CN115280244A - Method for cleaning substrate - Google Patents
Method for cleaning substrate Download PDFInfo
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- CN115280244A CN115280244A CN202180019641.XA CN202180019641A CN115280244A CN 115280244 A CN115280244 A CN 115280244A CN 202180019641 A CN202180019641 A CN 202180019641A CN 115280244 A CN115280244 A CN 115280244A
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- component
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/027—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34
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- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
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Abstract
The present invention provides, in one embodiment, a cleaning method which is excellent in resin mask removal performance and can suppress corrosion and discoloration of copper. The present invention relates to a method for cleaning a substrate, including a step of peeling a resin mask from a substrate having a metal layer containing copper and the resin mask on a surface thereof by using a cleaning composition containing an alkaline agent (component a) and ammonium ions (NH)4 +Component B), thioglycolic acid (component C) and water (component D), wherein the molar ratio (B/C) of component B to component C is 1.5 or more.
Description
Technical Field
The present invention relates to a cleaning agent composition for resin mask peeling, a method for cleaning a substrate using the same, and a method for manufacturing an electronic component.
Background
In recent years, low power consumption, high processing speed, and miniaturization of personal computers and various electronic devices have been advanced, and miniaturization of wiring of package substrates and the like mounted on the personal computers and the electronic devices has been advanced year by year. In order to form such fine wiring and connection terminals such as pillars and bumps, a metal mask method has been mainly used, but the versatility is low, and it is difficult to cope with miniaturization of wiring and the like, and therefore, the development of new methods is advanced.
As one of the new methods, a method is known in which a thick film resin mask is formed using a dry film resist instead of a metal mask. The resin mask is finally peeled and removed, and a cleaning agent for resin mask peeling containing an alkaline agent and water is known as a cleaning agent used for cleaning such as peeling and removal.
For example, japanese patent laying-open No. 2014-78009 (patent document 1) describes a composition containing an alkanolamine, an organic solvent, water, a hydroxide, and an anticorrosive agent, which can effectively remove a film or a resist without damaging a substrate structure underlying the thick film or the resist.
Jp 2015-79244 a (patent document 2) discloses a cleaning agent composition for a resin mask layer, which contains a specific quaternary ammonium hydroxide, a water-soluble amine, an acid or an ammonium salt thereof, and water, as a cleaning agent capable of simultaneously promoting removal of the resin mask layer after heat treatment of a solder bump and suppressing solder corrosion and improving solder connection reliability.
Disclosure of Invention
The present invention relates to a method for cleaning a substrate, including a step of peeling a resin mask from a substrate having a metal layer containing copper and the resin mask on a surface thereof by using a cleaning composition containing an alkaline agent (component a) and ammonium ions (NH)4 +Component B), thioglycolic acid (component C) and water (component D), wherein the molar ratio (B/C) of component B to component C is 1.5 or more.
In one embodiment, the present invention relates to a method for manufacturing an electronic component, including a step of peeling a resin mask from a substrate having a copper-containing metal layer and the resin mask on a surface thereof by using the cleaning method of the present invention.
The present invention relates to a cleaning agent composition for stripping a resin mask, which contains an alkaline agent (component A) and ammonium ions (NH)4 +Component B), thioglycolic acid (component C) and water (component D), wherein the molar ratio (B/C) of component B to component C is1.5 or more.
The present invention relates to a use of a cleaning composition for cleaning a substrate having a metal layer containing copper and a resin mask on a surface thereof, the cleaning composition containing an alkaline agent (component A) and ammonium ions (NH)4 +Component B), thioglycolic acid (component C) and water (component D), wherein the molar ratio (B/C) of component B to component C is 1.5 or more.
Detailed Description
After forming fine wiring on a printed board or the like, a high cleaning property is required for the cleaning agent composition in order to reduce the residue of a resin mask and the residue of an auxiliary agent or the like contained in solder, a plating solution or the like used in forming the fine wiring or the bump.
Here, the resin mask is formed using a resist whose physical properties such as solubility in a developer are changed by light, electron beams, or the like. Resists are broadly classified into negative type and positive type according to their reaction method with light or electron beams. Negative resists have the property of decreasing solubility in a developer when exposed, and a layer including a negative resist (hereinafter also referred to as a "negative resist") is exposed and developed, and then the exposed portion is used as a resin mask. A positive resist has a characteristic that solubility in a developer increases when exposed, and a layer including a positive resist (hereinafter also referred to as a "positive resist") is exposed and developed, and then the exposed portion is removed, and an unexposed portion is used as a resin mask. By using a resin mask having such characteristics, a fine connection portion of a circuit board such as a metal wiring, a metal post, and a solder bump can be formed. The resin mask must be removed after the formation of the fine wiring and the bump.
However, with the miniaturization of wiring, it becomes difficult to remove the resin mask located in a fine gap, and high resin mask removability is required for the cleaning agent composition. Furthermore, corrosion and discoloration of copper, which is often used for wiring and connection terminals, cause deterioration in the quality and value of the package substrate, and therefore, a high corrosion resistance and discoloration resistance are required for the cleaning agent composition. Further, it is known that discoloration of copper is caused by, for example, generation of sulfides on the surface of copper, and in the case where a copper removal step (for example, a seed etching step) is performed after the cleaning step, it is difficult to remove the discolored copper.
Accordingly, the present invention provides, in one embodiment, a method for cleaning a substrate and a cleaning agent composition for stripping a resin mask, which have excellent resin mask removal properties and can suppress corrosion and discoloration of copper.
The present invention is based on the following recognition: by using a cleaning agent composition containing ammonium ions and thioglycolic acid in a specific molar ratio, corrosion of copper can be suppressed, and the resin mask can be efficiently removed from the surface of the substrate.
The present invention relates to a method for cleaning a substrate (hereinafter, also referred to as "the cleaning method of the present invention") including a step of peeling a resin mask from a substrate having a copper-containing metal layer and the resin mask on a surface thereof by using a cleaning composition (hereinafter, also referred to as "the cleaning composition of the present invention") containing an alkaline agent (component a) and ammonium ions (NH)4 +Component B), thioglycolic acid (component C) and water (component D), wherein the molar ratio (B/C) of component B to component C is 1.5 or more.
