percent of water, wherein the sum of the mass fractions of the components is 100 percent;
Figure BDA0003042594560000021
in the preparation method, the strong base is a conventional strong base in the field, and preferably, the strong base is selected from one or more of quaternary ammonium base, quaternary phosphonium base and guanidine compound; more preferably, the strong base is a quaternary ammonium base, also for example tetramethylammonium hydroxide.
The quaternary ammonium base is preferably a tetraalkyl quaternary ammonium base and/or a quaternary ammonium base having a hydroxyl substituent on the alkyl group.
The tetraalkyl quaternary ammonium base is preferably tetramethyl ammonium hydroxide and/or tetrapropyl ammonium hydroxide; such as tetramethylammonium hydroxide.
The quaternary ammonium base having a hydroxyl substituent on the alkyl group is preferably one or more of choline, (2-hydroxyethyl) trimethylammonium hydroxide and tris (2-hydroxyethyl) methylammonium hydroxide.
The quaternary phosphonium base is preferably a tetraalkyl quaternary phosphonium base and/or a quaternary phosphonium base substituted with a hydroxyl group on the alkyl group; more preferably, the quaternary phosphonium base is tetrabutyl phosphine oxide.
The guanidine compound is preferably tetramethylguanidine.
In the preparation method, the alcohol amine is conventional in the field, and is preferably monoethanolamine.
In the preparation method, the antioxidant is a conventional antioxidant in the field, and is preferably ascorbic acid.
In the preparation method, the corrosion inhibitor is a corrosion inhibitor conventional in the field, and is preferably 2-mercaptobenzothiazole.
In the preparation method, the chelating agent is a chelating agent conventional in the field, and is preferably malonic acid.
In the preparation method, the surfactant is a conventional surfactant in the field; the surfactant is preferably an ionic surfactant or a non-ionic surfactant, more preferably a non-ionic surfactant, such as dodecylbenzene sulfonic acid.
In the preparation method, the water is water conventional in the field, and the water is pure water; preferably, the water is selected from one or more of deionized water, distilled water and ultrapure water.
In the preparation method, the mass fraction of the strong base is preferably 1% to 20%, and more preferably, the mass fraction of the strong base is 5% to 15%, for example, 20%, 15%, 5%, or 10%.
In the preparation method, the mass fraction of the alcohol amine is preferably 1% to 10%, more preferably 5% to 8%, for example 8%.
In the preparation method, the mass fraction of the antioxidant is preferably 0.002% to 0.1%, more preferably 0.005% to 0.01%, for example, 0.01%.
In the preparation method, the mass fraction of the copper complex shown in the formula a is preferably 0.01% to 0.05%, and more preferably, the mass fraction of the copper complex shown in the formula a is 0.01% to 0.03%, for example, 0.025%, 0.01%, 0.05%, or 0.1%.
In the preparation method, the mass fraction of the corrosion inhibitor is preferably 0.1% to 1%, more preferably 0.5% to 0.8%, for example 0.8%.
In the preparation method, the mass fraction of the chelating agent is preferably 0.1% to 1%, more preferably 0.3% to 0.9%, for example 0.9%.
In the preparation method, the mass fraction of the surfactant is preferably 0.1% to 1%, more preferably 0.2% to 0.7%, for example 0.7%.
Preferably, the cleaning solution comprises the following raw materials in percentage by mass: 0.01 to 25 percent of strong base, 0.01 to 30 percent of alcohol amine, 0.001 to 1 percent of antioxidant, 0.01 to 0.1 percent of copper complex shown as the formula A, 0.01 to 10 percent of corrosion inhibitor, 0.01 to 10 percent of chelating agent, 0.01 to 5 percent of surfactant and water for the balance, wherein the sum of the mass fractions of the components is 100 percent.
