CN113774392A - Cleaning solution used after chemical mechanical polishing and preparation method thereof - Google Patents
Cleaning solution used after chemical mechanical polishing and preparation method thereof Download PDFInfo
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- CN113774392A CN113774392A CN202110926058.9A CN202110926058A CN113774392A CN 113774392 A CN113774392 A CN 113774392A CN 202110926058 A CN202110926058 A CN 202110926058A CN 113774392 A CN113774392 A CN 113774392A
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- histidine
- cysteine
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- 238000004140 cleaning Methods 0.000 title claims abstract description 45
- 238000005498 polishing Methods 0.000 title abstract description 19
- 239000000126 substance Substances 0.000 title abstract description 8
- 238000002360 preparation method Methods 0.000 title abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 235000018417 cysteine Nutrition 0.000 claims abstract description 50
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims abstract description 50
- HNDVDQJCIGZPNO-UHFFFAOYSA-N histidine Natural products OC(=O)C(N)CC1=CN=CN1 HNDVDQJCIGZPNO-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000004094 surface-active agent Substances 0.000 claims abstract description 36
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims abstract description 23
- HNDVDQJCIGZPNO-YFKPBYRVSA-N L-histidine Chemical compound OC(=O)[C@@H](N)CC1=CN=CN1 HNDVDQJCIGZPNO-YFKPBYRVSA-N 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 16
- -1 alcohol amine Chemical class 0.000 claims abstract description 15
- 230000007797 corrosion Effects 0.000 claims abstract description 13
- 238000005260 corrosion Methods 0.000 claims abstract description 13
- 239000003112 inhibitor Substances 0.000 claims abstract description 13
- 235000001014 amino acid Nutrition 0.000 claims abstract description 12
- 150000001413 amino acids Chemical class 0.000 claims abstract description 12
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 11
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 11
- 239000002738 chelating agent Substances 0.000 claims abstract description 11
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical group C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 44
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 44
- OFOBLEOULBTSOW-UHFFFAOYSA-N malonic acid group Chemical group C(CC(=O)O)(=O)O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 44
- 239000000243 solution Substances 0.000 claims description 38
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical group NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 22
- 229960005070 ascorbic acid Drugs 0.000 claims description 22
- 235000010323 ascorbic acid Nutrition 0.000 claims description 22
- 239000011668 ascorbic acid Substances 0.000 claims description 22
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 20
- 235000006708 antioxidants Nutrition 0.000 claims description 10
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 125000005496 phosphonium group Chemical group 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- KYVBNYUBXIEUFW-UHFFFAOYSA-N 1,1,3,3-tetramethylguanidine Chemical compound CN(C)C(=N)N(C)C KYVBNYUBXIEUFW-UHFFFAOYSA-N 0.000 claims description 4
- KIZQNNOULOCVDM-UHFFFAOYSA-M 2-hydroxyethyl(trimethyl)azanium;hydroxide Chemical compound [OH-].C[N+](C)(C)CCO KIZQNNOULOCVDM-UHFFFAOYSA-M 0.000 claims description 4
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 claims description 4
- 239000007983 Tris buffer Substances 0.000 claims description 4
- ZRALSGWEFCBTJO-UHFFFAOYSA-N anhydrous guanidine Natural products NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 claims description 4
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 claims description 4
- 229960001231 choline Drugs 0.000 claims description 4
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 claims description 4
- LFETXMWECUPHJA-UHFFFAOYSA-N methanamine;hydrate Chemical compound O.NC LFETXMWECUPHJA-UHFFFAOYSA-N 0.000 claims description 4
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 2
- BJQWBACJIAKDTJ-UHFFFAOYSA-N tetrabutylphosphanium Chemical compound CCCC[P+](CCCC)(CCCC)CCCC BJQWBACJIAKDTJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 7
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000010949 copper Substances 0.000 description 17
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 16
- 229910052802 copper Inorganic materials 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000002791 soaking Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- VVNCNSJFMMFHPL-VKHMYHEASA-N D-penicillamine Chemical compound CC(C)(S)[C@@H](N)C(O)=O VVNCNSJFMMFHPL-VKHMYHEASA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- C23G1/205—Other heavy metals refractory metals
Abstract
The invention discloses a cleaning solution used after chemical mechanical polishing and a preparation method thereof. The cleaning liquid 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 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, wherein the balance is complemented by 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 solution has better effect of cleaning the BTA.
Description
Technical Field
The invention relates to a cleaning solution used after chemical mechanical polishing and a preparation method thereof.
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 current post-CMP cleaning solution, the cleaning solution for removing the BTA is a great technical difficulty. The present invention is a technical result obtained in the process of solving this technical problem.
