CN116905052A - Additive for inhibiting variable-amplitude wide-edge copper junction and preparation method thereof - Google Patents
Additive for inhibiting variable-amplitude wide-edge copper junction and preparation method thereof Download PDFInfo
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- CN116905052A CN116905052A CN202310860711.5A CN202310860711A CN116905052A CN 116905052 A CN116905052 A CN 116905052A CN 202310860711 A CN202310860711 A CN 202310860711A CN 116905052 A CN116905052 A CN 116905052A
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- tpm
- copper
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- inhibitor
- junction
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- 239000010949 copper Substances 0.000 title claims abstract description 50
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 49
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000000654 additive Substances 0.000 title claims abstract description 33
- 230000000996 additive effect Effects 0.000 title claims abstract description 33
- 230000002401 inhibitory effect Effects 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 101100537780 Mus musculus Tpm2 gene Proteins 0.000 claims abstract description 27
- 101100537773 Solanum lycopersicum TPM-1 gene Proteins 0.000 claims abstract description 22
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 36
- 239000003112 inhibitor Substances 0.000 claims description 22
- 238000005282 brightening Methods 0.000 claims description 19
- 239000002202 Polyethylene glycol Substances 0.000 claims description 17
- 229920001223 polyethylene glycol Polymers 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 239000007810 chemical reaction solvent Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 10
- 239000012964 benzotriazole Substances 0.000 claims description 9
- 125000003354 benzotriazolyl group Chemical group N1N=NC2=C1C=CC=C2* 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- -1 polydithio-dipropyl Polymers 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- FRTIVUOKBXDGPD-UHFFFAOYSA-M sodium;3-sulfanylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CCCS FRTIVUOKBXDGPD-UHFFFAOYSA-M 0.000 claims description 5
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 5
- 238000013329 compounding Methods 0.000 claims description 2
- 239000011888 foil Substances 0.000 abstract description 28
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 abstract description 4
- 238000000151 deposition Methods 0.000 abstract description 3
- 230000008021 deposition Effects 0.000 abstract description 3
- 238000005868 electrolysis reaction Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 125000000168 pyrrolyl group Chemical group 0.000 abstract description 2
- 238000005956 quaternization reaction Methods 0.000 abstract description 2
- OKJPEAGHQZHRQV-UHFFFAOYSA-N Triiodomethane Natural products IC(I)I OKJPEAGHQZHRQV-UHFFFAOYSA-N 0.000 abstract 1
- 239000003792 electrolyte Substances 0.000 description 21
- 238000006243 chemical reaction Methods 0.000 description 15
- 239000011889 copper foil Substances 0.000 description 11
- 238000009713 electroplating Methods 0.000 description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 7
- 239000002253 acid Substances 0.000 description 7
- 229910000365 copper sulfate Inorganic materials 0.000 description 7
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 7
- 239000010936 titanium Substances 0.000 description 7
- 229910052719 titanium Inorganic materials 0.000 description 7
- OBDVFOBWBHMJDG-UHFFFAOYSA-M 3-sulfanylpropane-1-sulfonate Chemical compound [O-]S(=O)(=O)CCCS OBDVFOBWBHMJDG-UHFFFAOYSA-M 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 2
- 244000046052 Phaseolus vulgaris Species 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention belongs to the technical field of metal electrolysis foil production, and particularly relates to a variable-amplitude wide-edge copper junction inhibiting additive and a preparation method thereof. In order to solve the problem of copper bonding in the electrolytic foil production process, the additive of the invention is prepared by connecting Triphenylmethane (TPM) with three pyrrole rings to obtain TPM-1 and then carrying out quaternization reaction with iodomethane to obtain TPM-2, wherein the TPM-2 utilizes the small molecular structure of the TPM-1 and I ‑ The mutual cooperation controls copper deposition under the nano scale, can effectively inhibit the continuous growth trend of junction copper, and simultaneously realizes the control of the copper junction degree with high precision and high efficiency on the basis of saving labor cost compared with the existing manual copper removal method.
Description
Technical Field
The invention belongs to the technical field of metal electrolysis foil production, and particularly relates to a variable-amplitude wide-edge copper junction inhibiting additive and a preparation method thereof.
Background
With the rapid development of the electronic information industry and the power battery industry in recent years, the demand of copper foil is gradually increasing. In the electronics industry, copper foil is used as the primary material for Copper Clad Laminates (CCL) and Printed Circuit Boards (PCB); in the energy storage field, the excellent conductivity of copper foil makes it one of the important raw materials for lithium current collectors. Among the methods for producing copper foil again, the electrodeposition copper production method is the main process for producing copper foil at home and abroad due to the advantages of cost process and the like.