In a preferred embodiment, the cleaning solution is prepared from the following raw materials in scheme 1, scheme 2, scheme 3, scheme 4, scheme 5, scheme 6, scheme 7, scheme 8, scheme 9 or scheme 10:
in the scheme 1, the raw materials of the cleaning solution consist of the following components in percentage by mass: 15 percent of tetramethylammonium hydroxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.025 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100 percent;
in the scheme 2, the raw materials of the cleaning solution consist of the following components in percentage by mass: 15 percent of tetramethylammonium hydroxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.01 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100 percent;
in the scheme 3, the raw materials of the cleaning solution consist of the following components in percentage by mass: 15 percent of tetramethylammonium hydroxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.05 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100 percent;
in the scheme 4, the raw materials of the cleaning solution consist of the following components in percentage by mass: 5 percent of tetramethylammonium hydroxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.01 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100 percent;
in the scheme 5, the raw materials of the cleaning solution consist of the following components in percentage by mass: 15% of choline, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.1% of copper complex shown as formula A, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid, 0.7% of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100%;
in the scheme 6, the cleaning solution comprises the following raw materials in percentage by mass: 5% of tetrapropylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.025% of copper complex shown as formula A, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid, 0.7% of dodecylbenzene sulfonic acid and water for balancing, wherein the sum of the mass fractions of the components is 100%;
in the scheme 7, the raw materials of the cleaning solution consist of the following components in percentage by mass: 20 percent of (2-hydroxyethyl) trimethyl ammonium hydroxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.025 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100 percent;
in the scheme 8, the raw materials of the cleaning solution consist of the following components in percentage by mass: 10% of tris (2-2-hydroxyethyl) methyl ammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.025% of copper complex shown as the formula A, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid, 0.7% of dodecylbenzene sulfonic acid, and the balance of water, wherein the sum of the mass fractions of the components is 100%;
in the scheme 9, the raw materials of the cleaning solution consist of the following components in percentage by mass: 15 percent of tetrabutyl hydrogen phosphine oxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.025 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid and water to make up the balance, wherein the sum of the mass fractions of the components is 100 percent.
In the scheme 10, the raw materials of the cleaning solution consist of the following components in percentage by mass: 15 percent of tetramethylguanidine, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.025 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100 percent.
In the preparation method, the mixing is preferably performed by adding the solid in the raw materials into the liquid and uniformly stirring.
In the preparation method, the temperature of the mixing is preferably room temperature; for example 20 to 35 deg.c.
In the preparation method, preferably, the preparation method further comprises shaking and/or filtering; the purpose of the shaking is to mix the raw material components thoroughly, the shaking speed and time are not limited, and the filtration is to remove insoluble substances.
Preferably, the cleaning solution is a cleaning solution for a semiconductor device after chemical mechanical polishing, and more preferably, the semiconductor device is preferably one or more of a copper-based chip, a cobalt-based chip and a tungsten-based chip, such as a copper-based chip.
The above preferred conditions can be arbitrarily combined to obtain preferred embodiments of the present invention without departing from the common general knowledge in the art.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows: the cleaning solution prepared by the invention has stronger cleaning capability, lower corrosion rate, stronger BTA removing capability and better stability, and can simultaneously realize the effects of cleaning, corrosion inhibition and BTA removing.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
First, preparation of cleaning solutions of examples 1 to 10 and comparative examples 1 to 3
The preparation method comprises the following steps:
the component types of the examples and the comparative examples also comprise water, and the raw materials of the components of the examples and the comparative examples are mixed. The temperature of mixing was room temperature. After mixing, the method further comprises shaking and filtering operations.
The raw material compositions of examples 1 to 10 are shown in Table 1.
TABLE 1
Figure BDA0003042594560000061
The structure of the copper (I) complex is shown as formula A:
Figure BDA0003042594560000062
the contents of the respective raw materials of examples 1 to 10 are shown in Table 2 (less than 100% of the raw materials were made up with water).
TABLE 2
Figure BDA0003042594560000071
The raw material compositions of comparative examples 1 to 3 are shown in Table 3.
TABLE 3
Figure BDA0003042594560000072
The methylene bridged 1, 8-naphthyridine ligand is shown as the following formula
Figure BDA0003042594560000073
The complex of the biquinoline phenylphosphine cuprous bromide (I) is shown as the following formula
Figure BDA0003042594560000074
The copper (III) sulfate complex is cuprous tris (1-isocyano-2-methoxy-2-methylpropane) sulfate.
The contents of the respective raw materials of comparative examples 1 to 3 are shown in Table 4 (less than 100% of the total amount was made up with water).
TABLE 4
Figure BDA0003042594560000081
Performance test of cleaning solutions of examples 1 to 10 and comparative examples 1 to 3
1. Preparation of copper wafers:
1.1, pretreatment: for the wafer (copper plating thickness about 1um) after 8 inches of Cu electroplating, 10% H is adopted2SO4Treating at 25 deg.C for 2 min;
1.2, cleaning with pure water, and drying with nitrogen;
2. polishing:
the polishing machine is 8' Mirra, the rotating speed of the polishing disk and the polishing head is 93/87rpm, the flow rate of the polishing solution is 150ml/min, the polishing pad used for copper polishing is IC1010, and the polishing pad used for barrier layer polishing is Fujibo H7000. The copper polishing solution was AEP U3000 and the barrier polishing solution was TCU2000H 4. The prepared copper wafer is subjected to a polishing process.