Disclosure of Invention
The invention provides a cleaning solution used after chemical mechanical polishing and a preparation method thereof, aiming at overcoming the defect that the cleaning solution after CMP is difficult to remove BTA in the prior art. The cleaning solution has better effect of cleaning the BTA.
The present invention mainly solves the above-mentioned problems by the following technical means.
The invention provides a cleaning solution which is prepared from 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 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, wherein the balance of the water is complemented, and the sum of the mass fractions of the components is 100 percent; the amino acid is a combination of histidine and cysteine with the mass ratio of 1: 1; the structure of the surfactant is as follows:
In the present 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 hydroxide is preferably a quaternary ammonium hydroxide having a hydroxyl substituent, and 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, more preferably tetrabutylphosphine oxide.
The guanidine compound is preferably tetramethyl guanidine.
In the present invention, the alcohol amine is an alcohol amine which is conventional in the art, and monoethanolamine is preferred.
In the present invention, the antioxidant is an antioxidant conventionally used in the art, and ascorbic acid is preferred.
In the present invention, the corrosion inhibitor is a corrosion inhibitor conventional in the art, preferably 2-mercaptobenzothiazole.
In the present invention, the chelating agent is a chelating agent conventional in the art, preferably malonic acid.
In the present invention, the mass fraction of the strong base is preferably 1% to 20%, more preferably 5% to 15%, for example 15%.
In the present invention, the mass fraction of the alcohol amine is preferably 1% to 10%, more preferably 5% to 8%, for example 8%.
In the present invention, the antioxidant is preferably present at a mass fraction of 0.002% to 0.1%, more preferably 0.005% to 0.01%, for example 0.01%.
In the present invention, the surfactant is preferably present in a mass fraction of 0.01% to 0.05%, more preferably 0.01% to 0.02%, for example 0.01%, 0.02%, 0.05% or 0.1%.
In 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 present invention, 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 present invention, the mass fraction of the chelating agent is preferably 0.1% to 1%, more preferably 0.3% to 0.9%, for example, 0.9%.
Preferably, the raw materials of the cleaning solution consist of the strong base, the alcohol amine, the antioxidant, the surfactant, the amino acid, the corrosion inhibitor, the chelating agent and water, wherein the balance of the water is supplemented, and the sum of the mass fractions of the components is 100%.
In a 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: 15% of tetramethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% 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 2: 15% of tetramethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.01% 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 3: 15% 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: 15% 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 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 5: 15% of choline, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% of surfactant C, 0.02% of a combination of histidine and cysteine, 0.8% of 2-mercaptobenzothiazole, 0.9% of malonic acid and water, and the balance of water, wherein the sum of the mass fractions of the components is 100%; the mass ratio of histidine to cysteine is 1: 1;
scheme 6: 15% of tetrapropylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% 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 7: 15 percent of (2-hydroxyethyl) trimethyl ammonium hydroxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.02 percent of surfactant C, 0.02 percent of combination of histidine and cysteine, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid and water, wherein the water is used for complementing the balance, and the sum of the mass fractions of the components is 100 percent; the mass ratio of histidine to cysteine is 1: 1;
scheme 8: 15% of tris (2-2-hydroxyethyl) methylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% 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 9: 15% of tetrabutyl hydrogen phosphine oxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% 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 10: 15% of tetramethylguanidine, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% 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 was 1: 1.
The invention also provides a preparation method of the cleaning solution, which comprises the following steps: and mixing the raw materials of the cleaning solution.
In the preparation method, the temperature of the mixing is preferably room temperature, for example, 20 to 35 ℃.
The invention also provides application of the cleaning solution in cleaning a semiconductor device after chemical mechanical polishing. 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 positive progress effects of the invention are as follows: the cleaning solution has better effect of cleaning the BTA.
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.
In the following examples and comparative examples, the cleaning solution was prepared by the following steps: mixing the corresponding raw materials.
In the following examples, the specific operation temperature is not limited, and all the operations are carried out at room temperature.
The amino acids in tables 1 and 3 are histidine and cysteine combinations;
50% histidine and 50% cysteine mean that the mass ratio of histidine to cysteine is 1: 1;
70% histidine and 30% cysteine mean that the mass ratio of histidine to cysteine is 7: 3;
30% histidine and 70% cysteine mean that the mass ratio of histidine to cysteine is 3: 7.
The raw material components in the tables 1 and 3 are respectively and uniformly mixed according to the mass fractions in the tables 2 and 4, and water is used for complementing the balance to 100%.
In tables 1 and 3 below, the component species in each example also included water.
