CN113774392B - Cleaning liquid for chemical mechanical polishing and preparation method thereof - Google Patents
Cleaning liquid for chemical mechanical polishing and preparation method thereof Download PDFInfo
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- CN113774392B CN113774392B CN202110926058.9A CN202110926058A CN113774392B CN 113774392 B CN113774392 B CN 113774392B CN 202110926058 A CN202110926058 A CN 202110926058A CN 113774392 B CN113774392 B CN 113774392B
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- 238000004140 cleaning Methods 0.000 title claims abstract description 47
- 239000007788 liquid Substances 0.000 title abstract description 23
- 238000005498 polishing Methods 0.000 title abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000000126 substance Substances 0.000 title abstract description 8
- 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 35
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims abstract description 24
- HNDVDQJCIGZPNO-YFKPBYRVSA-N L-histidine Chemical compound OC(=O)[C@@H](N)CC1=CN=CN1 HNDVDQJCIGZPNO-YFKPBYRVSA-N 0.000 claims abstract description 24
- -1 alcohol amine Chemical class 0.000 claims abstract description 15
- 239000002994 raw material Substances 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
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 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
- 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
- 239000002585 base Substances 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 20
- 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
- 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
- AOTOMVRCWUMWDC-UHFFFAOYSA-N CCCCP(CCCC)(CCCC)CCCC.O Chemical group CCCCP(CCCC)(CCCC)CCCC.O AOTOMVRCWUMWDC-UHFFFAOYSA-N 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
- 125000002887 hydroxy group Chemical group [H]O* 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
- 239000000463 material Substances 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 7
- 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
- 235000012431 wafers Nutrition 0.000 description 10
- 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
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 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
- 238000002791 soaking Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 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
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000007664 blowing Methods 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
- 238000011056 performance test 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
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- 229910000420 cerium 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
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 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
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000012545 processing Methods 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 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, 0.01 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, 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 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 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 BTA is difficult to clean by cleaning liquid after CMP in the prior art, and provides a cleaning liquid after chemical mechanical polishing and a preparation method thereof. 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 a cleaning solution 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, 0.01% -0.1% 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%; the amino acid is a combination of histidine and cysteine in a mass ratio of 1:1; the surfactant has the structure that:
r=linear 16-carbon alkyl.
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 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 present invention, the alcohol amine is alcohol amine conventional in the art, preferably monoethanolamine.
In the present invention, the antioxidant is an antioxidant conventionally used in the art, preferably ascorbic acid.
In the present invention, the corrosion inhibitor is a conventional corrosion inhibitor 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 alcohol amine is preferably 1% to 10% by mass, more preferably 5% to 8% by mass, for example 8% by mass.
In the present invention, the antioxidant is preferably 0.002% to 0.1%, more preferably 0.005% to 0.01%, for example 0.01%.
In the present invention, the surfactant is preferably 0.01% to 0.05%, more preferably 0.01% to 0.02%, for example 0.01%, 0.02%, 0.05% or 0.1% by mass.
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 chelating agent is preferably 0.1% to 1%, more preferably 0.3% to 0.9%, for example 0.9%.
Preferably, the cleaning solution is prepared from the raw materials of strong alkali, alcohol amine, antioxidant, surfactant, amino acid, corrosion inhibitor, chelating agent and water, wherein the balance is water, 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 1:15% 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 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 2:15% 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 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 3:15% 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 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 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 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 5:15% 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 being water, wherein the sum of the mass percentages 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 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 7:15% of (2-hydroxyethyl) trimethylammonium 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 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 8:15% of tris (2-2-hydroxyethyl) methyl ammonium 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 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 9:15% of tetrabutylphosphine hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% of surfactant C, 0.02% of 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 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 invention also provides a preparation method of the cleaning liquid, which comprises the following steps: mixing the raw materials of the cleaning liquid.
In the preparation process, the temperature of the mixing is preferably room temperature, for example 20 to 35 ℃.
The invention also provides application of the cleaning liquid in cleaning the 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, 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:
the structural formula of the surfactant E is as follows:
r=linear 16-carbon alkyl
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. and (5) drying with nitrogen after pure water cleaning.
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: and (3) soaking the copper sheet (soaked for 2min at 25 ℃) after the BTA film is soaked by the cleaning liquid, 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 5nm, 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 examples have better results than the comparative examples, indicating that the cleaning liquid of the present invention has a stronger BTA cleaning ability.
Claims (10)
1. The cleaning fluid is prepared from the following raw materials in parts 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, 0.01 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, the balance being water, and the sum of the mass fractions of the components is 100 percent; 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:r=linear 16-carbon alkyl.
2. The cleaning solution 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 cleaning solution of claim 2 wherein said quaternary ammonium base is a hydroxyl-substituted quaternary ammonium base;
and/or the quaternary phosphonium base is a quaternary phosphonium base with hydroxyl substituent;
and/or the guanidine compound is tetramethyl guanidine.
4. A cleaning solution 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 cleaning solution of claim 1, wherein the strong base is present in an amount of 1% to 20% by mass;
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 0.01% -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 of claim 5, wherein the strong base has a mass fraction of 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 of any one of claims 1-6, 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, and the balance is water, and the sum of the mass fractions of the components is 100%.
8. The cleaning solution of claim 1, prepared from the following materials, said materials consisting of the components according to 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 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 2:15% 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 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 3:15% 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 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 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 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 5:15% 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 percentages 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 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 7:15% of (2-hydroxyethyl) trimethylammonium 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 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 8:15% of tris (2-2-hydroxyethyl) methyl ammonium 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 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 9:15% of tetrabutylphosphine hydroxide, 8% of monoethanolamine, 0.01% of ascorbic acid, 0.02% of surfactant C, 0.02% of 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 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. A method for preparing a cleaning solution according to any one of claims 1 to 8, comprising the steps of: mixing the raw materials.
10. The method of claim 9, wherein the temperature of the mixing is 20 to 35 ℃.
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