Chemical liquid for producing semiconductor in container, method for producing chemical liquid for producing semiconductor in container, and method for storing chemical liquid for producing semiconductor

Abstract

To provide a chemical liquid for producing a semiconductor in a container capable of suppressing increase of particles in the chemical liquid with time, and also suppressing generation of defects, a method for producing a chemical liquid for producing a semiconductor in a container, and a method for storing a chemical liquid for producing a semiconductor.SOLUTION: A chemical liquid for producing a semiconductor is housed in a container, where the container includes a base material composed of passivation-treated austenitic stainless steel, a passivation-treated surface is an inner surface of the container, the chemical liquid for producing a semiconductor includes one or more metal constituents selected from the group consisting of V, Sn, and Pb, and an organic solvent, and the content of the metal constituent after the lapse of 30 days from the time of filling into the container is 0.1 mass ppt-1 mass ppm. Also provided are a method for producing a chemical liquid for producing a semiconductor in a container, and a method for storing a chemical liquid for producing a semiconductor.SELECTED DRAWING: None

Description

Technical Field

[0001] The present invention relates to a chemical solution for semiconductor manufacturing contained in a container, a method for manufacturing the chemical solution for semiconductor manufacturing contained in a container, and a method for storing the chemical solution for semiconductor manufacturing.

Background Art

[0002] A semiconductor device is formed by laminating a low dielectric layer, an insulating layer, a metal wiring (layer), etc. on a substrate such as a silicon wafer. Such a semiconductor device is manufactured by a lithography method in which an etching process is performed using a resist pattern as a mask to form each of the above-described layers and metal wiring.

[0003] In the manufacturing process of a semiconductor device including the above-described lithography process, various chemical solutions for semiconductor manufacturing are used as a resist solution, a developer, a stripping solution, a cleaning solution, a pre-rinse solution, a rinse solution, a chemical mechanical polishing (CMP) slurry, etc.

[0004] Regarding such a technique, for example, Patent Document 1 discloses a chemical solution container having a container and a chemical solution contained in the container, wherein the chemical solution contains a solvent, metal-containing particles containing metal atoms, and an organic compound having a higher ClogP value than the solvent, the content of the metal-containing particles is 10 mass ppt or less with respect to the total mass of the chemical solution, a gas containing an organic compound having a higher ClogP value than the solvent exists in the void portion of the container, and the total content of the organic compound in the gas and the organic compound in the chemical solution is 100,000 mass ppt or less with respect to the total mass of the chemical solution.

Prior Art Documents

Patent Documents

[0005]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0006] By the way, if fine particles are contained in the chemical solution for semiconductor manufacturing, they will cause defects in semiconductor devices. However, as a result of intensive studies by the present inventors, it has been found that simply reducing the content of particles in the chemical solution for semiconductor manufacturing cannot achieve both suppression of the increase in particles over time in the chemical solution due to the passage of storage days and suppression of the occurrence of defects.

[0007] The present invention has been made in view of the above circumstances, and an object thereof is to provide a chemical solution for semiconductor manufacturing in a container, a method for manufacturing the chemical solution for semiconductor manufacturing in a container, and a method for storing the chemical solution for semiconductor manufacturing, which can suppress the increase in particles over time in the chemical solution and also suppress the occurrence of defects.

Means for Solving the Problems

[0008] As a result of intensive studies by the present inventors to achieve the above-described object, a chemical solution for semiconductor manufacturing contained in a container, the container contains a passivated austenitic stainless steel as a base material, the passivated surface is the inner surface of the container, the chemical solution for semiconductor manufacturing contains one or more metal components selected from the group consisting of V, Sn, and Pb, and an organic solvent, and the content of the metal component in the chemical solution for semiconductor manufacturing 30 days after filling the container is 0.1 mass ppt to 1 mass ppm. Based on this finding, the present invention has been completed.