Table 1: EXAMPLES cleaning solution of each raw Material component
TABLE 2 example cleaning solutions for the mass fractions of the respective raw material components
Table 3: comparative example cleaning solution of 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:
the structural formula of the surfactant E is as follows:
Table 4 mass fractions of respective raw material components in comparative example cleaning liquid
The "balance" in tables 2 and 4 is the mass percentage of 100% minus the other components except water in each example.
Effect examples 1 to 10 and effect comparative examples 1 to 10: performance testing of cleaning solutions
Firstly, preparing a copper wafer:
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;
2. and cleaning with pure water and drying with nitrogen.
Secondly, 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.
BTA removal capability
The detection method 1:
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: different cleaning solutions are respectively used for soaking the copper sheet with the BTA film (soaking for 1min at 25 ℃), and the thickness is measured by a profilometer to represent the BTA removing effect.
The detection method 2 comprises the following steps:
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: the copper sheet with the BTA film is soaked in cleaning solution (soaking at 25 ℃ for 2min), and the contact angle of deionized water is tested.
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.
Table 5: examples 1-10 and comparative examples 1-10 Performance testing
The residual thickness of BTA in examples 1-10 ranged from-2 to 5nm, and the variation of contact angle ranged from-1 to 5; in comparative examples 1 to 10, the residual thickness of BTA was in the range of 6 to 10nm and the variation of contact angle was in the range of 6 to 10. The examples are more effective than the comparative examples, which shows that the cleaning solution of the present invention has a stronger BTA cleaning ability.
Claims (10)
1. The cleaning solution is prepared from 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 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, wherein the balance is complemented by water, and the sum of the mass fractions of the components is 100 percent; wherein the mass ratio of the amino acid to the histidine to the cysteine is 1:1 in combination; the surfactant is a surfactant C, and the structure of the surfactant C is as follows:
r ═ linear 16 carbon alkyl.
2. The cleaning solution as claimed in claim 1, wherein the strong base is one or more of quaternary ammonium base, quaternary phosphonium base and 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 cleaning solution according to claim 2, wherein the quaternary ammonium hydroxide is a quaternary ammonium hydroxide having a hydroxyl substituent;
and/or the quaternary phosphonium base is a quaternary phosphonium base with a hydroxyl substituent;
and/or the guanidine compound is tetramethylguanidine.
4. The cleaning solution according to claim 3, wherein the quaternary ammonium hydroxide having hydroxyl substituents is one or more of tetramethylammonium hydroxide, choline, tetrapropylammonium hydroxide, (2-hydroxyethyl) trimethylammonium hydroxide, and tris (2-2-hydroxyethyl) methylammonium hydroxide;
and/or said quaternary phosphonium base having hydroxyl substituents is tetrabutyl phosphine oxide.
5. The cleaning solution as claimed in claim 1, wherein the mass fraction of the strong base is 1% to 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 surfactant is 0.01-0.05%;
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 cleaning solution as claimed in claim 5, wherein the mass fraction of the strong base is 5% to 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 surfactant is 0.01-0.02%;
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 cleaning solution according to any one of claims 1 to 6, characterized in that it is prepared from the following raw materials consisting of the strong base, the alcohol amine, the antioxidant, the surfactant, the amino acid, the corrosion inhibitor, the chelating agent and water, wherein the balance is water, and the sum of the mass fractions of the components is 100%.
8. The cleaning solution according to claim 1, wherein the cleaning solution is prepared from the following raw materials, and the raw materials consist of the components shown in any one of the following schemes:
scheme 1: 15% of tetramethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% 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 2: 15% of tetramethylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.01% 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 3: 15% 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: 15% 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 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 5: 15% of choline, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% 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: 15% of tetrapropylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% 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 7: 15 percent of (2-hydroxyethyl) trimethyl ammonium hydroxide, 8 percent of monoethanolamine, 0.01 percent of ascorbic acid, 0.02 percent of surfactant C, 0.02 percent of combination of histidine and cysteine, 0.8 percent of 2-mercaptobenzothiazole, 0.9 percent of malonic acid and water, wherein the water is used for complementing the balance, and the sum of the mass fractions of the components is 100 percent; the mass ratio of histidine to cysteine is 1: 1;
scheme 8: 15% of tris (2-2-hydroxyethyl) methylammonium hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% 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 9: 15% of tetrabutyl hydrogen phosphine oxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% 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 10: 15% of tetramethylguanidine, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% 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 was 1: 1.
9. A method for preparing a cleaning fluid according to any one of claims 1 to 8, comprising the steps of: and mixing the raw materials.
10. The method of claim 9, wherein the temperature of the mixing is 20 to 35 ℃.
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