In order to meet the requirements of copper foils with different widths in the industry, a shielding layer is adopted to treat the anode and cathode so as to prepare copper foils with different widths. In the electrolytic foil production process, copper beans (hereinafter referred to as copper bonding) which are difficult to strip easily appear at the edge of the shielding layer, the quantity of copper bonding is large, and copper bonding particles are large. Because the running time of the electrolytic machine is long, copper beans are long, and the problems of tearing edges of raw foil, risk of a cathode roller motor, concave-convex points on the foil surface and the like are easily caused.
The nucleation mode of copper shows that the copper growth trend is generally tip nucleation, and the cathode roller has certain surface roughness (Rz) in the copper plating process, so that the hole bottom current density is small, the hole opening current density is large and the uneven local current density distribution accelerates the hole opening copper deposition rate in the electroplating process, thereby leading to the generation of junction copper. When the cathode is treated by the shielding layer, the surface roughness (Rz) of the cathode roller at the edge of the shielding layer is further amplified, and the problem of copper bonding is more obvious.
Disclosure of Invention
In order to solve the problem of copper bonding in the electrolytic foil production process, the invention provides the additive for inhibiting the copper bonding at the wide side of the variable amplitude and the preparation method thereof, wherein the additive is prepared by connecting Triphenylmethane (TPM) with three pyrrole rings to obtain TPM-1 and then carrying out quaternization reaction with methyl iodide to obtain TPM-2, and the TPM-2 utilizes the small molecular structure and the I-interaction of the TPM-1 to control copper deposition under the nanoscale, so that the tendency of continuous growth of the copper bonding can be effectively inhibited, and compared with the existing manual copper removing method, the additive can simultaneously realize high-precision and high-efficiency control of the copper bonding degree on the basis of saving labor cost.
In order to achieve the technical purpose, the technical scheme of the invention is realized as follows:
the additive for inhibiting variable-amplitude wide-edge copper bonding comprises 5-16 ppm, 2-9 ppm, 0.1-3 ppm, 0.2-2 ppm and deionized water, wherein the weight percentages of the brightening agent, the inhibitor, the leveling agent and the TPM-2 are respectively 5-16 ppm, 2-9 ppm, 0.1-2 ppm and the balance of deionized water.
Further, the brightening agent is one or a mixture of several of sodium polydithio-dipropyl sulfonate (SPS), 3-mercapto-1-propane sulfonate (MPS) and thiourea according to any ratio.
Further, the inhibitor is polyethylene glycol (PEG).
Further, the leveling agent is benzotriazole.
Further, the preparation method of the TPM-2 comprises the following steps: methyl iodide, TPM-1 and a reaction solvent NMP are mixed and reacted for 4 to 6 hours at the temperature of 80 to 90 ℃ to obtain TPM-2.
Still further, the molar ratio of methyl iodide to TPM-1 is 1:1.
A preparation method of a copper additive for inhibiting variable width edge junction comprises the following steps:
step 1, mixing methyl iodide, TPM-1 and a reaction solvent NMP, and reacting for 4-6 hours at 80-90 ℃ to obtain TPM-2;
and 2, after cooling to room temperature, compounding TPM-2, brightening agent, inhibitor, leveling agent and deionized water according to a proportion to obtain the additive.
Compared with the prior art, the invention has the following beneficial effects:
the phenomenon of copper bonding caused by edge defects can be effectively inhibited by introducing new components TPM-1 and I-. The action mechanism is mainly that Cu is treated by a three-fold symmetrical micromolecule structure of TPM-1 2+ But the same as the common leveling agent, the leveling agent and TPM-1 are in a reversible adsorption and desorption process in the charge concentration area, which means that when the thickness of the copper foil approaches the height of the copper junction, the leveling agent moves to the next tip nuclear point to cover, and the nuclear point is formed to further grow the copper junction; when I-is introduced, TPM-1 realizes irreversible adsorption and desorption under the action of I-to prevent the nucleation point from growing continuously, thereby inhibiting copper formation.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which are derived by a person skilled in the art based on the embodiments of the invention, fall within the scope of protection of the invention.
Example 1
In this example, the brightening agent is sodium polydithio-dipropyl sulfonate (SPS), the inhibitor is polyethylene glycol (PEG), and the leveling agent is benzotriazole.
Adding methyl iodide, TPM-1 and a reaction solvent NMP in a molar ratio of 1:1 into a reaction kettle for reaction, and reacting at 80 ℃ for 6 hours to obtain TPM-2; after cooling to room temperature, TPM-2, brightening agent, inhibitor and leveling agent are compounded in the weight ratio of 0.2ppm to 10ppm to 3ppm to 0.6ppm and deionized water to obtain the new additive.
