CN115433940B - Copper etching solution and preparation method and application thereof - Google Patents

Copper etching solution and preparation method and application thereof Download PDF

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Publication number
CN115433940B
CN115433940B CN202211073590.1A CN202211073590A CN115433940B CN 115433940 B CN115433940 B CN 115433940B CN 202211073590 A CN202211073590 A CN 202211073590A CN 115433940 B CN115433940 B CN 115433940B
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copper
acid
etching solution
etching
surfactant
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CN115433940A (en
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赵方方
李泰亨
王丹宇
白晓鹏
王泽�
陈红波
董童威
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Yi'an Aifu Wuhan Technology Co ltd
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Yi'an Aifu Wuhan Technology Co ltd
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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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • ing And Chemical Polishing (AREA)

Abstract

The application provides a copper etching solution, a preparation method and application thereof, wherein the copper etching solution comprises phosphoric acid, strong oxidizing acid, an inhibitor, a surfactant, a dispersing agent and deionized water; the dispersing agent is one or more of naphthalene sulfonate, lignin sulfonate, sodium humate and polycarboxylate. The copper etching liquid disclosed by the application is stable in liquid property, can effectively disperse particles, inhibit agglomeration of organic matters and copper ions, enables the surface of a substrate to be clean and pollution-free, and can ensure that the copper etching liquid has a smaller etching taper angle and a smaller CDloss variation.