According to the present invention, a cleaning method which is excellent in resin mask removability and can suppress corrosion and discoloration of copper can be provided. Further, by using the cleaning method of the present invention, high-quality electronic components can be obtained with high yield. Further, by using the cleaning method of the present invention, an electronic component having a fine wiring pattern can be efficiently manufactured.
The detailed mechanism of action exhibited by the effects of the present invention is not known, but is presumed as follows.
It is considered that the alkali agent penetrates into the resin mask to promote dissociation of the alkali-soluble resin incorporated in the resin mask, and further promotes peeling of the resin mask by causing repulsion of charges generated by the dissociation, thereby improving the resin mask removability. On the other hand, the alkaline agent is considered to participate in etching (corrosion) of copper. Thioglycolic acid is believed to inhibit etching of copper by alkaline agents, but forms salts with copper leading to discoloration of the copper. It is considered that by combining ammonium ions with thioglycolic acid in a specific ratio in a detergent composition containing water, the formation of copper salts of thioglycolic acid is suppressed by the ammonium ions being present in excess relative to the thioglycolic acid, etching (corrosion) suppression of copper and good stripping performance are exhibited in the presence of an alkaline agent, and discoloration of copper is suppressed.
However, the present invention is not limited to this mechanism.
The resin mask to be peeled and removed in the present invention is a mask for protecting the surface of a substance from etching, plating, heating, or other treatment, that is, a mask functioning as a protective film. In one or more embodiments, the resin mask may be a resist layer after an exposure and development step, a resist layer subjected to at least one of exposure and development (hereinafter, also referred to as "subjected to exposure and/or development treatment"), or a cured resist layer. In one or more embodiments, the resin material for forming the resin mask may be a film-like photosensitive resin, a resist film, or a photoresist. As the resist film, a general-purpose resist film can be used.
[ cleaning agent composition ]
In one or more embodiments, the cleaning agent composition of the present invention is a cleaning agent composition for resin mask peeling, which contains an alkaline agent (component a), ammonium ions (component B), thioglycolic acid (component C), and water (component D), and the molar ratio (B/C) of the component B to the component C is 1.5 or more. According to the cleaning agent composition of the present invention, in one or more embodiments, corrosion inhibition of copper and good resin mask peeling property can be exhibited, and discoloration of copper can be inhibited. According to the cleaning agent composition of the present invention, in one or more embodiments, the resin mask positioned in the fine gap can be efficiently peeled off and removed. According to the cleaning agent composition of the present invention, in one or more embodiments, damage to a substrate resin can be suppressed. Examples of the substrate resin include a solder resist.
[ alkaline agent (component A) ]
The alkaline agent (hereinafter also simply referred to as "component a") contained in the cleaning agent composition of the present invention includes at least 1 selected from inorganic bases and organic bases in one or more embodiments, and is preferably an inorganic base from the viewpoint of reducing the load of wastewater treatment. The component A may be 1 kind or a combination of 2 or more kinds.
In one or more embodiments, the inorganic base may be a hydroxide, carbonate, or silicate of an alkali metal or an alkaline earth metal, and specifically, at least 1 selected from the group consisting of sodium hydroxide, potassium hydroxide, lithium hydroxide, calcium hydroxide, sodium carbonate, potassium carbonate, sodium silicate, and potassium silicate. Among them, from the viewpoint of improving the resin mask removability, a combination of 1 or 2 or more selected from sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate is preferable, at least one of sodium hydroxide and potassium hydroxide is more preferable, and potassium hydroxide is even more preferable. In the present invention, the inorganic base does not contain ammonia (NH)3) And ammonium ion (NH)4 +)。
In one or more embodiments, the organic base may be tetraalkylammonium hydroxide, an organic amine, or the like. Examples of the tetraalkylammonium hydroxide include quaternary ammonium hydroxides represented by the following formula (I). Examples of the organic amine include amines represented by the following formula (II). In one or more embodiments, the component a is preferably a combination of a quaternary ammonium hydroxide represented by formula (I) and an amine represented by formula (II) from the viewpoint of improving the resin mask removability.
[ chemical formula 1]
In the above formula (I), R1、R2、R3And R4Each independently is at least 1 selected from the group consisting of methyl, ethyl, propyl, hydroxymethyl, hydroxyethyl, and hydroxypropyl.
[ chemical formula 2]
In the above formula (II), R5RepresentHydrogen atom, methyl, ethyl or aminoethyl, R6Is at least 1 selected from hydrogen atom, hydroxyethyl group, hydroxypropyl group, methyl group or ethyl group, R7Is at least 1 selected from aminoethyl, hydroxyethyl or hydroxypropyl, or in formula (II), R5Is at least 1 selected from methyl, ethyl, aminoethyl, hydroxyethyl or hydroxypropyl, R6And R7Bonded to each other to form a pyrrolidine ring or a piperazine ring together with the N atom in formula (II).
Examples of the quaternary ammonium hydroxide represented by the formula (I) include: salts comprising quaternary ammonium cations and hydroxides, and the like. Specific examples of the quaternary ammonium hydroxide include at least 1 selected from the group consisting of tetramethylammonium hydroxide (TMAH), tetraethylammonium hydroxide, tetrapropylammonium hydroxide, 2-hydroxyethyltrimethylammonium hydroxide (choline), 2-hydroxyethyltriethylammonium hydroxide, 2-hydroxyethyltripropylammonium hydroxide, 2-hydroxypropyltrimethylammonium hydroxide, 2-hydroxypropyltriethylammonium hydroxide, 2-hydroxypropyltripropylammonium hydroxide, dimethylbis (2-hydroxyethyl) ammonium hydroxide, diethylbis (2-hydroxyethyl) ammonium hydroxide, dipropylbis (2-hydroxyethyl) ammonium hydroxide, tris (2-hydroxyethyl) methylammonium hydroxide, tris (2-hydroxyethyl) ethylammonium hydroxide, tris (2-hydroxyethyl) propylammonium hydroxide, tetrakis (2-hydroxyethyl) ammonium hydroxide, and tetrakis (2-hydroxypropyl) ammonium hydroxide. Among them, tetramethylammonium hydroxide and tetraethylammonium hydroxide are preferable, and tetramethylammonium hydroxide is more preferable, from the viewpoint of improving the removability of the resin mask.
