CN113774391B - Application of cleaning liquid after chemical mechanical polishing - Google Patents
Application of cleaning liquid after chemical mechanical polishing Download PDFInfo
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- CN113774391B CN113774391B CN202110926048.5A CN202110926048A CN113774391B CN 113774391 B CN113774391 B CN 113774391B CN 202110926048 A CN202110926048 A CN 202110926048A CN 113774391 B CN113774391 B CN 113774391B
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/16—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions using inhibitors
- C23G1/18—Organic inhibitors
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/20—Other heavy metals
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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
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
Abstract
The invention discloses application of a cleaning solution after chemical mechanical polishing. The application of the cleaning liquid in cleaning the semiconductor device after chemical mechanical polishing is specifically disclosed, wherein the cleaning liquid comprises the following raw materials in percentage by mass: 0.01 to 25 percent of strong alkali, 0.01 to 30 percent of alcohol amine, 0.001 to 1 percent of antioxidant, 0.05 to 0.2 percent of surfactant, 0.01 to 0.1 percent of amino acid, 0.01 to 10 percent of corrosion inhibitor, 0.01 to 10 percent of chelating agent and water, the balance being water, and the sum of the mass fractions of the components is 100 percent; wherein the amino acid is a combination of histidine and cysteine. The cleaning liquid has the effect of better cleaning BTA.
Description
Technical Field
The invention relates to application of a cleaning solution after chemical mechanical polishing.
Background
Metal materials such as copper, aluminum, tungsten, etc. are commonly used wire 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 liquid generally contains abrasive particles, complexing agents, metal corrosion inhibitors, oxidizing agents, and the like. Wherein the abrasive particles are mainly silicon dioxide, aluminum oxide, silicon dioxide doped with aluminum or covered with aluminum, cerium oxide, titanium dioxide, macromolecule abrasive particles and the like. After the metal CMP process, the wafer surface is contaminated with metal ions and abrasive particles themselves in the polishing liquid, which can affect the electrical characteristics of the semiconductor and the reliability of the device. These metal ions and abrasive particle residues can affect the planarity of the wafer surface, which can reduce device performance and affect subsequent processing or device operation. Therefore, after the metal CMP process, it is necessary to remove metal ions, metal corrosion inhibitors, and abrasive grains remaining on the wafer surface, improve the hydrophilicity of the wafer surface after cleaning, and reduce surface defects.
At present, cleaning of BTA by cleaning liquid is a great technical difficulty in the development process of cleaning liquid after CMP. The invention is the technical result obtained in the process of solving the technical problem.
Disclosure of Invention
The invention aims to overcome the defect that the BTA is difficult to clean by the cleaning liquid after CMP in the prior art, and provides an application of the cleaning liquid after chemical mechanical polishing. The cleaning liquid has the effect of better cleaning BTA.
The invention mainly solves the technical problems through the following technical means.
The invention provides application of a cleaning solution in cleaning a semiconductor device subjected to chemical mechanical polishing, which is prepared from the following raw materials in parts by mass: 0.01% -25% of strong alkali, 0.01% -30% of alcohol amine, 0.001% -1% of antioxidant, 0.05% -0.2% of surfactant, 0.01% -0.1% of amino acid, 0.01% -10% of corrosion inhibitor, 0.01% -10% of chelating agent and water, wherein the balance is water, and the sum of the mass fractions of the components is 100%; wherein the mass ratio of the histidine to the cysteine of the amino acid is 1:1, a combination of two or more of the above; the surfactant is surfactant C, and has the structure:
in the application of the invention, the strong base is a strong base conventional in the art, preferably one or more of quaternary ammonium base, quaternary phosphonium base and guanidine compound, more preferably quaternary ammonium base.
The quaternary ammonium base is preferably a quaternary ammonium base having a hydroxyl substituent, more preferably one or more of tetramethylammonium hydroxide, choline, tetrapropylammonium hydroxide, (2-hydroxyethyl) trimethylammonium hydroxide and tris (2-2-hydroxyethyl) methylammonium hydroxide.
The quaternary phosphonium base is preferably a quaternary phosphonium base having a hydroxyl substituent, and more preferably tetrabutylphosphine hydroxide.
The guanidine compound is preferably tetramethyl guanidine.
In the application of the invention, the alcohol amine is conventional alcohol amine in the field, preferably monoethanolamine.
In the application of the invention, the antioxidant is an antioxidant which is conventional in the art, preferably ascorbic acid.
In the application of the invention, the corrosion inhibitor is a corrosion inhibitor which is conventional in the field, preferably 2-mercaptobenzothiazole.
In the application of the invention, the chelating agent is a chelating agent conventional in the art, preferably malonic acid.
In the applications of the present invention, the mass fraction of the strong base is preferably 1% to 30%, more preferably 5% to 20%, for example 20%.