3. Detection of ER
The test method comprises the following steps:
3.1, cutting the polished copper wafer into square pieces of 3cm by 3 cm;
3.2, measuring the thickness of the copper wafer and the functional relation of the resistivity of the copper wafer by adopting a four-point probe instrument to generate a regression curve, and determining the functional relation of the thickness of the copper and the resistivity for calculating the corrosion rate of the copper;
3.3, soaking 50ml of cleaning solution at 25 ℃ for 1min for corrosion;
and 3.4, measuring the resistance by a four-point probe instrument, then calculating the thickness change of the metal before and after corrosion, and calculating the corrosion rate.
4. Surface corrosion detection
The test method comprises the following steps:
4.1, cutting the polished copper wafer into square pieces of 3cm by 3 cm;
4.2, soaking the substrate for 1min at 25 ℃ by adopting a cleaning solution for corrosion;
4.3, the copper wafer after etching is subjected to Atomic Force Microscope (AFM) test to test the RMS value.
5. Cleaning capability detection
The test method comprises the following steps:
5.1, cutting the polished copper wafer into square pieces of 3cm by 3 cm;
5.2, soaking and cleaning for 2min in a cleaning solution at 25 ℃;
5.3, observation under SEM.
6. BTA removal capability
BTA residual thickness (nm) detection method:
1. cutting the polished copper wafer into square pieces of 3cm by 3 cm;
2. treating with 3% citric acid at 25 deg.C for 2 min; soaking the copper sheet in 1+1 nitric acid solution for 2min at 25 ℃, and then testing the thickness of the copper by using a surface profiler;
3. cleaning with pure water and drying with nitrogen;
4. Cu-BTA film formation: soaking the treated copper sheet in a 3% hydrogen peroxide solution, 0.5% BTA and 20ppm sulfuric acid solution at 25 ℃ for 10 min;
5. BTA removal: soaking the copper sheet with the BTA film in different cleaning solutions (soaking for 1min at 25 ℃), and measuring the thickness by using a profilometer to represent the BTA removal effect;
detection of change in contact angle:
1. cutting the polished copper wafer into square pieces of 3cm by 3 cm;
2. treating with 3% citric acid at 25 deg.C for 2 min; then testing the contact angle of the deionized water;
3. cleaning with pure water and drying with nitrogen;
4. Cu-BTA film formation: soaking the treated copper sheet in a 3% hydrogen peroxide solution, 0.5% BTA and 20ppm sulfuric acid solution at 25 ℃ for 10 min; testing the contact angle of deionized water;
5. BTA removal: soaking the copper sheet with the BTA film in a cleaning solution (soaking for 2min at 25 ℃), and testing the contact angle of deionized water;
the BTA film has certain hydrophobicity, and whether the BTA is completely removed or not is characterized by subtracting the contact angle measured in the step 2 from the step 5. The more BTA residuals are accounted for if the difference is larger and positive.
7. Solution stability testing
0.4 liter of the cleaning solution was poured into a 0.5L plastic container, the remaining 0.1 liter was filled with nitrogen gas, and the following changes were observed in the placement for 4 days, 7 days, and 1 month:
1. a change in color of the solution;
2. the generation of bubbles;
3. a change in pH;
4. change in copper corrosion rate (detection method same as before);
5. the AFM detects the change in surface roughness RMS (detection method same as that described above).
Evaluation criteria for effects:
the results of the performance test and the results of the stability test of the cleaning liquids of examples 1 to 10 and the cleaning liquids of comparative examples 1 to 3 are shown in tables 5 to 12.
Table 5: EXAMPLES 1-10 cleaning solution Performance test results (fresh formulation)
Figure BDA0003042594560000101
Table 6: examples 1-10 stability test results (day 4)
Figure BDA0003042594560000102
Figure BDA0003042594560000111
Table 7: examples 1-10 stability test results (day 7)
Figure BDA0003042594560000112
Table 8: examples 1-10 stability test results (day 30)
Figure BDA0003042594560000113
Table 9: comparative examples 1-3 cleaning solution Performance test results (fresh preparation)
Figure BDA0003042594560000114
Table 10: comparative examples 1-3 stability test results (day 4)
Figure BDA0003042594560000121
Table 11: comparative examples 1-3 stability test results (day 7)
Figure BDA0003042594560000122
Table 12: comparative examples 1-3 stability test results (month 1)
Figure BDA0003042594560000123
According to the cleaning solution performance test results (tables 5 and 9) of examples 1 to 10 and comparative examples 1 to 3, compared with the cleaning solution of the comparative example, the cleaning solution of the present invention has stronger cleaning ability, lower corrosion rate and stronger BTA removal ability, and can simultaneously achieve cleaning, corrosion inhibition and BTA removal. According to the cleaning solution stability test results of examples 1 to 10 and comparative examples 1 to 3 (tables 6 to 8 and tables 10 to 12, the cleaning solution of the present invention did not significantly deteriorate at 1 month (30 days) compared to the cleaning solution of the comparative example, and the cleaning solution remained colorless and free of bubbles.