Examples of the amine represented by the formula (II) include alkanolamines, primary to tertiary amines, and heterocyclic compounds. Specific examples of the amine include at least 1 selected from the group consisting of monoethanolamine, monoisopropanolamine, N-methylmonoethanolamine, N-methylisopropanolamine, N-ethylmonoethanolamine, N-ethylisopropanolamine, diethanolamine, diisopropanolamine, N-dimethylmonoethanolamine, N-dimethylmonoisopropanolamine, N-methyldiethanolamine, N-methyldiisopropanolamine, N-diethylmonoethanolamine, N-diethylmonoisopropanolamine, N-ethyldiethanolamine, N-ethyldiisopropanolamine, N- (. Beta. -aminoethyl) ethanolamine, N- (. Beta. -aminoethyl) isopropanolamine, N- (. Beta. -aminoethyl) diethanolamine, N- (. Beta. -aminoethyl) diisopropanolamine, 1-methylpiperazine, 1- (2-hydroxyethyl) pyrrolidine, 1- (2-hydroxyethyl) piperazine, ethylenediamine and diethylenetriamine. Among them, monoethanolamine and diethanolamine are preferable, and monoethanolamine is more preferable from the viewpoint of improving the resin mask removability.
The content of component a in the case of using the cleaning agent composition of the present invention is preferably 0.5% by mass or more, more preferably 2% by mass or more, and is preferably 8% by mass or less, more preferably 6% by mass or less from the same viewpoint of improving the removability of the resin mask and suppressing the corrosion of copper. More specifically, the content of the component a when the cleaning agent composition of the present invention is used is preferably 0.5% by mass or more and 8% by mass or less, and more preferably 2% by mass or more and 6% by mass or less. When the component a is a combination of 2 or more, the content of the component a means the total content thereof.
The "content of each component when the detergent composition is used" in the present invention means the content of each component at the time of cleaning, that is, at the time when cleaning using the detergent composition is started.
[ ammonium ion: NH (NH)4 +(component B)]
The ammonium ion (hereinafter also referred to as "component B") contained in the cleaning agent composition of the present invention is represented by the formula NH4 +Ammonium ion as shown.
As the supply source of the component B, in one or more embodiments, ammonium ion (NH) may be supplied4 +) The compound (b) is not particularly limited, but from the viewpoint of resin mask removability and copper corrosion inhibition, at least 1 kind of ammonia and ammonium salt of organic acid may be mentioned. Ammonia can also be used in a gaseous state, but from the viewpoint of workability, it is preferably used in the form of an aqueous solution (ammonia water). Examples of the ammonium salt of the organic acid include an ammonium salt of thioglycolic acid (component C). The supply source of the component B is preferably a combination of ammonia and an ammonium salt of thioglycolic acid (component C) or a combination of ammonia and an ammonium salt of carboxylic acid from the viewpoints of resin mask removability and copper corrosion inhibition.
The content of component B (mol/100 g) relative to 100g of the detergent composition in the use of the detergent composition of the present invention is preferably 0.02mol/100g or more, more preferably 0.04mol/100g or more, and is preferably 0.08mol/100g or less, more preferably 0.06mol/100g or less from the same viewpoint of improving the removability of the resin mask and suppressing the corrosion of copper. More specifically, when the detergent composition of the present invention is used, the content (mol/100 g) of component B relative to 100g of the detergent composition is preferably 0.02mol/100g or more and 0.08mol/100g or less, and more preferably 0.04mol/100g or more and 0.06mol/100g or less.
Mercaptoacetic acid (component C)
The source of the thioglycolic acid (component C) contained in the cleaning agent composition of the present invention includes thioglycolic acid or a salt thereof. For example, ammonium salts of thioglycolic acid may be used as the source of component B and component C. For example, monoethanolamine thioglycolate can be used as a supply source of the component A and the component C.
The content (mass%) of thioglycolic acid (hereinafter also referred to as "component C") when the cleaning agent composition of the present invention is used is preferably 0.5 mass% or more, more preferably 1 mass% or more, and from the same viewpoint, is preferably 3 mass% or less, more preferably 2 mass% or less, from the viewpoint of improving the removability of the resin mask and suppressing corrosion of copper. More specifically, the content of the component C in the cleaning agent composition of the present invention is preferably 0.5% by mass or more and 3% by mass or less, and more preferably 1% by mass or more and 2% by mass or less.
The content (mol/100 g) of the component C with respect to 100g of the cleaning composition of the present invention is preferably 0.005mol/100g or more, more preferably 0.01mol/100g or more, and from the same viewpoint of improving the removability of the resin mask and suppressing the corrosion of copper, and is preferably 0.03mol/100g or less, more preferably 0.02mol/100g or less. More specifically, when the cleaning composition of the present invention is used, the content of component C is preferably 0.005mol/100g or more and 0.03mol/100g or less, and more preferably 0.01mol/100g or more and 0.02mol/100g or less, based on 100g of the cleaning composition.
From the viewpoint of improving the resin mask removability, suppressing copper corrosion, and suppressing copper discoloration, the molar ratio (B/C) of the component B to the component C (content of the component B/content of the component C) in the cleaning agent composition of the present invention is 1.5 or more, preferably 2 or more, and more preferably 3 or more, and from the same viewpoint, preferably 5 or less, and more preferably 4 or less. More specifically, the molar ratio (B/C) is preferably 2 or more and 5 or less, and more preferably 3 or more and 4 or less.
[ Water (component D) ]
Examples of the water (hereinafter, also referred to as "component D") contained in the cleaning agent composition of the present invention include ion-exchanged water, RO water, distilled water, pure water, and ultrapure water in one or more embodiments.