In the applications of the present invention, the alcohol amine is preferably 1% to 10% by mass, more preferably 5% to 8% by mass, for example 8% by mass.
In the applications of the present invention, the antioxidant is preferably 0.002% -0.1% by mass, more preferably 0.005% -0.01% by mass, for example 0.01% by mass.
In the applications of the present invention, the surfactant is preferably present in an amount of 0.05% to 0.1%, more preferably 0.05% to 0.075%, for example 0.05%, 0.075%, 0.1% or 0.2%.
In the application of the present invention, the mass fraction of the amino acid is preferably 0.01% to 0.05%, more preferably 0.01% to 0.02%, for example 0.02%.
In the applications according to the invention, the corrosion inhibitor is preferably present in an amount of 0.1% to 1%, more preferably 0.5% to 0.8%, for example 0.8%.
In the applications of the present invention, the chelating agent is preferably present in an amount of 0.1% to 1%, more preferably 0.3% to 0.9%, for example 0.9%.
Preferably, in the application, the cleaning solution is prepared from the raw materials of the strong alkali, the alcohol amine, the antioxidant, the surfactant, the amino acid, the corrosion inhibitor, the chelating agent and water, wherein the water is used for supplementing the balance, and the sum of the mass fractions of the components is 100%.
In a certain preferred embodiment of the present invention, the raw materials of the cleaning solution may be composed of components shown in any one of the following schemes:
scheme 1:20% of tetramethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 2:20% of tetramethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.1% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 3:20% of tetramethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.05% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the balance is water, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 4:20% of tetramethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.2% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 5:20% of choline, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the balance is water, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 6:20% of tetrapropylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 7:20% of (2-hydroxyethyl) trimethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 8:20% of tris (2-2-hydroxyethyl) methyl ammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 9:20% of tetrabutylphosphine hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of histidine and cysteine combination, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the balance is water, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 10:20% of tetramethylguanidine, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1.
The semiconductor device is preferably one or more of a copper-based chip, a cobalt-based chip and a tungsten-based chip, for example, a copper-based chip.
The above preferred conditions can be arbitrarily combined on the basis of not deviating from the common knowledge in the art, and thus, each preferred embodiment of the present invention can be obtained.
The invention has the positive progress effects that: the cleaning liquid has the effect of better cleaning BTA.
Detailed Description
The invention is further illustrated by means of the following examples, which are not intended to limit the scope of the invention. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
In the following examples and comparative examples, the preparation method of the cleaning liquid includes the following steps: mixing the corresponding raw materials.
In the following examples, the specific operating temperatures are not limited, and all refer to being conducted under room temperature conditions.
The amino acids in tables 1 and 3 are histidine and cysteine combinations;
50% histidine +50% cysteine means that the mass ratio of histidine to cysteine is 1:1;
70% histidine+30% cysteine means that the mass ratio of histidine to cysteine is 7:3;
30% histidine +70% cysteine means that the mass ratio of histidine to cysteine is 3:7.
The raw material components in tables 1 and 3 are uniformly mixed according to the mass fractions in tables 2 and 4, respectively, and the balance is made up to 100% by water.
In tables 1 and 3 below, the component types in each example also include water.
Table 1: example cleaning solution raw material components
TABLE 2 mass fractions of raw material components in cleaning liquid of examples
Table 3: comparative example cleaning solution Each raw material component
The structural formula of the surfactant A is as follows:
the structural formula of the surfactant B is as follows:
the structural formula of the surfactant D is as follows:
TABLE 4 mass fractions of raw material components in comparative cleaning liquid
The "balance" in tables 2 and 4 is the mass percent of the components other than water subtracted from 100% in each example.
Effect examples 1 to 10 and effect comparative examples 1 to 10: performance test of cleaning liquid
1. Preparation of copper wafers:
1. pretreatment: for an 8 inch electroplated Cu wafer (copper plating thickness of about 1 um), 10% H was used 2 SO 4 Treating at 25deg.C for 2min;
2. blowing nitrogen after cleaning by pure water;
2. polishing:
the polishing machine table is 8' Mirra, the rotation speed of a polishing disk and a polishing head is 93/87rpm, the flow rate of polishing liquid 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 is AEP U3000, and the barrier layer polishing solution is TCU2000H4. The prepared copper wafer is subjected to polishing treatment.
3. BTA removal capability
The detection method 1 comprises the following steps:
1. cutting the polished copper wafer into square pieces of 3cm x 3 cm;
2. treating with 3% citric acid at 25deg.C for 2min; soaking a copper sheet in 1+1 nitric acid solution for 2min at 25 ℃, and then testing the thickness of the copper by adopting a surface profiler;
3. blowing nitrogen after cleaning by pure water;
4. film formation of Cu-BTA: soaking the treated copper sheet in a sulfuric acid solution of 3% hydrogen peroxide and 0.5% BTA and 20ppm at 25 ℃ for 10min;
5. removal of BTA: the copper sheets (soaked for 1min at 25 ℃) of the long BTA film are soaked by different cleaning liquids respectively, and the thickness is measured by a profilometer to represent the removal effect of the BTA.