And mixing the compounded novel additive with the acid copper sulfate main electrolyte prepared by dissolving copper to obtain the green foil electrolyte. The raw foil electrolyte is pumped into an electrolytic tank through a heat exchanger to 50 ℃, the cathode of the electrolytic tank is a titanium roller treated by a shielding layer, the anode is an anode plate with size limitation, and the anode plate is at 7000A/m 2 Electroplating green foil is performed at a current density of (2).
Example 2
In this example, the brightening agent is sodium 3-mercapto-1-propanesulfonate (MPS), the inhibitor is polyethylene glycol (PEG), and the leveler is benzotriazole.
Adding methyl iodide, TPM-1 and a reaction solvent NMP in a molar ratio of 1:1 into a reaction kettle for reaction, and obtaining TPM-2 after reaction for 4 hours at 90 ℃; after cooling to room temperature, TPM-2, brightening agent, inhibitor, leveling agent and deionized water are compounded according to the mass percentage of 0.5ppm to 12ppm to 6ppm to 0.4ppm, and the balance is deionized water to obtain the novel additive.
And mixing the compounded novel additive with the acid copper sulfate main electrolyte prepared by dissolving copper to obtain the green foil electrolyte. The raw foil electrolyte is pumped into an electrolytic tank through a heat exchanger to 60 ℃, the cathode of the electrolytic tank is a titanium roller treated by a shielding layer, the anode is an anode plate with size limitation, and the anode plate is at 7000A/m 2 Electroplating green foil is performed at a current density of (2).
Example 3
In this example, the brightening agent is thiourea, the inhibitor is polyethylene glycol (PEG), and the leveling agent is benzotriazole.
Adding a reaction kettle with the molar ratio of 1:1, methyl iodide, TPM-1 and a reaction solvent NMP are reacted, and TPM-2 is obtained after the reaction is carried out for 5 hours at 85 ℃; after cooling to room temperature, TPM-2, brightening agent, inhibitor and leveling agent are compounded in the weight ratio of 0.3ppm to 11ppm to 5ppm to 0.6ppm and deionized water to obtain the new additive.
And mixing the compounded novel additive with the acid copper sulfate main electrolyte prepared by dissolving copper to obtain the green foil electrolyte. The raw foil electrolyte is pumped into an electrolytic tank through a heat exchanger to 70 ℃, the cathode of the electrolytic tank is a titanium roller treated by a shielding layer, the anode is an anode plate with size limitation, and the anode plate is at 7000A/m 2 Electroplating green foil is performed at a current density of (2).
Example 4
In this example, the brightening agent is a mixture of sodium polydithio-dipropyl sulfonate (SPS) and sodium 3-mercapto-1-propane sulfonate (MPS), the inhibitor is polyethylene glycol (PEG), and the leveling agent is benzotriazole.
Adding methyl iodide, TPM-1 and a reaction solvent NMP in a molar ratio of 1:1 into a reaction kettle for reaction, and reacting for 5 hours at 85 ℃ to obtain TPM-2; after cooling to room temperature, TPM-2, brightening agent, inhibitor, leveling agent and water are compounded according to the mass percentage of 1.2ppm to 16ppm to 2ppm to 0.4ppm, and the rest is deionized water to obtain the novel additive.
And mixing the compounded novel additive with the acid copper sulfate main electrolyte prepared by dissolving copper to obtain the green foil electrolyte. The raw foil electrolyte is pumped into an electrolytic tank through a heat exchanger to 60 ℃, the cathode of the electrolytic tank is a titanium roller treated by a shielding layer, the anode is an anode plate with size limitation, and the anode plate is at 7000A/m 2 Electroplating green foil is performed at a current density of (2).
Example 5
In this example, the brightening agent is a mixture of sodium polydithio-dipropyl sulfonate (SPS) and thiourea, the inhibitor is polyethylene glycol (PEG), and the leveler is benzotriazole.
Adding methyl iodide, TPM-1 and a reaction solvent NMP in a molar ratio of 1:1 into a reaction kettle for reaction, and reacting for 5 hours at 85 ℃ to obtain TPM-2; after cooling to room temperature, TPM-2, brightening agent, inhibitor, leveling agent and water are compounded according to the mass percentage of 1.6ppm to 14ppm to 2ppm to 0.3ppm, and the rest is deionized water to obtain the novel additive.
And mixing the compounded novel additive with the acid copper sulfate main electrolyte prepared by dissolving copper to obtain the green foil electrolyte. The raw foil electrolyte is pumped into an electrolytic tank through a heat exchanger to 60 ℃, the cathode of the electrolytic tank is a titanium roller treated by a shielding layer, the anode is an anode plate with size limitation, and the anode plate is at 7000A/m 2 Electroplating green foil is performed at a current density of (2).
