CN113430521A - Environment-friendly acidic etching additive suitable for thin line manufacturing and application thereof - Google Patents
Environment-friendly acidic etching additive suitable for thin line manufacturing and application thereof Download PDFInfo
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- CN113430521A CN113430521A CN202110991679.5A CN202110991679A CN113430521A CN 113430521 A CN113430521 A CN 113430521A CN 202110991679 A CN202110991679 A CN 202110991679A CN 113430521 A CN113430521 A CN 113430521A
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- bank protection
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/18—Acidic compositions for etching copper or alloys thereof
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
- H05K3/06—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding the conductive material being removed chemically or electrolytically, e.g. by photo-etch process
- H05K3/067—Etchants
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- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- ing And Chemical Polishing (AREA)
Abstract
The invention provides an environment-friendly acidic etching additive suitable for fine line manufacturing, which consists of a bank protection agent, a wetting agent and water, wherein the wetting agent is one or more of saturated aliphatic diol, saturated aliphatic triol, glycolic acid and carboxylic acid, and the component concentration of the wetting agent is 100-3000 ppm; the bank protection agent is a structural formula component
One or more of them, the component concentration is 5-200 ppm; wherein A is a carbon atom or a nitrogen atom, R1Is one of H, C1-4 alkyl, phenyl, 4-halogen substituted phenyl, 2-pyrrolyl, 3-pyrrolyl, imidazolyl, pyridyl and pyrazinyl, R2Is H, C1-6 alkyl, phenyl, 4-halogen substituted phenyl, 2-pyrrolyl, 3-pyrrolyl, imidazolyl, pyridyl or pyrazinylOne of (1) and (b). The bank protection agent can be properly adsorbed on the copper surface in the etching liquid spraying process, so that the side wall of the circuit is effectively protected, and the side corrosion is reduced; the wetting agent allows the etching solution to sufficiently react with copper by increasing the hydrophilicity of the copper surface sites.
Description
Technical Field
The invention relates to the technical field of etching reagents, in particular to an environment-friendly acidic etching additive suitable for manufacturing a fine line and application thereof.
Background
With the continuous update of integrated circuit and electronic packaging technologies, circuit board technologies are developing towards high-density and fine-line circuits. The high-density circuit board can provide a substrate for fine line, small hole and high-density surface packaging, can meet the requirements of miniaturization, multifunctionality, high speed and high I/O number of electronic products, and can be matched with electronic packaging technologies such as Flip Chip, BGA, CSP, MCM and the like, so that the application level of the high-density circuit board is wider. At present, the ultra-fine circuit manufacturing process in the field of circuit board manufacturing has been developed to a line width and line distance below 40 [ mu ] m/40 [ mu ] m, so that the use of etching liquid is more important to the etching quality. At present, two reliable ultra-fine line manufacturing processes are available: one is a flash etching process, which is a fine circuit manufacturing technology based on a sulfuric acid-hydrogen peroxide system, but because the cost of materials and equipment used by the process is high, and the difficulty of technical management and control of pattern transfer, electroplating quality, dust-free level of environment and the like is high, a lot of circuit board manufacturers are prohibited; in another process, an acidic etching additive is added to the acidic etching solution to improve the etching quality. The existing basic acidic etching solution is matched with a vacuum etching line, and a circuit with the line width/line distance of 40 mu m/40 mu m can be processed reluctantly under the condition that the thickness of a copper foil is not more than 20 mu m, wherein the etching factor is generally 2-3. Once the thickness of the copper foil is larger than 12 mu m or the processing of a fine circuit (the line width/line distance is not more than 35 mu m/35 mu m) is finished, the current acidic etching solution matched with a vacuum etching line cannot meet the requirement.