Description

Copper etching solution and preparation method and application thereof
Technical Field
The application relates to the technical field of etching solutions, in particular to a copper etching solution, a preparation method and application thereof.
Background
Copper metal has good conductivity and is therefore widely used for wiring, where the etching of the wiring often etches a specialty chemical with a wet process to etch away the metal not protected by the photoresist to form the wiring. At present, the copper etching solution in the market is mainly hydrogen peroxide copper etching solution (such as CN 104498951B), and the hydrogen peroxide is easy to decompose due to heating, so that the etching is unstable; and along with the extension of etching time, the increase of copper ion content in the liquid medicine can promote the decomposition of hydrogen peroxide, thereby shortening the etching life of the liquid medicine, and in addition, the decomposition and heat release of hydrogen peroxide are easy to induce potential safety hazards. To ensure good etching performance of the copper etchant, some surfactants are usually added to the copper etchant to maintain the surface tension and wetting effect of the metal surface, but most surfactants often exhibit different shapes of aggregate morphology such as micelle, bilayer film or liquid crystal morphology in organic solvents or aqueous solutions, and these aggregate morphology may cause substrate contamination and etching instability. Therefore, a non-hydrogen peroxide copper etching solution with good dispersibility and stable performance is needed.
Disclosure of Invention
In view of the above, the application provides a non-hydrogen peroxide copper etching solution with good dispersibility and stable performance, and a preparation method and application thereof.
The technical scheme of the application is realized as follows:
in a first aspect, the present application provides a copper etchant comprising phosphoric acid, a strong oxidizing acid, an inhibitor, a surfactant, a dispersant, and deionized water; the dispersing agent is one or more of naphthalene sulfonate, lignin sulfonate, sodium humate and polycarboxylate.
On the basis of the technical scheme, preferably, the etching solution comprises, by mass, 100% of phosphoric acid, 1-10% of strong oxidizing acid, 0.05-1% of inhibitor, 0.01-1% of surfactant, 0.01-1% of dispersing agent and the balance of deionized water.
On the basis of the technical scheme, preferably, the naphthalene sulfonate is one or a combination of more of sodium methylene dinaphthyl sulfonate, methyl naphthalene sulfonate formaldehyde condensate and benzyl naphthalene sulfonate formaldehyde condensate; the lignosulfonate is one or a combination of more of sodium lignosulfonate, potassium lignosulfonate and calcium lignosulfonate; the polycarboxylate is one or more of TERSPERSE 2700, SD-819, GY-D1252 and SD-661.
On the basis of the technical scheme, the method preferably further comprises a biological flocculant, wherein the biological flocculant is one or a combination of more than one of polyamino acid, glucan, mannan, glycoprotein and N-acetylglucosamine.
Based on the above technical solution, preferably, the polyamino acid is one or more of polyglutamic acid, polyalanine and polyaspartic acid.
On the basis of the technical scheme, preferably, the etching solution comprises, by mass, 100% of phosphoric acid, 4-8% of strong oxidizing acid, 0.2-0.4% of inhibitor, 0.2-0.4% of surfactant, 0.3-0.4% of dispersing agent, 0.5-0.9% of biological flocculant and the balance of deionized water.
On the basis of the technical scheme, preferably, the strong oxidizing acid is one or a combination of more of sulfuric acid, hydrochloric acid, perchloric acid and nitric acid.
On the basis of the technical scheme, preferably, the inhibitor is one or a combination of more of 5-methyltetrazole, 5-aminotetrazole, benzotriazole and imidazole.
On the basis of the technical scheme, preferably, the surfactant is an alcohol nonionic surfactant.
Based on the above technical scheme, preferably, the surfactant is one or more of isopropanol, 2-phenoxyethanol, acetylenic diol and polyethylene glycol.
In a second aspect, the application provides a method for preparing a copper etching solution, comprising the following steps: adding phosphoric acid, strong oxidizing acid and deionized water into a container, and stirring at 25 deg.C and 600-800rpm for 10-20min; then adding inhibitor, surfactant, dispersant and bioflocculant, stirring at 25 deg.C and 800-1000rpm for 10-30min.
In a third aspect, the present application provides a use of a copper etchant for selectively etching metallic copper on a copper substrate at 32 ℃.
Compared with the prior art, the copper etching solution and the preparation method and application thereof have the following beneficial effects:
(1) In the copper etching solution, metallic copper is oxidized into copper ions under the action of phosphoric acid and strong oxidizing acid; the inhibitor is adsorbed on the copper surface, so that the side etching amount is reduced, and excessive etching of etching liquid is prevented; the surfactant enables the etching solution to fully contact with the copper surface, so that the etching rate is improved; the inhibitor and the surfactant act synergistically to maintain the etching taper angle; the dispersing agent can effectively disperse particles, inhibit agglomeration, ensure good etching performance and clean and pollution-free substrate.
(2) In the copper etching solution, the bioflocculant can effectively adsorb excessive copper ions, maintain the stability of the liquid medicine, maintain a smaller etching taper angle and keep the surface of the substrate free from residues.
(3) The etching liquid can ensure that the etching liquid has smaller etching taper angle and smaller CD loss variation, and the surface of the substrate has no residue.
Drawings
In order to more clearly illustrate the embodiments of the application or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the comparison of etching performance of a copper etchant of the present application;
FIG. 2 is a graph showing polymer deposition contrast of the etching solution of the present application.
Detailed Description
The following description of the embodiments of the present application will clearly and fully describe the technical aspects of the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present application without making any inventive effort, are intended to fall within the scope of the present application.
The reagents used in the present application are all commercially available, and the present application will be further described in detail by means of the following specific examples, which are only illustrative of the present application and should not be construed as limiting the present application.
Example 1
The copper etching solution of the embodiment comprises 10% of phosphoric acid, 1% of sulfuric acid, 0.05% of 5-methyltetrazole, 0.01% of isopropanol, 0.01% of sodium methylenedinaphthyl sulfonate and the balance of deionized water according to the mass percentage of 100%.
The preparation method of the copper etching solution comprises the following steps: adding phosphoric acid, sulfuric acid and deionized water into a container, and stirring at 25deg.C and 600rpm for 10min; then adding 5-methyltetrazole, isopropanol and sodium methylene dinaphthyl sulfonate, and stirring at 25 ℃ and 800rpm for 10 min.
Example 2
The copper etching solution of the embodiment comprises, by mass, 100% of phosphoric acid, 4% of hydrochloric acid, 0.2% of 5-aminotetrazole, 0.2% of 2-phenoxyethanol, 0.2% of sodium lignin sulfonate, 0.3% of polyalanine, 0.2% of mannan, and the balance of deionized water.