[0009] That is, the present invention is as follows. <1> A chemical solution for semiconductor manufacturing contained in a container, wherein the container contains, as a base material, a passivated austenitic stainless steel, the passivated surface is the inner surface of the container, the chemical solution for semiconductor manufacturing contains one or more metal components selected from the group consisting of V, Sn, and Pb, and an organic solvent, and the content of the metal component in the chemical solution for semiconductor manufacturing 30 days after filling the container is 0.1 mass ppt to 1 mass ppm. A chemical solution for semiconductor manufacturing contained in a container. <2> The chemical solution for semiconductor manufacturing contains two or more metal components selected from the group consisting of V, Sn, and Pb, and the content of each of the two or more metal components in the chemical solution for semiconductor manufacturing 30 days after filling the container is 1 mass ppm or less, and the content of at least one of the two or more metal components in the chemical solution for semiconductor manufacturing 30 days after filling the container is 1 mass ppt or more. It is the chemical solution for semiconductor manufacturing contained in the container according to <1>. <3> The ratio (30 days after filling / at filling) of the concentration of the metal component in the container 30 days after filling the container to the concentration of the metal component in the container at the time of filling the container is 1 or more and 1.5 or less. It is the chemical solution for semiconductor manufacturing contained in the container according to <1> or <2>. <4> The chemical solution for semiconductor manufacturing contains, as the organic solvent, one or more selected from the group consisting of alkylene glycol monoalkyl ether, alkylene glycol monoalkyl ether acetate, cyclohexanone, cyclopentanone, 2-heptanone, γ-butyrolactone, ethyl lactate, butyl acetate, and 3-methoxybutyl acetate. It is the chemical solution for semiconductor manufacturing contained in the container according to any one of <1> to <3>. <5> The chemical solution for semiconductor manufacturing contains two or more of the organic solvents. It is the chemical solution for semiconductor manufacturing contained in the container according to any one of <1> to <4>. <6> The chemical solution for semiconductor manufacturing in a container according to any one of <1> to <5>, wherein the passivation treatment is a GEP treatment or a GEPW treatment. <7> The chemical solution for semiconductor manufacturing in a container according to any one of <1> to <6>, wherein the chemical solution for semiconductor manufacturing is a developer for semiconductor manufacturing or a rinse solution for semiconductor manufacturing. <8> A method for manufacturing a chemical solution for semiconductor manufacturing in a container, in which the chemical solution for semiconductor manufacturing is contained in a container, the method including: preparing a container containing, as a base material, passivated austenitic stainless steel and having an inner surface as a passivated surface; and filling the container with the chemical solution for semiconductor manufacturing, wherein the chemical solution for semiconductor manufacturing contains at least one metal component selected from the group consisting of V, Sn, and Pb and an organic solvent, and the content of the metal component in the chemical solution for semiconductor manufacturing 30 days after filling the container is 0.1 mass ppt to 1 mass ppm. <9> A method for storing a chemical solution for semiconductor manufacturing, the method including: preparing a container containing, as a base material, passivated austenitic stainless steel and having an inner surface as a passivated surface; and filling the container with the chemical solution for semiconductor manufacturing, wherein the chemical solution for semiconductor manufacturing contains at least one metal component selected from the group consisting of V, Sn, and Pb and an organic solvent, and the content of the metal component in the chemical solution for semiconductor manufacturing 30 days after filling the container is 0.1 mass ppt to 1 mass ppm.

Advantages of the Invention

[0010] According to the present invention, it is possible to provide a chemical solution for semiconductor manufacturing in a container, a method for manufacturing a chemical solution for semiconductor manufacturing in a container, and a method for storing a chemical solution for semiconductor manufacturing, which can suppress an increase in particles over time in the chemical solution and also suppress the occurrence of defects.

Embodiments for Carrying Out the Invention

[0011] Hereinafter, embodiments for carrying out the present invention (hereinafter simply referred to as "the present embodiment") will be described in detail. The following present embodiment is an exemplification for explaining the present invention and is not intended to limit the present invention to the following content. The present invention can be appropriately modified and implemented within the scope of its gist.