The content of the component D in the cleaning agent composition of the present invention may be set to the balance excluding the component a, the component B, the component C and any component described later. Specifically, the content of the component D in the case of using the cleaning agent composition of the present invention is preferably 45 mass% or more, more preferably 60 mass% or more, and even more preferably 80 mass% or more, from the viewpoint of improving the resin mask removability, from the viewpoint of suppressing copper corrosion, reducing the load of the drain treatment, and from the viewpoint of reducing the influence on the substrate, and is preferably 99 mass% or less, more preferably 98 mass% or less, and even more preferably 97 mass% or less. More specifically, the content of the component D when the cleaning agent composition of the present invention is used is preferably 45 mass% or more and 99 mass% or less, more preferably 60 mass% or more and 98 mass% or less, and further preferably 80 mass% or more and 97 mass% or less.
The total amount of the component a, the component B, the component C and the component D when the cleaning agent composition of the present invention is used is preferably 60 mass% or more, more preferably 90 mass% or more, and still more preferably 95 mass% or more, from the viewpoints of improving the resin mask removability and suppressing copper corrosion.
[ organic solvent (component E) ]
The cleaning agent composition of the present invention may further contain an organic solvent (hereinafter also referred to as "component E") in one or more embodiments. The component E may be 1 kind or a combination of 2 or more kinds.
In one or more embodiments, component E includes at least 1 solvent selected from glycol ethers and aromatic ketones.
The glycol ether is a compound having a structure in which 1 to 3 moles of ethylene glycol are added to an alcohol having 1 to 8 carbon atoms, from the viewpoint of improving the resin mask removability, suppressing copper corrosion, and reducing the influence on the substrate. Specific examples of the glycol ether include at least 1 selected from the group consisting of diethylene glycol monobutyl ether (BDG), ethylene glycol monobenzyl ether, diethylene glycol monohexyl ether, ethylene glycol monophenyl ether, and diethylene glycol diethyl ether.
As the aromatic ketone, acetophenone and the like are mentioned from the viewpoints of improving the resin mask removability, suppressing copper corrosion, and reducing the influence on the substrate.
When the cleaning agent composition of the present invention contains the component E, the content of the component E in the case of using the cleaning agent composition of the present invention is preferably 1 mass% or more, more preferably 2 mass% or more, and further preferably 3 mass% or more from the viewpoint of improving the resin mask removability, and is preferably 40 mass% or less, more preferably 20 mass% or less, and further preferably 6 mass% or less from the viewpoint of suppressing copper corrosion, reducing the load of the drainage treatment, and reducing the influence on the substrate. More specifically, the content of the component E when the cleaning agent composition of the present invention is used is preferably 1% by mass or more and 40% by mass or less, more preferably 2% by mass or more and 20% by mass or less, and further preferably 3% by mass or more and 6% by mass or less. When the component E is a combination of 2 or more, the content of the component E means the total content thereof.
[ chelating agent (component F) ]
The cleaning agent composition of the present invention may further contain a chelating agent (hereinafter also referred to as "component F") in one or more embodiments. The component F may be 1 species or a combination of 2 or more species.
The component F includes, for example, a compound having at least 1 acid group selected from a carboxyl group and a phosphonic acid group of 2 or more, and a compound having the acid group of preferably 4 or less is preferable from the viewpoint of improving the resin mask removal property and suppressing copper corrosion. Specific examples of the component F include aminotrimethylene phosphonic acid, 2-phosphonobutane-1, 2, 4-tricarboxylic acid, etidronic acid (1-hydroxyethane-1, 1-diphosphonic acid, HEDP), and the like in one or more embodiments. Among them, 2-phosphonobutane-1, 2, 4-tricarboxylic acid, etidronic acid (HEDP), and the like, which are compounds not containing a nitrogen atom, are preferable from the viewpoint of reducing environmental load.
The molecular weight of the component F is preferably 1000 or less, and more preferably 500 or less, from the viewpoint of improving the removability of the resin mask and suppressing corrosion of copper.
When the cleaning agent composition of the present invention contains component F, the content of component F in the case of using the cleaning agent composition of the present invention is preferably 0.5 mass% or more, more preferably 1 mass% or more, and from the same viewpoint, preferably 5 mass% or less, more preferably 3 mass% or less, from the viewpoint of improving the resin mask removability and suppressing copper corrosion. More specifically, the content of the component F in the case of using the cleaning agent composition of the present invention is preferably 0.5% by mass or more and 5% by mass or less, and more preferably 1% by mass or more and 3% by mass or less. When the component F is a combination of 2 or more, the content of the component F means the total content thereof.
[ other ingredients ]
The cleaning agent composition of the present invention may contain other components as necessary in addition to the components A to F. Examples of the other components include components that can be used in a general cleaning agent, and examples thereof include organic solvents other than component E, surfactants, chelating agents other than component F, thickeners, dispersants, rust inhibitors, polymer compounds, solubilizing agents, antioxidants, preservatives, antifoaming agents, and antibacterial agents.
When the cleaning agent composition of the present invention is used, the content of the other component is preferably 0% by mass or more and 2% by mass or less, more preferably 0% by mass or more and 1.5% by mass or less, still more preferably 0% by mass or more and 1.3% by mass or less, and still more preferably 0% by mass or more and 1% by mass or less.
The cleaning agent compositions of the present invention may be free of fluorine compounds in one or more embodiments.
The total content of organic substances derived from the component a, the component B, the component C, and any component (the component E, the component F, and other components) when the cleaning agent composition of the present invention is used is preferably 30% by mass or less, more preferably 25% by mass or less, further preferably 20% by mass or less, and still further preferably 16% by mass or less, and from the viewpoint of improving the resin mask removability, is preferably 2% by mass or more, more preferably 3% by mass or more, further preferably 4% by mass or more, and still further preferably 6% by mass or more, from the viewpoint of reducing the load of the drainage treatment and reducing the influence on the substrate. More specifically, when the cleaning agent composition of the present invention is used, the total content of organic substances derived from the component a, the component B, the component C, and any component (the component E, the component F, and other components) is preferably 2 mass% or more and 30 mass% or less, more preferably 3 mass% or more and 25 mass% or less, still more preferably 4 mass% or more and 20 mass% or less, and still more preferably 6 mass% or more and 16 mass% or less.