Claims (10)

1. The preparation method of the cleaning solution is characterized by comprising the following steps of: mixing the raw materials; wherein the raw materials comprise the following components in percentage by mass: 0.01 to 25 percent of strong base, 0.01 to 30 percent of alcohol amine, 0.001 to 1 percent of antioxidant, 0.01 to 0.1 percent of copper complex shown as the formula A, 0.01 to 10 percent of corrosion inhibitor, 0.01 to 10 percent of chelating agent, 0.01 to 5 percent of surfactant and 14 to 75 percent of water, wherein the sum of the mass fractions of the components is 100 percent;
Figure FDA0003042594550000011
2. the method for preparing a cleaning solution according to claim 1, wherein the strong base is one or more selected from the group consisting of quaternary ammonium bases, quaternary phosphonium bases and guanidine compounds;
and/or, the alcohol amine is monoethanolamine;
and/or, the antioxidant is ascorbic acid;
and/or the corrosion inhibitor is 2-mercaptobenzothiazole;
and/or, the chelating agent is malonic acid;
and/or the surfactant is an ionic surfactant or a nonionic surfactant.
3. The method for preparing the cleaning solution according to claim 2, wherein the strong base is one or more selected from the group consisting of quaternary ammonium bases, quaternary phosphonium bases and guanidine compounds; the quaternary ammonium base is tetraalkyl quaternary ammonium base and/or quaternary ammonium base with hydroxyl substituent on alkyl;
and/or the strong base is selected from one or more of quaternary ammonium base, quaternary phosphonium base and guanidine compound; the quaternary phosphonium base is tetraalkyl quaternary phosphonium base and/or quaternary phosphonium base with hydroxyl substituted on the alkyl;
and/or the strong base is selected from one or more of quaternary ammonium base, quaternary phosphonium base and guanidine compound; the guanidine compound is tetramethylguanidine;
and/or, the water is pure water;
and/or the mass fraction of the strong base is 1-20%;
and/or the mass fraction of the alcohol amine is 1-10%;
and/or the mass fraction of the antioxidant is 0.002% -0.1%;
and/or the mass fraction of the copper complex shown as the formula A is 0.01-0.05%;
and/or the mass fraction of the corrosion inhibitor is 0.1-1%;
and/or the mass fraction of the chelating agent is 0.1-1%;
and/or the mass fraction of the surfactant is 0.1-1%.
4. The method for preparing a cleaning solution according to claim 3, wherein the strong base is one or more selected from the group consisting of quaternary ammonium bases, quaternary phosphonium bases and guanidine compounds; the quaternary ammonium base is tetraalkyl quaternary ammonium base and/or quaternary ammonium base with hydroxyl substituent on alkyl; the tetraalkyl quaternary ammonium hydroxide is tetramethylammonium hydroxide and/or tetrapropylammonium hydroxide;
and/or the strong base is selected from one or more of quaternary ammonium base, quaternary phosphonium base and guanidine compound; the quaternary ammonium base is tetraalkyl quaternary ammonium base and/or quaternary ammonium base with hydroxyl substituent on alkyl; the quaternary ammonium base with hydroxyl substituent on the alkyl is one or more of choline, (2-hydroxyethyl) trimethyl ammonium hydroxide and tri (2-hydroxyethyl) methyl ammonium hydroxide;
and/or the strong base is selected from one or more of quaternary ammonium base, quaternary phosphonium base and guanidine compound; the quaternary phosphonium base is tetrabutyl phosphine oxide;
and/or the surfactant is a nonionic surfactant;
and/or, the water is selected from one or more of deionized water, distilled water and ultrapure water;
and/or the mass fraction of the strong base is 5-15%;
and/or, the mass fraction of the alcohol amine is 5% -8%;
and/or the mass fraction of the antioxidant is 0.005% -0.01%;
and/or the mass fraction of the copper complex shown as the formula A is 0.01-0.03%;
and/or the mass fraction of the corrosion inhibitor is 0.5-0.8%;
and/or the mass fraction of the chelating agent is 0.3-0.9%;
and/or the mass fraction of the surfactant is 0.2-0.7%.