[0012] <Chemical solution for semiconductor manufacturing>

[0013] The chemical solution for semiconductor manufacturing according to the present embodiment (hereinafter sometimes simply abbreviated as "chemical solution") is a chemical solution for semiconductor manufacturing contained in a container. The container includes a passivated austenitic stainless steel as a base material, and the passivated surface is the inner surface of the container. The chemical solution for semiconductor manufacturing contains one or more metal components selected from the group consisting of V, Sn, and Pb and an organic solvent, and the content of the metal component in the chemical solution for semiconductor manufacturing 30 days after filling the container is 0.1 mass ppt to 1 mass ppm. It is a chemical solution for semiconductor manufacturing in a container. By using such a chemical solution, an increase in particles over time in the chemical solution can be suppressed, and the occurrence of defects can also be suppressed.

[0014] Conventionally, based on the finding that in order to suppress the occurrence of defects in a chemical solution for semiconductor manufacturing, it is better if there are fewer particles in the chemical solution, only a simple idea of removing fine particles that can become particles has been considered. However, the present inventors focused on the fact that simply reducing the concentration of fine particles may not be sufficient to suppress defects without remaining at such a simple idea.

[0015] As a result of intensive research by the present inventors, it has been surprisingly found that, with regard to chemical solutions for semiconductor manufacturing used in applications such as resist solutions, developing solutions, stripping solutions, cleaning solutions, pre-rinse solutions, rinse solutions, chemical mechanical polishing (CMP) slurries, etc., controlling the content of specific metal components (metal components) such as V, Sn, and Pb is effective in suppressing defects in semiconductor devices and the like. Furthermore, the present inventors have found that while storing the above chemical solutions with specific contents of metal components such as V, Sn, and Pb in conventionally widely used SUS containers, etc., over time as the storage period progresses, the content of various metals increases over time, which is also one of the reasons why defects cannot be sufficiently suppressed.

[0016] The chemical solution according to the present embodiment is based on the above findings, etc., and is a chemical solution for semiconductor manufacturing contained in a container. The container includes a passivated austenitic stainless steel as a base material, and the passivated surface is the inner surface of the container. The chemical solution for semiconductor manufacturing contains one or more metal components selected from the group consisting of V, Sn, and Pb and an organic solvent. By making it a chemical solution for semiconductor manufacturing contained in a container where the content of the metal component in the chemical solution for semiconductor manufacturing after 30 days from the time of container filling is 0.1 mass ppt to 1 mass ppm, surprisingly, an increase in particles over time in the chemical solution and the occurrence of defects can be suppressed, and the occurrence of defects that occur during the use of the chemical solution can also be suppressed to an extent that was not possible conventionally (however, the actions and effects of the present embodiment are not limited to the above-described content).

[0017] (Container)

[0018] The container contains a passivated austenitic stainless steel as the base material, and the passivated surface is the inner surface of the container. The austenitic stainless steel is not particularly limited, and examples thereof include SUS (Steel Use Stainless) 304 (Ni content: 8% by mass, Cr content: 18% by mass), SUS304L (Ni content: 9% by mass, Cr content: 18% by mass), SUS316 (Ni content: 10% by mass, Cr content: 16% by mass), SUS316L (Ni content: 12% by mass, Cr content: 16% by mass), etc.

[0019] Since the container of the present embodiment forms and / or grows a passive layer (sometimes called a passive film, a passivated film, etc.) by passivation treatment, elution of metal components into the chemical solution can be suppressed over a long period. Here, the passive layer does not include an oxide film or the like that is inevitably formed by an oxidation reaction with oxygen in the air, and exemplifies a passive layer intentionally formed by passivation treatment. From such a viewpoint, it is preferable that the passive layer is uniformly formed on the surface.

[0020] The method of passivation treatment is not particularly limited, but preferably a thermal oxidation treatment and / or an electrolytic polishing (EP: Electro Polishing) treatment, more preferably both a thermal oxidation treatment and an electrolytic polishing treatment, and even more preferably performing a thermal oxidation treatment after the electrolytic polishing treatment. By adopting these treatment methods, the passive layer can be formed more uniformly on the inner surface of the container, and pinholes in the barrier of the passive layer can be more effectively suppressed.