As acidic etching additives, additives of ammonia nitrogen systems are often used in the prior art. In order to further improve the etching effect of the ammonia nitrogen system, an additive is added into the additive: for example, a hydrochloride such as sodium chloride, potassium chloride or ammonium chloride is added as an auxiliary, or ammonium persulfate, ammonium sulfate, ammonium nitrate, sulfamic acid or ammonium hydrogen carbonate is added as an auxiliary. The addition of the auxiliary substances can cause the indexes of waste liquid, particularly high ammonia nitrogen, to be higher, and cannot meet the current increasingly strict wastewater discharge standard. In addition, such acidic etching additives, when used, have low etching rates.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: an etching additive is designed to achieve the effects of improving the quality of ultra-fine line manufacturing, reducing the technical control difficulty and reducing the wastewater treatment difficulty.
In order to solve the technical problems, the invention adopts the technical scheme that:
an environment-friendly acidic etching additive suitable for fine line manufacture comprises a bank protection agent, a wetting agent and water, wherein the wetting agent is one or more of saturated aliphatic diol, saturated aliphatic triol, glycolic acid and carboxylic acid, and the component concentration of the wetting agent is 100-3000 ppm; the bank protection agent is a structural formula component
One or more of them, the component concentration is 5-200 ppm; wherein A is a carbon atom or a nitrogen atom, R1Is one of H, C1-4 alkyl, phenyl, 4-halogen substituted phenyl, 2-pyrrolyl, 3-pyrrolyl, imidazolyl, pyridyl and pyrazinyl, R2Is one of H, C1-C6 alkyl, phenyl, 4-halogen substituted phenyl, 2-pyrrolyl, 3-pyrrolyl, imidazolyl, pyridyl and pyrazinyl; the acidic etching additive is suitable for finished fine lines with line width of less than 40 mu m and line distance of less than 40 mu m.
Further, the component concentration of the bank protection agent is 10-100 ppm.
Further, the component concentration of the bank protection agent is 20-50 ppm.
Further, the component concentration of the wetting agent is 200-1500 ppm.
Further, the component concentration of the wetting agent is 400-800 ppm.
Further, the halogen is chlorine or bromine; the humectant has carbon atom number of 2-4 and molecular weight of 100 or less.
The application of the environment-friendly acidic etching additive suitable for fine line manufacturing is applied to a hydrochloric acid-copper chloride etching system; the oxidant matched with the hydrochloric acid-copper chloride etching system is sodium chlorate; the component concentration of the sodium chlorate is 200-300g/L, the component concentration of the hydrochloric acid is 1-3mol/L, and the component concentration of the copper chloride is 240-300 g/L.
Furthermore, the linear velocity is controlled at 3.5-4m/min during etching.
Further, the sodium chlorate was placed in a secondary tank.
The invention has the beneficial effects that: the bank protection agent is a core component, can be properly adsorbed on a copper surface in an acid etching system, effectively protects the side wall of a circuit in the process of spraying the etching solution and reduces side etching; the wetting agent has the effect of wetting the copper surface, and the etching solution can fully react with the copper by increasing the hydrophilicity of the position of the copper surface (especially the bottom of the circuit), thereby improving the wettability of the etching solution and the exchange of divalent copper ions.
Principle explanation:
1. the working principle of the bank protection agent is as follows: the complex is adhered to the surface of copper by forming a complex with copper ions, so that the bottom copper between the lines is directly opposite to liquid jet flow in a horizontal spraying device, the complex protective film is easy to break so as to dissolve the bottom copper by an etching solution, and the complex protective film on the side wall of the line is less disturbed by the fluid so as to protect the copper on the side wall from being corroded.
2. The system adopts the micromolecular wetting agent, and compared with a macromolecular wetting agent (the macromolecular wetting agent refers to 200-20000-type polyethylene glycol, polyvinyl ether and polyoxyethylene ether), the micromolecular wetting agent has the obvious advantages of fast diffusion, good wettability, no interference on degradation products and the like.