[ Process for producing detergent composition ]
The cleaning agent composition of the present invention can be produced by blending an alkaline agent (component a), a supply source of ammonium ions (component B), thioglycolic acid (component C) or a salt thereof, water (component D), and optionally the above-mentioned optional components by a known method. For example, in one or more embodiments, the cleaning composition of the present invention may be one in which an alkaline agent (component a), a supply source of ammonium ions (component B), thioglycolic acid (component C) or a salt thereof, and water (component D) are blended.
Accordingly, the present invention relates to a method for producing a cleaning agent composition, which comprises a step of blending at least an alkaline agent (component a), a supply source of ammonium ions (component B), thioglycolic acid (component C) or a salt thereof, and water (component D). In the present invention, "blending" includes mixing an alkaline agent (component A), a supply source of ammonium ions (component B), thioglycolic acid (component C) or a salt thereof, water, and optionally the above-mentioned optional components simultaneously or in any order. In the method for producing the detergent composition of the present invention, the preferred amounts of the respective components may be the same as the preferred amounts of the respective components of the detergent composition of the present invention.
The cleaning agent composition of the present invention may be in a form directly used for cleaning, or may be prepared as a concentrate in which the amount of water (component D) is reduced within a range where storage stability is impaired without causing separation, precipitation, or the like. From the viewpoint of transportation and storage, the concentrate of the detergent composition is preferably a concentrate having a dilution ratio of 3 times or more, and from the viewpoint of storage stability, a concentrate having a dilution ratio of 30 times or less. The concentrate of the detergent composition can be diluted with water (component D) at the time of use so that the contents of the respective components (component a, component B, component C, component D, component E, component F, and others) are as described above (i.e., the content at the time of cleaning). Further, the concentrate of the cleaning agent composition may be used by adding each component separately at the time of use. The "in use" or "in cleaning" of the cleanser composition as the concentrate in the present invention means a state in which the concentrate of the cleanser composition is diluted.
[ subject to be cleaned ]
In one or more embodiments, the cleaning composition of the present invention can be used to clean a substrate having a metal layer comprising copper and a resin mask on a surface thereof. The copper-containing metal layer is a copper plating layer in one or more embodiments. The copper plating layer can be formed by, for example, electroless copper plating.
In another or more embodiments, the cleaning agent composition of the present invention can be used for cleaning an object to be cleaned to which a resin mask is attached. In one or more embodiments, examples of the object to be cleaned include objects to be cleaned having a copper-containing metal portion on the surface thereof, and examples thereof include electronic components and intermediate products for manufacturing the same. Examples of the electronic component include at least 1 component selected from metal plates such as a printed circuit board, a wafer, a copper plate, and an aluminum plate. The manufacturing intermediate is an intermediate product in a manufacturing process of an electronic component, and includes an intermediate product after a resin mask process. Specific examples of the object to be cleaned to which the resin mask is attached include: electronic components and the like having wiring, connection terminals, and the like formed on the surface of a substrate through a process of performing soldering, plating treatment (copper plating, aluminum plating, nickel plating, and the like), and the like using a resin mask. Accordingly, the present invention relates, in one aspect, to the use of the cleaning agent composition of the present invention as a cleaning agent in the production of electronic parts.
In one or more embodiments, the cleaning agent composition of the present invention is excellent in removability of a resin mask located in a fine gap. The object to be cleaned is preferably a substrate having a fine gap and a resin mask is present in the gap, from the viewpoint of exhibiting resin mask removability of the cleaning agent composition. Examples of the substrate having a fine gap include: a substrate having copper wiring (wire) and having a minimum value of a wiring interval (gap) of preferably 1 μm or more and preferably 10 μm or less, more preferably 6 μm or less.
In addition, the cleaning agent composition of the present invention can suppress damage to a substrate resin in one or more embodiments. In view of the low damage of the cleaning agent composition to the substrate resin, the object to be cleaned may be a substrate having a resin on the surface thereof, and for example, the substrate is preferably a substrate having a solder resist resin.
In terms of cleaning effect, the cleaning agent composition of the present invention can be suitably used in one or more embodiments for cleaning an object to be cleaned to which a resin mask is attached, or a resin mask further subjected to plating treatment and/or heat treatment. The resin mask may be, for example, a negative resin mask or a positive resin mask. The negative resin mask of the present invention is formed using a negative resist, and examples thereof include a negative resist subjected to exposure and/or development treatment. The positive type resin mask in the present invention is formed using a positive type resist, and examples thereof include a positive type resist subjected to exposure and/or development treatment.
[ cleaning method ]
The cleaning method of the present invention, in one or more embodiments, comprises: a step of peeling the resin mask from the substrate (object to be cleaned) having the copper-containing metal layer and the resin mask on the surface thereof by using the cleaning agent composition of the present invention (hereinafter, also referred to simply as "peeling step"). In one or more embodiments, the stripping step comprises contacting the object to be cleaned with the cleaning composition of the present invention. According to the cleaning method of the present invention, the resin mask can be efficiently removed by peeling off while suppressing corrosion and discoloration of copper. According to the cleaning method of the present invention, in one or more embodiments, the resin mask positioned in the minute gap can be efficiently peeled off and removed. According to the cleaning method of the present invention, in one or more embodiments, damage to the substrate resin can be suppressed. Examples of the substrate resin include a solder resist.
Examples of the method for peeling a resin mask from an object to be cleaned using the cleaning composition of the present invention or the method for bringing the cleaning composition of the present invention into contact with an object to be cleaned include: a method of performing contact by immersing in a cleaning bath containing a cleaning agent composition; a method of spraying the cleaning agent composition in a spray form to contact the substrate (spraying method); an ultrasonic cleaning method in which ultrasonic irradiation is performed during immersion, and the like. The cleaning agent composition of the invention can be directly used for cleaning without dilution. The object to be cleaned may be the above-mentioned object to be cleaned.