5. The method for preparing a cleaning solution according to claim 2, wherein the surfactant is dodecylbenzenesulfonic acid;
and/or, the strong base is a quaternary ammonium base; such as tetramethylammonium hydroxide;
and/or the mass fraction of the strong base is 20%, 15%, 5% or 10%;
and/or the mass fraction of the alcohol amine is 8%;
and/or the mass fraction of the antioxidant is 0.01 percent;
and/or the mass fraction of the copper complex shown as the formula A is 0.025%, 0.01%, 0.05% or 0.1%;
and/or the mass fraction of the corrosion inhibitor is 0.8%;
and/or the mass fraction of the chelating agent is 0.9%;
and/or the mass fraction of the surfactant is 0.7%.
6. The method for preparing the cleaning solution as claimed in claim 1, wherein the raw materials of the cleaning solution comprise the following components in parts by mass: 0.01 to 25 percent of strong base, 0.01 to 30 percent of alcohol amine, 0.001 to 1 percent of antioxidant, 0.01 to 0.1 percent of copper complex shown as the formula A, 0.01 to 10 percent of corrosion inhibitor, 0.01 to 10 percent of chelating agent, 0.01 to 5 percent of surfactant and water for the balance, wherein the sum of the mass fractions of the components is 100 percent.
7. The method for producing a cleaning solution according to claim 1, wherein a raw material of the cleaning solution is a solution of scheme 1, scheme 2, scheme 3, scheme 4, scheme 5, scheme 6, scheme 7, scheme 8, scheme 9 or scheme 10:
in the scheme 1, the raw materials of the cleaning solution consist of the following components in percentage by mass: 15 percent of tetramethylammonium hydroxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.025 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100 percent;
in the scheme 2, the raw materials of the cleaning solution consist of the following components in percentage by mass: 15 percent of tetramethylammonium hydroxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.01 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100 percent;
in the scheme 3, the raw materials of the cleaning solution consist of the following components in percentage by mass: 15 percent of tetramethylammonium hydroxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.05 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100 percent;
in the scheme 4, the raw materials of the cleaning solution consist of the following components in percentage by mass: 5 percent of tetramethylammonium hydroxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.01 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100 percent;
in the scheme 5, the raw materials of the cleaning solution consist of the following components in percentage by mass: 15% of choline, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.1% of copper complex shown as formula A, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid, 0.7% of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100%;
in the scheme 6, the cleaning solution comprises the following raw materials in percentage by mass: 5% of tetrapropylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.025% of copper complex shown as formula A, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid, 0.7% of dodecylbenzene sulfonic acid and water for balancing, wherein the sum of the mass fractions of the components is 100%;
in the scheme 7, the raw materials of the cleaning solution consist of the following components in percentage by mass: 20 percent of (2-hydroxyethyl) trimethyl ammonium hydroxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.025 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100 percent;
in the scheme 8, the raw materials of the cleaning solution consist of the following components in percentage by mass: 10% of tris (2-2-hydroxyethyl) methyl ammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.025% of copper complex shown as the formula A, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid, 0.7% of dodecylbenzene sulfonic acid, and the balance of water, wherein the sum of the mass fractions of the components is 100%;
in the scheme 9, the raw materials of the cleaning solution consist of the following components in percentage by mass: 15 percent of tetrabutyl hydrogen phosphine oxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.025 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100 percent;
in the scheme 10, the raw materials of the cleaning solution consist of the following components in percentage by mass: 15 percent of tetramethylguanidine, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.025 percent of copper complex shown as a formula A, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid, 0.7 percent of dodecylbenzene sulfonic acid, and water for balancing, wherein the sum of the mass fractions of the components is 100 percent.
8. The cleaning solution preparation method according to any one of claims 1 to 7, further comprising shaking and/or filtration;
and/or the cleaning solution is a cleaning solution for the semiconductor device after chemical mechanical polishing.
9. The method for preparing a cleaning solution according to claim 8, wherein the cleaning solution is a cleaning solution for a semiconductor device after chemical mechanical polishing, and the semiconductor device is one or more of a copper-based chip, a cobalt-based chip, and a tungsten-based chip;
and/or the temperature of the mixing is room temperature.
10. The method for preparing a cleaning solution according to claim 9, wherein the temperature of the mixing is 20 to 35 ℃;
and/or the cleaning solution is used for cleaning a semiconductor device after chemical mechanical polishing, and the semiconductor device is a copper-based chip.
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CN115323383A (en) * 2022-08-09 2022-11-11 河南大学 Preparation method of hydrotalcite composite coating modified by ionic liquid corrosion inhibitor and application of hydrotalcite composite coating in magnesium alloy corrosion prevention

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