Detailed Description
Example 1
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is benzimidazole, and the component concentration of the bank protection agent is 5 ppm; the wetting agent is ethylene glycol, and the component concentration is 800 ppm.
Example 2
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is benzimidazole, and the component concentration of the bank protection agent is 50 ppm; the humectant is glycerin with a component concentration of 1500 ppm.
Example 3
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2-methylbenzimidazole, and the component concentration of the bank protection agent is 10 ppm; the wetting agent was ethylene glycol, and the component concentration was 1500 ppm.
Example 4
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2-methylbenzimidazole, and the component concentration of the bank protection agent is 100 ppm; the humectant is glycolic acid with a component concentration of 200 ppm.
Example 5
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2-butyl benzimidazole, and the component concentration of the bank protection agent is 50 ppm; the wetting agent was ethylene glycol, and the component concentration was 1500 ppm.
Example 6
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2-butyl benzimidazole, and the component concentration of the bank protection agent is 100 ppm; the humectant is glycolic acid with a component concentration of 200 ppm.
Example 7
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2-phenylbenzimidazole, and the component concentration of the bank protection agent is 50 ppm; the wetting agent was ethylene glycol, and the component concentration was 1500 ppm.
Example 8
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2-phenylbenzimidazole, and the component concentration of the bank protection agent is 200 ppm; the humectant is lactic acid, and the component concentration is 100 ppm.
Example 9
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2- (4-chlorphenyl) benzimidazole, and the component concentration is 100 ppm; the humectant is glycerin, and its component concentration is 2000 ppm.
Example 10
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2- (4-chlorphenyl) benzimidazole, and the component concentration is 200 ppm; the humectant is lactic acid, and the component concentration is 100 ppm.
Example 11
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 1H-imidazo [4,5-b ] pyrazine, and the component concentration is 5 ppm; the wetting agent is ethylene glycol, and the component concentration is 800 ppm.
Example 12
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 1H-imidazo [4,5-b ] pyrazine, and the component concentration is 50 ppm; the humectant is glycerin with a component concentration of 1500 ppm.
Example 13
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2-methyl-1H-imidazo [4,5-b ] pyrazine, and the component concentration is 5 ppm; the wetting agent was ethylene glycol, and the component concentration was 1500 ppm.
Example 14
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2-methyl-1H-imidazo [4,5-b ] pyrazine, and the component concentration is 10 ppm; the humectant is glycolic acid with a component concentration of 200 ppm.
Example 15
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2-phenyl-1H-imidazo [4,5-b ] pyrazine, and the component concentration is 20 ppm; the wetting agent was ethylene glycol, and the component concentration was 1500 ppm.
Example 16
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2-phenyl-1H-imidazo [4,5-b ] pyrazine, and the component concentration is 100 ppm; the humectant is glycolic acid with a component concentration of 200 ppm.
Example 17
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2- (4-chlorphenyl) -1H-imidazo [4,5-b ] pyrazine, and the component concentration is 50 ppm; the wetting agent was ethylene glycol, and the component concentration was 1500 ppm.
Example 18
An environment-friendly acid etching additive suitable for manufacturing fine lines, which consists of a bank protection agent, a wetting agent and water; the bank protection agent is 2- (4-chlorphenyl) -1H-imidazo [4,5-b ] pyrazine, and the component concentration is 50 ppm; the humectant is lactic acid, and the component concentration is 100 ppm.
Comparative example 1: proportion of empty ginseng and white ginseng
A hydrochloric acid-copper chloride etching system; the oxidant matched with the hydrochloric acid-copper chloride etching system is sodium chlorate; the component concentration of the sodium chlorate is 200-300g/L, the component concentration of the hydrochloric acid is 1-3mol/L, and the component concentration of the copper chloride is 240-300 g/L. The sodium chlorate is used in a secondary tank.
Comparative example 2
On the basis of comparative example 1, 50ppm of 1H-imidazo [4,5-b ] pyrazine as a bank protection agent was added.