In one or more embodiments, the cleaning method of the present invention may include a step of contacting the object to be cleaned with the cleaning agent composition, washing the object with water, and drying the object. The cleaning method of the present invention may include, in one or more embodiments, a step of bringing the object to be cleaned into contact with the cleaning agent composition and then rinsing the object with water.
In the cleaning method of the present invention, it is preferable that ultrasonic waves are irradiated when the cleaning composition of the present invention is brought into contact with an object to be cleaned, and the ultrasonic waves are more preferably of a relatively high frequency, from the viewpoint of facilitating the exertion of the cleaning power of the cleaning composition of the present invention. From the same viewpoint, the irradiation conditions of the ultrasonic waves are, for example, preferably 26 to 72kHz and 80 to 1500W, more preferably 36 to 72kHz and 80 to 1500W.
In the cleaning method of the present invention, the temperature of the cleaning composition of the present invention is preferably 40 ℃ or higher, more preferably 50 ℃ or higher, from the viewpoint of easily exerting the cleaning power of the cleaning composition of the present invention, and is preferably 70 ℃ or lower, more preferably 60 ℃ or lower, from the viewpoint of reducing the influence on the substrate.
[ method for producing electronic component ]
The present invention relates to a method for manufacturing an electronic component (hereinafter, also referred to as "method for manufacturing an electronic component of the present invention") including: a step (cleaning step) of cleaning a substrate (object to be cleaned) having a copper-containing metal layer and a resin mask on the surface thereof by using the cleaning method of the present invention. Examples of the object to be cleaned include the above-mentioned object to be cleaned. The method for manufacturing an electronic component of the present invention may include, in one or more embodiments, the steps of: and a step of etching the metal layer containing copper after the cleaning step.
In the method for manufacturing an electronic component according to the present invention, the cleaning by the cleaning method of the present invention can suppress corrosion and discoloration of copper and effectively remove a resin mask attached to the electronic component, thereby realizing the manufacture of an electronic component with high reliability. Further, by performing the cleaning method of the present invention, the resin mask adhering to the electronic component can be easily removed, and therefore, the cleaning time can be shortened, and the manufacturing efficiency of the electronic component can be improved.
[ set ]
The present invention relates to a kit (hereinafter also referred to as "kit of the present invention") for use in any one of the cleaning method of the present invention and the method for manufacturing an electronic component of the present invention. The kit of the invention is in one or more embodiments a kit for making the detergent composition of the invention. According to the kit of the present invention, a cleaning agent composition which is excellent in resin mask removability and can suppress corrosion and discoloration of copper can be obtained.
One embodiment of the kit of the present invention includes the following kit (three-component type cleaning agent composition): the solution containing the component A (solution 1), the solution containing the component B (solution 2), and the solution containing the component C (solution 3) are included in a state of not being mixed with each other, at least one selected from the solution 1, the solution 2, and the solution 3 further contains a part or all of water (component D), and the solution 1, the solution 2, and the solution 3 are mixed at the time of use. After mixing the 1 st, 2 nd and 3 rd liquids, the mixture may be diluted with water (component D) as necessary. The liquid 1, the liquid 2 and the liquid 3 may each contain any of the above components as necessary.
Other embodiments of the kit of the present invention include the following kits (two-pack type cleaning agent composition): the solution containing the component A (solution 1) and the solution containing the components B and C (solution 2) are included in a state where they are not mixed with each other, and at least one of the solution 1 and the solution 2 further contains a part or all of water (component D), and the solution 1 and the solution 2 are mixed at the time of use. After mixing the 1 st liquid and the 2 nd liquid, the mixture may be diluted with water (component D) as necessary. The 1 st liquid and the 2 nd liquid may each contain any of the above-mentioned components as necessary.
Examples
The present invention will be specifically described below with reference to examples, but the present invention is not limited to these examples at all.
1. Preparation of cleaning agent compositions of examples 1 to 9 and comparative examples 1 to 3
The components shown in tables 1 to 2 were mixed in the amounts (mass%, effective components) described in tables 1 to 2, and the mixture was stirred and mixed to prepare cleaning agent compositions of examples 1 to 9 and comparative examples 1 to 3. The content (mol/100 g, active ingredient) of ammonium ion (component B), the content (mass%, mol/100g, active ingredient) of thioglycolic acid (component C), and the molar ratio (B/C) of ammonium ion/thioglycolic acid in each of the prepared detergent compositions are shown in tables 1 to 2.
The following were used in the preparation of the cleaning agent compositions of examples 1 to 9 and comparative examples 1 to 3.
TMAH: tetramethylammonium hydroxide [ 25% concentration manufactured by Showa Denko K.K. ] (component A)
MEA: monoethanolamine [ manufactured by Japan catalyst of Kabushiki Kaisha ] (component A)
Ammonia [ Fuji film and Wako pure chemical industries, first-class, 25% aqueous solution ] (supply of component B)
Ammonium thioglycolate [ 60% aqueous solution manufactured by Tokyo chemical industry Co., ltd ] (supply sources of component B and component C)
Water [ pure water of 1. Mu.S/cm or less produced by Water purifier G-10DSTSET, manufactured by ORGANO corporation ] (component D)
BDG: diethylene glycol monobutyl ether [ diethylene glycol monobutyl ether, manufactured by Nippon emulsifier Co., ltd. ]component E)
HEDP: etidronic acid [ Dequest2010, 60% concentration, manufactured by Italmatch Japan K.K. ] (component F)
Ammonium formate [ Fuji film and Guangdong Kabushiki Kaisha ]
Dimethyl sulfoxide [ Fuji film and Guangdong chemical Co., ltd ]
2. Evaluation of cleaning composition (examples 1 to 9 and comparative examples 1 to 2)
The following evaluations were made with respect to the cleaning agent compositions of examples 1 to 9 and comparative examples 1 to 2.
[ production of test piece 1]
A PKG (package) substrate circuit-forming photosensitive film was laminated on the surface of the electroless-plated substrate under the following conditions, and cured by exposure treatment (exposure step), thereby obtaining a substrate (test piece 1, 30mm × 50 mm) having a resin mask (cured resist).