The preparation method of the copper etching solution comprises the following steps: adding phosphoric acid, hydrochloric acid and deionized water into a container, and stirring at 25deg.C and 700rpm for 15min; then adding 5-aminotetrazole, 2-phenoxyethanol, sodium lignin sulfonate, polyalanine and mannans, and stirring at 25 ℃ and 900rpm for 20min.
Example 3
The copper etching solution of the embodiment comprises, by mass, 100% of phosphoric acid, 6% of perchloric acid, 0.4% of benzotriazole, 0.3% of acetylenic diol, 0.2% of sodium methylenedinaphthyl sulfonate, 0.1% of sodium humate, 0.4% of mannan, 0.2% of glucan and the balance of deionized water.
The preparation method of the copper etching solution comprises the following steps: adding phosphoric acid, perchloric acid and deionized water into a container, and stirring at 25 ℃ and 700rpm for 15min; then adding benzotriazole, acetylenic diol, sodium methylene dinaphthyl sulfonate, sodium humate, mannans and dextran, and stirring at 25 ℃ and 900rpm for 20min.
Example 4
The copper etching solution of this example comprises, by mass, 100% of phosphoric acid, 8% of nitric acid, 0.2% of 5-methyltetrazole, 0.2% of imidazole, 0.2% of 2-phenoxyethanol, 0.2% of propargyl alcohol, 0.3% of potassium lignin sulfonate, 0.1% of TERSPERSE 2700, 0.9% of N-acetylglucosamine, and the balance of deionized water.
The preparation method of the copper etching solution comprises the following steps: adding phosphoric acid, nitric acid and deionized water into a container, and stirring at 25deg.C and 800rpm for 20min; then 5-methyltetrazole, imidazole, 2-phenoxyethanol, propargyl alcohol, potassium lignin sulfonate, TERSPERSE 2700 and N-acetylglucosamine were added and stirred at 1000rpm at 25℃for 30min.
Example 5
The copper etching solution of the embodiment comprises, by mass, 100% of phosphoric acid, 10% of sulfuric acid, 0.6% of 5-methyltetrazole, 0.4% of benzotriazole, 0.4% of 2-phenoxyethanol, 0.6% of polyethylene glycol, 0.8% of methylnaphthalene sulfonate formaldehyde condensate, 0.2% of GYD-1252,0.5% of polyglutamic acid, 0.4% of mannans and the balance of deionized water.
The preparation method of the copper etching solution comprises the following steps: adding phosphoric acid, sulfuric acid and deionized water into a container, and stirring at 25deg.C and 800rpm for 20min; then 5-methyltetrazole, benzotriazole, 2-phenoxyethanol, polyethylene glycol, methylnaphthalene sulfonate formaldehyde condensate, GYD-1252, polyglutamic acid and mannan were added and stirred at 25℃and 1000rpm for 30min.
Comparative example 1
The copper etchant composition of comparative example 1 was substantially the same as the preparation method as in example 1, except that the copper etchant composition of comparative example 1 lacks a dispersant.
Comparative example 2
The copper etchant composition of comparative example 2 was substantially the same as the preparation method as in example 1, except that the copper etchant composition of comparative example 1 lacks a dispersant and an inhibitor.
Comparative example 3
The copper etchant composition of comparative example 3 was substantially the same as the preparation method as in example 1, except that the copper etchant composition of comparative example 1 lacks a surfactant and a dispersant.
The etching methods of examples and comparative examples were: the copper etchant selectively etches metallic copper on the copper substrate at 32 ℃.
1. Etching performance
Copper substrates were etched at 32 ℃ using an etcher to a uniform over-etch of 100% oe, and cross-sectional views of the substrates were taken by SEM using a scanning electron microscope, and the substrate etch taper angle, CD loss, and residue were observed, and the results are shown in table 1 and fig. 1.
Table 1 etching performance of the example and comparative example etchant
Etching performance Cone angle/° CDLoss/μm Residue of SEM image
Example 1 53 1.18 Without any means for 1-A
Example 2 45 1.14 Without any means for /
Example 3 40 1.15 Without any means for /
Example 4 42 1.12 Without any means for /
Example 5 44 1.13 Without any means for /
Comparative example 1 45 1.34 Has the following components 1-B
Comparative example 2 62 1.32 Has the following components 1-C
Comparative example 3 64 1.34 Has the following components 1-D
The tip adsorption effect makes the adsorption amount of the etching solution inhibitor on different parts of the copper surface different in the spraying process, so that the side adsorption amount is larger than the front surface, the side etching rate is lower than the front surface, the side etching amount is smaller, the cone angle is smaller, and the surfactant can reduce the interfacial attraction between the etching solution and the copper surface and can produce a synergistic effect with the inhibitor.
As can be seen from the data in Table 1, examples 1-5 all had good etching taper angles, no residue, and relatively stable etching performance. The absence of the dispersant in comparative examples 1 to 3 resulted in residues on the substrate surface, and the absence of the inhibitor or surfactant in comparative examples 2 and 3 resulted in an increase in the etched taper angle, and the presence of residues or excessive taper angle had an effect on the post-coating process.
2. Whether or not the polymer is precipitated
8000ppm copper powder is added into etching solution, after the copper powder is completely dissolved at room temperature, the copper powder is poured into an etching machine, after the copper powder is continuously sprayed for 36 hours under the condition of 32 ℃ and 0.15Mpa, 500ml of leaching liquor is taken out and filtered for three times by using a 0.8 mu m filter membrane, whether precipitates appear or not is observed, and whether attachments exist on the surface of a substrate or not is observed by using a Scanning Electron Microscope (SEM) for photographing, and the results are shown in table 2 and figure 2.
TABLE 2 Polymer precipitation results
As is clear from Table 2, in examples 2 to 5, the addition of the biological flocculation agent effectively adsorbed excessive copper ions, and maintained the stability of the chemical solution, so that the chemical solution maintained good etching properties, and the substrate surface was free of attachments, and the metal film layer and the etched taper angle were clearly seen. The lack of dispersant and coagulant in comparative examples 1-3 resulted in more residue on the substrate surface, no etching angle was seen, and etching performance was poor.
3. Copper powder increasing effect on etching
Copper powders of 2000ppm, 4000ppm and 8000ppm were dissolved in the prepared copper etchant, the copper substrate was etched by an etcher at 32℃and 0.15MPa, and a cross-sectional view was taken by using a Scanning Electron Microscope (SEM), and the effect of the increase in copper powder on the etching performance of the substrate was observed, and the results are shown in Table 3.
TABLE 3 influence of copper powder on etching
As shown in the data of table 3, examples 2-5 still have good etching taper angles with increasing copper powder content, and the etching performance is more stable and the etching life is longer. In the embodiment 1, due to the lack of the biological flocculating agent, when the content of copper powder is more than or equal to 8000ppm, excessive copper ions make the liquid medicine unstable, thereby reducing the etching effect and generating residues on the surface of the substrate. In comparative examples 1 to 3, the etching angle was too large and there was a residual, and as the copper powder content increased, the residual became severe, and the copper ion content in the liquid medicine increased to cause unstable etching effect, with a certain potential safety hazard.
The foregoing description of the preferred embodiments of the application 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 application.