Comparative example 3
On the basis of comparative example 1, 200ppm of glycolic acid as a wetting agent was added.
TABLE 1 results of the influence of additives of different compositions on the etching factor
Note: 42 [ mu ] m/28 [ mu ] m/18 [ mu ] m represents that the line width before etching is 42 [ mu ] m, the line distance is 28 [ mu ] m, the line height is 18 [ mu ] m, and the rest is analogized.
Respectively adding the additives of examples 1 to 18 into the etching system of comparative example 1, and then respectively etching the circuit board with the line width/line spacing/copper thickness of 42 mu m/28 mu m/18 mu m or 36 mu m/24 mu m/18 mu m or 32 mu m/18 mu m/12 mu m under the condition that the online speed is controlled to be 3.5-4 m/min. Meanwhile, the system of comparative examples 1-3 is adopted, and the lines with the line width/line spacing/copper thickness of 42 [ mu ] m/28 [ mu ] m/18 [ mu ] m or 36 [ mu ] m/24 [ mu ] m/18 [ mu ] m or 32 [ mu ] m/18 [ mu ] m/12 [ mu ] m are also etched respectively under the condition that the online speed is controlled to be 3.5-4 m/min. After the etching was completed, the etching factors were calculated based on the blank reference ratio, and the calculation results are detailed in table 1.
As can be seen from Table 1, the additive system provides about 40% to 90% improvement in etching factor: for the value of 42 mu m/28 mu m/18 mu m before etching (the line width/line distance after etching is about 35 mu m/35 mu m), the etching factor is averagely increased by 89% through the addition of additives; for the condition that the etching factor is 36 mu m/24 mu m/18 mu m before etching (the line width/line distance after etching is about 25 mu m/25 mu m), the etching factor is averagely increased by 89% through the addition of additives; for the value of 42 mu m/28 mu m/18 mu m before etching (the line width/line distance after etching is about 35 mu m/35 mu m), the etching factor is averagely improved by 59 percent through the addition of the additive; the etching factor is 32 mu m/18 mu m/12 mu m before etching (the line width/line distance after etching is about 20 mu m/20 mu m), and the etching factor is averagely increased by 41% through the addition of additives. The additive system greatly improves the etching factors of the circuits with three groups of sizes, and the improvement effect of the circuits with larger sizes is particularly obvious. Through analysis of the three groups of comparative examples, the bank protection agent has a certain effect of improving the etching factor, but for fine lines, a wetting agent is still needed to assist the bank protection agent to infiltrate the part to be etched between the lines as soon as possible to achieve the bank protection effect, and the more fine the lines, the more important the assistance requirement is.
In conclusion, when the additive is added into a hydrochloric acid-copper chloride etching system, the etching factor can be improved, and the waste water after etching is low in ammonia nitrogen content and easy to treat; the etched circuit has good quality, the requirement on etching conditions is low, and the circuit with the thickness not more than 18 mu m and the fine circuit with the line width/line distance not more than 40 mu m/40 mu m can be processed.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (9)
1. An environment-friendly acidic etching additive suitable for manufacturing fine lines is characterized by comprising a bank protection agent, a wetting agent and water, wherein the wetting agent is one or more of saturated aliphatic diol, saturated aliphatic triol, glycolic acid and carboxylic acid, and the component concentration of the wetting agent is 100-3000 ppm; the bank protection agent is a structural formula component
One or more of them, the component concentration is 5-200 ppm; wherein A is a carbon atom or a nitrogen atom, R1Is one of H, C1-4 alkyl, phenyl, 4-halogen substituted phenyl, 2-pyrrolyl, 3-pyrrolyl, imidazolyl, pyridyl and pyrazinyl, R2Is one of H, C1-C6 alkyl, phenyl, 4-halogen substituted phenyl, 2-pyrrolyl, 3-pyrrolyl, imidazolyl, pyridyl and pyrazinyl; the acidic etching additive is suitable for finished fine lines with line width of less than 40 mu m and line distance of less than 40 mu m.