(1) Laminating: the treatment was carried out at a roll temperature of 50 ℃ and a roll pressure of 1.4Bar using a cleaning roll (manufactured by RAYON Industrial Co., ltd., RY-505Z) and a vacuum applicator (manufactured by Rohm and Haas Co., ltd., VA7024/HP 5).
(2) Exposure: using a direct writing apparatus for a printed circuit board (Mercurex LI-9500, manufactured by SCREEN Graphic and Precision Solutions Co., ltd.), 15mJ/cm2The exposure amount of (2) is increased.
[ cleaning test ]
100g of each of the cleaning agent compositions of examples 1 to 9 and comparative examples 1 to 2 was added to a tall-type 200mL glass beaker, heated to 50 ℃ and stirred at 600rpm using a rotor (fluororesin (PTFE), φ 8mm × 25 mm), and the test piece 1 was immersed for 10 minutes in this state. Then, the glass was immersed in a rinsing bath containing 100g of water in a 100mL glass beaker, rinsed, and dried with a nitrogen blower.
[ evaluation of peeling time (removability) of resin mask ]
In the above cleaning test, the time (minutes) until the resin mask was completely removed by visual observation was measured.
[ evaluation of Cu etching Rate (evaluation of Corrosion (corrosiveness)) of copper ]
2.5L of each of the cleaning agent compositions was prepared, heated to 50 ℃ and subjected to copper plating on the surface (about an area, each side of which is 25cm in area) while circulating by means of a box-type spray cleaning machine equipped with a solid cone nozzle (J020, manufactured by Takara Shuzo Co., ltd.) as a spray nozzle2Double sides of 50cm2) The test piece 2 (substrate having a copper-plated layer on the surface) was sprayed for 4 minutes (pressure: 0.05MPa; spraying distance: 80 mm). After diluting the cleaning agent composition, the amount of elution of copper was measured by ICP analysis (Agilent 5110 ICP-OES manufactured by Agilent Technologies), and the density of copper was measured by the following formula, and the density of copper was taken to be 8.94g/cm3And the Cu etching rate (. Mu.m/min) was evaluated from the elution amount. The lower the value of the Cu etching rate, the more excellent the copper corrosion inhibition effect can be judged.
Cu etching rate (μm/min) = elution amount of copper (weight) ÷ density of copper ÷ plating area ÷ processing time
Appearance of copper on substrate (evaluation of discoloration of copper)
In the above evaluation of the etching rate, the presence or absence of discoloration of the copper portion was visually observed.
[ evaluation of damage to substrate resin ]
The substrate (test piece 3) having the solder resist resin was subjected to the above cleaning test, and whether or not a change in color or the like occurred in the resin portion of the substrate before and after the above cleaning test was visually confirmed, and evaluated according to the following evaluation criteria.
< evaluation criteria >
A: no change was observed before and after the washing test.
B: changes were visible before and after the cleaning test.
[ Table 1]
As shown in Table 1, it is understood that the cleaning agent compositions of examples 1 to 9 inhibit corrosion and discoloration of copper and are excellent in resin mask removability, as compared with comparative example 1 in which the molar ratio B/C is not within the predetermined range and comparative example 2 in which component C is not contained.
In addition, in the case of using thioglycerol instead of ammonium thioglycolate for the cleaning agent composition of example 3, the resin mask removability and the copper discoloration suppression effect were inferior to those of example 3 (data not shown).
3. Evaluation of cleaning composition (example 8 and comparative example 3)
The following evaluations were carried out using the prepared cleaner compositions of example 8 and comparative example 3.
[ production of test piece 4 with Thick film DF ]
A substrate (test piece 4, 30mm × 50 mm) having a resin mask (cured resist layer) was obtained by laminating a photosensitive thick film (thickness 140 μm) for forming a PKG substrate circuit on the surface of the electroless plated substrate under the following conditions and curing the film by exposure treatment (exposure step).
(1) Laminating: the treatment was carried out at a roll temperature of 50 ℃ and a roll pressure of 1.4Bar using a cleaning roll (Clean Roller) (manufactured by RAYON Industrial Co., ltd., RY-505Z) and a vacuum applicator (manufactured by Rohm and Haas Co., ltd., VA7024/HP 5).
(2) Exposure: using a direct writing apparatus for a printed circuit board (Mercurex LI-9500, manufactured by SCREEN Graphic and Precision Solutions Co., ltd.), 15mJ/cm2The exposure amount of (2) is increased.
[ production of test piece 5 having thin line Circuit Pattern ]
A PKG substrate circuit-forming photosensitive film was laminated on the surface of the electroless-plated substrate under the following conditions, and cured by exposure treatment (exposure step), and then electrolytic plating was performed, thereby obtaining a substrate (test piece 5, 30mm × 50 mm) having a resin mask (cured resist layer) with a line/space of 5 μm/5 μm and a fine line circuit pattern.
(1) Laminating: the treatment was carried out at a roll temperature of 50 ℃ and a roll pressure of 1.4Bar using a cleaning roll (Clean Roller) (manufactured by RAYON Industrial Co., ltd., RY-505Z) and a vacuum applicator (manufactured by Rohm and Haas Co., ltd., VA7024/HP 5).
(2) Exposure: using a direct writing apparatus for a printed circuit board (Mercurex LI-9500, manufactured by SCREEN Graphic and Precision Solutions Co., ltd.), at 15mJ/cm2The exposure amount of (2) is increased.
[ cleaning test ]
100g of each of the cleaning agent compositions of example 8 and comparative example 3 was added to a tall-type 200mL glass beaker, heated to 50 ℃ and stirred at 600rpm using a rotor (fluororesin (PTFE), 8 mm. Times.25 mm), and the test piece 4 or 5 was immersed in this state for 10 minutes. Then, the glass was immersed in a rinsing bath containing 100g of water in a 100mL glass beaker, rinsed, and dried with a nitrogen blower.
[ peeling time of resin mask (evaluation of removability) ]
In the above cleaning test of the test piece 4, the time (minutes) until the resin mask was completely removed by visual observation was measured.