Claims (3)

1. A copper etchant, characterized in that: comprises phosphoric acid, strong oxidizing acid, inhibitor, surfactant, dispersant, biological flocculant and deionized water;
the copper etching solution comprises, by mass, 100% of phosphoric acid, 4-8% of strong oxidizing acid, 0.2-0.4% of inhibitor, 0.2-0.4% of surfactant, 0.3-0.4% of dispersing agent, 0.5-0.9% of biological flocculant and the balance of deionized water;
the dispersing agent is one or a combination of more of naphthalene sulfonate, lignin sulfonate, sodium humate and polycarboxylate; the naphthalene sulfonate is one or a combination of more of methylene dinaphthyl sulfonate sodium, methyl naphthalene sulfonate formaldehyde condensate and benzyl naphthalene sulfonate formaldehyde condensate; the lignosulfonate is one or a combination of more of sodium lignosulfonate, potassium lignosulfonate and calcium lignosulfonate; the polycarboxylate is one or more of TERSPERSE 2700, SD-819, GYD-1252 and SD-661;
the bioflocculant is one or a combination of more than one of polyamino acid, glucan, mannans, glycoprotein and N-acetylglucosamine;
the strong oxidizing acid is one or a combination of more of sulfuric acid, hydrochloric acid, perchloric acid and nitric acid;
the inhibitor is one or more of 5-methyltetrazole, 5-aminotetrazole, benzotriazole and imidazole;
the surfactant is one or more of isopropanol, 2-phenoxyethanol, acetylenic diol and polyethylene glycol.
2. The method for preparing the copper etching solution according to claim 1, wherein: the method comprises the following steps: adding phosphoric acid, strong oxidizing acid and deionized water into a container, and stirring at 25 deg.C and 600-800rpm for 10-20min; then adding inhibitor, surfactant, dispersant and bioflocculant, stirring at 25 deg.C and 800-1000rpm for 10-30min.
3. The use of a copper etchant according to claim 1, wherein: copper etchant is used to selectively etch copper metal on the substrate at 32 ℃.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005350708A (en) * 2004-06-09 2005-12-22 Okuno Chem Ind Co Ltd Composition for etching
CN101039553A (en) * 2000-07-27 2007-09-19 阿托特希德国有限公司 Improved adhesion of polymeric materials to metal surfaces
WO2010082439A1 (en) * 2009-01-16 2010-07-22 三洋半導体製造株式会社 Etchant composition
CN111334800A (en) * 2020-04-24 2020-06-26 信丰正天伟电子科技有限公司 Novel PCB micro-etching solution and preparation method thereof
CN111808612A (en) * 2020-07-08 2020-10-23 江苏和达电子科技有限公司 Etching solution and etching supplementary solution for copper/molybdenum (niobium)/IGZO film layer, and preparation method and application thereof
CN113604804A (en) * 2021-07-07 2021-11-05 湖北兴福电子材料有限公司 Etching solution for stabilizing line width loss and etching cone angle in panel copper plating process

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101039553A (en) * 2000-07-27 2007-09-19 阿托特希德国有限公司 Improved adhesion of polymeric materials to metal surfaces
JP2005350708A (en) * 2004-06-09 2005-12-22 Okuno Chem Ind Co Ltd Composition for etching
WO2010082439A1 (en) * 2009-01-16 2010-07-22 三洋半導体製造株式会社 Etchant composition
CN111334800A (en) * 2020-04-24 2020-06-26 信丰正天伟电子科技有限公司 Novel PCB micro-etching solution and preparation method thereof
CN111808612A (en) * 2020-07-08 2020-10-23 江苏和达电子科技有限公司 Etching solution and etching supplementary solution for copper/molybdenum (niobium)/IGZO film layer, and preparation method and application thereof
CN113604804A (en) * 2021-07-07 2021-11-05 湖北兴福电子材料有限公司 Etching solution for stabilizing line width loss and etching cone angle in panel copper plating process

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