2. The environmentally friendly acidic etching additive suitable for fine line fabrication as claimed in claim 1 wherein the component concentration of the bank protecting agent is 10-100 ppm.
3. The environmentally friendly acidic etching additive suitable for fine line fabrication as claimed in claim 2 wherein the component concentration of the bank protecting agent is 20-50 ppm.
4. The environmentally friendly acidic etching additive suitable for fine line fabrication as claimed in claim 1, wherein the wetting agent has a component concentration of 200-1500 ppm.
5. The environmentally friendly acidic etching additive suitable for fine line fabrication as claimed in claim 4, wherein the wetting agent has a component concentration of 400-800 ppm.
6. The environmentally friendly acidic etching additive suitable for fine line fabrication as claimed in any one of claims 1 to 5, wherein the halogen is chlorine or bromine; the humectant has carbon atom number of 2-4 and molecular weight of 100 or less.
7. The use of the environmentally friendly acidic etching additive suitable for fine line fabrication according to any one of claims 1 to 6 in a hydrochloric acid-copper chloride etching system; the oxidant matched with the hydrochloric acid-copper chloride etching system is sodium chlorate; the component concentration of the sodium chlorate is 200-300g/L, the component concentration of the hydrochloric acid is 1-3mol/L, and the component concentration of the copper chloride is 240-300 g/L.
8. The environment-friendly acidic etching additive suitable for fine line manufacture as claimed in claim 7, wherein the linear velocity is controlled to 3.5-4m/min during etching.
9. The environmentally friendly acidic etching additive suitable for fine line fabrication of claim 8 wherein the sodium chlorate is disposed in the secondary tank.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110991679.5A CN113430521A (en) | 2021-08-27 | 2021-08-27 | Environment-friendly acidic etching additive suitable for thin line manufacturing and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110991679.5A CN113430521A (en) | 2021-08-27 | 2021-08-27 | Environment-friendly acidic etching additive suitable for thin line manufacturing and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115074735A (en) * | 2022-08-04 | 2022-09-20 | 温州珑泰深拓新材料有限公司 | Novel nitrogen-free fluorine-free environment-friendly tin stripping liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103114288A (en) * | 2011-11-14 | 2013-05-22 | Mec股份有限公司 | Etching solution, supplying solution and method of forming copper wiring |
| CN103952702A (en) * | 2014-05-04 | 2014-07-30 | 深圳市实锐泰科技有限公司 | Etching liquid and method for etching fine lines of flexible circuit board by using same |
| CN104762620A (en) * | 2014-06-13 | 2015-07-08 | 叶涛 | High-efficient high-quality acidic copper chloride circuit board etching solution |
| US20180105702A1 (en) * | 2015-03-31 | 2018-04-19 | Commonwealth Scientific And Industrial Research Organisation | Composition for inhibiting corrosion |
-
2021
- 2021-08-27 CN CN202110991679.5A patent/CN113430521A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103114288A (en) * | 2011-11-14 | 2013-05-22 | Mec股份有限公司 | Etching solution, supplying solution and method of forming copper wiring |
| CN103952702A (en) * | 2014-05-04 | 2014-07-30 | 深圳市实锐泰科技有限公司 | Etching liquid and method for etching fine lines of flexible circuit board by using same |
| CN104762620A (en) * | 2014-06-13 | 2015-07-08 | 叶涛 | High-efficient high-quality acidic copper chloride circuit board etching solution |
| US20180105702A1 (en) * | 2015-03-31 | 2018-04-19 | Commonwealth Scientific And Industrial Research Organisation | Composition for inhibiting corrosion |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115074735A (en) * | 2022-08-04 | 2022-09-20 | 温州珑泰深拓新材料有限公司 | Novel nitrogen-free fluorine-free environment-friendly tin stripping liquid |
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