[ detachability (evaluation of removability) of thin line circuit pattern ]
The presence or absence of the resin mask remaining in the fine line circuit pattern of the test piece 5 after the cleaning test was visually confirmed by magnifying the resin mask to 1000 times using an optical microscope "digital microscope VHX-2000" (manufactured by keyence corporation).
[ Table 2]
As shown in table 2, it is understood that the cleaning agent composition of example 8 is superior in resin mask removability to comparative example 3 containing no component C.
Industrial applicability
According to the present invention, a cleaning method which is excellent in resin mask removability and can suppress corrosion and discoloration of copper can be provided. The cleaning method of the present invention can shorten the cleaning process of the electronic component adhered with the resin mask, improve the performance and reliability of the manufactured electronic component, and improve the productivity of the semiconductor device.
Claims (14)
1. A method for cleaning a substrate, comprising a step of peeling a resin mask from a substrate having a metal layer containing copper and the resin mask on the surface thereof by using a cleaning agent composition,
the cleaning agent composition contains: alkaline agent, namely component A; ammonium ions, i.e. NH4 +A component B; thioglycolic acid, component C; and water, component D, wherein the molar ratio of component B to component C, that is, B/C, is 1.5 or more.
2. The cleaning method according to claim 1, wherein the copper-containing metal layer is a copper plated layer.
3. The cleaning method according to claim 1 or 2, wherein the resin mask is a cured resist layer.
4. The cleaning method according to any one of claims 1 to 3, wherein a content of the component D is 60% by mass or more when the cleaning agent composition is used.
5. The cleaning method according to any one of claims 1 to 4, wherein component A is tetraalkylammonium hydroxide.
6. The cleaning method according to any one of claims 1 to 5, wherein the substrate has copper wirings, and a minimum value of intervals of the wirings is 1 μm or more and 10 μm or less.
7. The cleaning method according to any one of claims 1 to 6, wherein the substrate is a substrate having a solder resist resin.
8. A method for manufacturing an electronic component, comprising a step of cleaning a substrate having a metal layer containing copper and a resin mask on a surface thereof by using the cleaning method according to any one of claims 1 to 7.
9. A cleaning agent composition for stripping a resin mask, comprising: alkaline agent, namely component A; ammonium ions, i.e. NH4 +A component B; thioglycolic acid, component C; and water, component D, and
the molar ratio of component B to component C, namely B/C, is 1.5 or more.
10. The cleaning agent composition according to claim 9, wherein the component A is tetraalkylammonium hydroxide.
11. The cleaning agent composition according to claim 9 or 10, wherein the content of the component A is 0.5% by mass or more and 10% by mass or less, and the content of the component C is 0.4% by mass or more and 4% by mass or less.
12. The cleaning agent composition according to any one of claims 9 to 11, wherein the total amount of the component A, the component B, the component C and the component D is 90% by mass or more.
13. The cleaning agent composition according to any one of claims 9 to 12, wherein the content of the component D is 60% by mass or more.
14. The use of a cleaning agent composition for cleaning a substrate having a metal layer containing copper and a resin mask on the surface thereof,
the cleaning agent composition comprises: alkaline agent, namely component A; ammonium ions, i.e. NH4 +A component B; thioglycolic acid, i.e. component C; and water, namely component D, wherein the molar ratio of component B to component C, namely B/C, is 1.5 or more.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
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| JP2020-072961 | 2020-04-15 | ||
| JP2020072961 | 2020-04-15 | ||
| PCT/JP2021/015404 WO2021210599A1 (en) | 2020-04-15 | 2021-04-14 | Method of cleaning substrate |
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| CN115280244A true CN115280244A (en) | 2022-11-01 |
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| CN202180019641.XA Pending CN115280244A (en) | 2020-04-15 | 2021-04-14 | Method for cleaning substrate |
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| JP (1) | JPWO2021210599A1 (en) |
| CN (1) | CN115280244A (en) |
| TW (1) | TW202215172A (en) |
| WO (1) | WO2021210599A1 (en) |
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| CN115261879A (en) * | 2022-07-05 | 2022-11-01 | 南通群安电子材料有限公司 | Organic film removing liquid suitable for MSAP (multiple-site amplification process) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4914629B1 (en) * | 1970-12-08 | 1974-04-09 | ||
| JPS5192735A (en) * | 1975-02-12 | 1976-08-14 | KINZOKUSENJOYOSOSEIBUTSU | |
| JPS60218488A (en) * | 1984-04-12 | 1985-11-01 | Rinrei:Kk | Iron rust remover |
| JP2597931B2 (en) * | 1991-08-19 | 1997-04-09 | 株式会社不二越 | Removal agent for titanium coating on high speed tool steel |
| JPH08283791A (en) * | 1993-10-22 | 1996-10-29 | Kazuyuki Urushibara | Remover for ink and oil stain |
| JP3041763B2 (en) * | 1995-11-14 | 2000-05-15 | 修 弓田 | Method for producing rust remover for wheel and rust remover for wheel obtained by this method |
| JP2003027092A (en) * | 2001-07-16 | 2003-01-29 | Techno Trading:Kk | Rust remover detergent composition |
| JP3797541B2 (en) * | 2001-08-31 | 2006-07-19 | 東京応化工業株式会社 | Photoresist stripping solution |
| JP2007114519A (en) * | 2005-10-20 | 2007-05-10 | Tokyo Ohka Kogyo Co Ltd | Photoresist stripping liquid |
| JP5637548B2 (en) * | 2012-02-09 | 2014-12-10 | クラシエ製薬株式会社 | Exfoliating composition |
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2021
- 2021-04-14 WO PCT/JP2021/015404 patent/WO2021210599A1/en active Application Filing
- 2021-04-14 CN CN202180019641.XA patent/CN115280244A/en active Pending
- 2021-04-14 JP JP2022515407A patent/JPWO2021210599A1/ja active Pending
- 2021-04-15 TW TW110113568A patent/TW202215172A/en unknown
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| WO2021210599A1 (en) | 2021-10-21 |
| TW202215172A (en) | 2022-04-16 |
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