The detection method 2 comprises the following steps:
1. cutting the polished copper wafer into square pieces of 3cm x 3 cm;
2. treating with 3% citric acid at 25deg.C for 2min; post-testing the contact angle of deionized water;
3. blowing nitrogen after cleaning by pure water;
4. film formation of Cu-BTA: soaking the treated copper sheet in a sulfuric acid solution of 3% hydrogen peroxide and 0.5% BTA and 20ppm at 25 ℃ for 10min; testing the contact angle of deionized water;
5. removal of BTA: soaking a copper sheet (soaked for 2min at 25 ℃) after a long BTA film is soaked by a cleaning solution, and testing the contact angle of deionized water;
the BTA film has a certain hydrophobicity and is characterized by the difference of contact angles measured in step 5 minus step 2. If the difference is larger and positive, the BTA residual is more.
Table 5: performance test of examples 1-10 and comparative examples 1-10
The residual thickness of BTA in examples 1-10 ranged from-2 to 4nm, and the contact angle varied from 1 to 5; the residual thickness of BTA in comparative examples 1-10 ranged from 6-10nm, and the contact angle varied from 6-10. The effect of the example is better than that of the comparative example, which shows that the cleaning liquid has stronger cleaning ability to BTA in the application of the cleaning liquid.
Claims (10)
1. Use of a cleaning solution for cleaning a semiconductor device after chemical mechanical polishing, said cleaning solution being prepared from the following raw materials, said raw materials comprising the following components in mass fraction: 0.01% -25% of strong alkali, 0.01% -30% of alcohol amine, 0.001% -1% of antioxidant, 0.05% -0.2% of surfactant, 0.01% -0.1% of amino acid, 0.01% -10% of corrosion inhibitor, 0.01% -10% of chelating agent and water, wherein the balance is water, and the sum of the mass fractions of the components is 100%; wherein the amino acid is histidine and cysteine with the mass ratio of 1:1, a combination of two or more of the above; the surfactant is surfactant C, and the structure is as follows:
，n=14。
2. the use of claim 1, wherein the strong base is one or more of a quaternary ammonium base, a quaternary phosphonium base, and a guanidine compound;
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.
3. The use according to claim 2, wherein the quaternary ammonium base is a quaternary ammonium base having a hydroxy substituent;
and/or the quaternary phosphonium base is a quaternary phosphonium base with hydroxyl substituent;
and/or the guanidine compound is tetramethyl guanidine.
4. The use according to claim 3, wherein the quaternary ammonium base having a hydroxy substituent is one or more of tetramethylammonium hydroxide, choline, tetrapropylammonium hydroxide, (2-hydroxyethyl) trimethylammonium hydroxide and tris (2-2-hydroxyethyl) methylammonium hydroxide;
and/or the quaternary phosphonium base with hydroxyl substituent is tetrabutylphosphine hydroxide.
5. The use according to claim 1, wherein the mass fraction of the strong base is 1% -30%;
and/or, the alcohol amine is 1-10% by mass;
and/or, the mass fraction of the antioxidant is 0.002% -0.1%;
and/or, the mass fraction of the surfactant is 0.05% -0.1%;
and/or, the mass fraction of the amino acid 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%.
6. The use according to claim 5, wherein the mass fraction of the strong base is 5% to 20%;
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 surfactant is 0.05% -0.075%;
and/or the mass fraction of the amino acid is 0.01% -0.02%;
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%.
7. The use according to any one of claims 1 to 6, wherein the cleaning solution is prepared from the following raw materials, wherein the raw materials comprise the strong base, the alcohol amine, the antioxidant, the surfactant, the amino acid, the corrosion inhibitor, the chelating agent and water, the water is used for the balance, and the sum of the mass fractions of the components is 100%.
8. The use according to claim 1, wherein the cleaning solution is prepared from the following raw materials, said raw materials consisting of the components according to any one of the following schemes:
scheme 1:20% of tetramethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 2:20% of tetramethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.1% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 3:20% of tetramethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.05% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the balance is water, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 4:20% of tetramethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.2% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 5:20% of choline, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the balance is water, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 6:20% of tetrapropylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 7:20% of (2-hydroxyethyl) trimethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 8:20% of tris (2-2-hydroxyethyl) methyl ammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 9:20% of tetrabutylphosphine hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of histidine and cysteine combination, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the balance is water, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1;
scheme 10:20% of tetramethylguanidine, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.075% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, wherein the water makes up the balance, and the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1:1.
9. The use of claim 1, wherein the semiconductor device is one or more of a copper-based chip, a cobalt-based chip, and a tungsten-based chip.
10. The use of claim 9, wherein the semiconductor device is a copper-based chip.
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