Example 6
In this example, the brightening agent is a mixture of sodium 3-mercapto-1-propanesulfonate (MPS) and thiourea, the inhibitor is polyethylene glycol (PEG), and the leveler is benzotriazole.
Adding methyl iodide, TPM-1 and a reaction solvent NMP in a molar ratio of 1:1 into a reaction kettle for reaction, and reacting at 80 ℃ for 6 hours to obtain TPM-2; after cooling to room temperature, TPM-2, brightening agent, inhibitor and leveling agent are compounded to obtain the new additive in the weight ratio of 0.8ppm to 7ppm to 6.2ppm to 0.2ppm and deionized water.
And mixing the compounded novel additive with the acid copper sulfate main electrolyte prepared by dissolving copper to obtain the green foil electrolyte. The raw foil electrolyte is pumped into an electrolytic tank through a heat exchanger to 60 ℃, the cathode of the electrolytic tank is a titanium roller treated by a shielding layer, the anode is an anode plate with size limitation, and the anode plate is at 7000A/m 2 Electroplating green foil is performed at a current density of (2).
Example 7
In this example, the brightening agent is sodium 3-mercapto-1-propanesulfonate (MPS), the inhibitor is polyethylene glycol (PEG), and the leveler is benzotriazole.
Adding methyl iodide, TPM-1 and a reaction solvent NMP in a molar ratio of 1:1 into a reaction kettle for reaction, and reacting at 80 ℃ for 6 hours to obtain TPM-2; after cooling to room temperature, TPM-2, brightening agent, inhibitor and leveling agent are compounded to obtain the new additive in the weight ratio of 1.1ppm to 5ppm to 8.6ppm to 0.8ppm and deionized water.
And mixing the compounded novel additive with the acid copper sulfate main electrolyte prepared by dissolving copper to obtain the green foil electrolyte. The raw foil electrolyte is pumped into an electrolytic tank through a heat exchanger to 60 ℃, the cathode of the electrolytic tank is a titanium roller treated by a shielding layer, the anode is an anode plate with size limitation, and the anode plate is at 7000A/m 2 Electroplating green foil is performed at a current density of (2).
The basic physical properties of the electrodeposited copper foil of examples 1-7 are shown in Table 1:
TABLE 1 basic physical Property results of electrolytic copper foil
As shown in Table 1, the present invention was carried out at a temperature of 50 to 70℃and 7000A/m 2 The electrolytic copper foil prepared under the current density operation condition has good physical properties, and meanwhile, the shielding edge part of the cathode roller has no higher copper junction rate, which proves that the mutual synergistic effect of TPM-1 and I-can effectively inhibit the copper junction problem of the shielding layer edge part to a certain extent.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (7)
1. The additive is characterized by comprising 5-16 ppm, 2-9 ppm, 0.1-3 ppm, 0.2-2 ppm and deionized water in percentage by mass.
2. The additive for inhibiting variable width edge copper binding according to claim 1, wherein the brightening agent is one or a mixture of several of sodium polydithio-dipropyl sulfonate, sodium 3-mercapto-1-propane sulfonate and thiourea according to any ratio.
3. A variable width edge copper bonding inhibitor additive according to claim 1, wherein the inhibitor is polyethylene glycol.
4. A variable width edge copper bonding inhibitor additive according to claim 1 wherein the leveler is benzotriazole.
5. The additive for inhibiting variable width edge copper bonding according to claim 1, wherein the preparation method of the TPM-2 is as follows:
and mixing methyl iodide, TPM-1 and a reaction solvent NMP, and reacting for 4-6 hours at 80-90 ℃ to obtain TPM-2.
6. A variable width edge copper bonding inhibitor additive according to claim 5, wherein the molar ratio of methyl iodide to TPM-1 is 1:1.
7. A method of preparing a variable width edge junction copper additive according to any one of claims 1 to 6, comprising the steps of:
step 1, mixing methyl iodide, TPM-1 and a reaction solvent NMP, and reacting for 4-6 hours at 80-90 ℃ to obtain TPM-2;
and 2, after cooling to room temperature, compounding TPM-2, brightening agent, inhibitor, leveling agent and deionized water according to a proportion to obtain the additive.
Priority Applications (1)
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CN202310860711.5A CN116905052A (en) | 2023-07-14 | 2023-07-14 | Additive for inhibiting variable-amplitude wide-edge copper junction and preparation method thereof |
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CN202310860711.5A CN116905052A (en) | 2023-07-14 | 2023-07-14 | Additive for inhibiting variable-amplitude wide-edge copper junction and preparation method thereof |
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