[0021] Furthermore, as the passivation treatment, it is preferably a GEP (Gold Electro Polishing) treatment or a GEPW (Gold Electro Polishing White) treatment.

[0022] In the case of GEP treatment, after electrolytic polishing treatment (EP treatment), thermal oxidation treatment is performed. By this, an iron oxide layer on the surface layer and a chromium oxide layer on the lower layer can be grown. As a result, unintentional elution of particles such as metal components into the chemical solution contained in the container can be more effectively suppressed.

[0023] In the case of GEPW treatment, after electrolytic polishing treatment (EP treatment), thermal oxidation treatment is carried out, and further, the grown chromium oxide layer is left by removing the iron oxide layer on the surface layer. As a result, unintentional elution of particles such as metal components into the chemical solution contained in the container can be more effectively suppressed.

[0024] Thus, GEP treatment and GEPW treatment can be performed as additional treatments for electrolytic polishing (EP), and a passive layer can be grown on the stainless steel as the base material. Furthermore, depending on the composition of the chemical solution, GEP treatment and GEPW treatment can be used separately. For example, when the chemical solution contains a large amount of alcohols or the like, GEP treatment is suitable, and when the chemical solution contains a large amount of amines or the like, GEPW treatment is suitable. Also, it would be possible to use GEP treatment and GEPW treatment separately according to the degree of dissolved oxygen content in the chemical solution (however, the actions and effects of this embodiment are not limited to these).

[0025] (Components of the chemical solution)

[0026] The chemical solution for semiconductor manufacturing contains one or more metal components selected from the group consisting of V, Sn, and Pb. V, Sn, and Pb may be present in the chemical solution as particles of the metal alone, or may be eluted as metal ions in the chemical solution.

[0027] The content of metal components in the chemical solution for semiconductor manufacturing is such that the content of metal components in the chemical solution for semiconductor manufacturing 30 days after container filling (which may be abbreviated as "content after passage") is 0.1 mass ppt to 1 mass ppm (1,000,000 mass ppt). The lower limit of the content of metal components is preferably 0.5 mass ppt or more, more preferably 2 mass ppt or more, still more preferably 5 mass ppt or more, and even more preferably 50 mass ppt or more. The upper limit of the content of metal components is preferably 500,000 mass ppt or less, more preferably 50,000 mass ppt or less, still more preferably 5,000 mass ppt or less, even more preferably 650 mass ppt or less, and even more preferably 500 mass ppt or less. By the content after passage of the metal components being within the above numerical range, the generation of defects can be more effectively suppressed. In addition, when containing two or more of V, Sn, and Pb as metal components, it is more preferable that the total content of the metal components is within the above range.

[0028] Furthermore, the content of metal components in the chemical solution for semiconductor manufacturing is preferably such that the content of metal components in the chemical solution for semiconductor manufacturing immediately after container filling (which may be abbreviated as "content after filling") is 0.1 mass ppt to 1 mass ppm (1,000,000 mass ppt). The lower limit of the content of metal components is preferably 0.5 mass ppt or more, more preferably 5 mass ppt or more, and still more preferably 50 mass ppt or more. The upper limit of the content of metal components is more preferably 500,000 mass ppt or less, still more preferably 50,000 mass ppt or less, even more preferably 5,000 mass ppt or less, still even more preferably 600 mass ppt or less, and yet even more preferably 500 mass ppt or less. By the content of metal components after the above-mentioned lapse of time being within the above numerical range, the content of metal components after the lapse of time can be controlled with higher precision so as to be within the above numerical range, and the occurrence of defects can be suppressed more effectively. In addition, when containing two or more of V, Sn, and Pb as metal components, it is more preferable that the total content of metal components is within the above range.

[0029] When the chemical solution for semiconductor manufacturing contains two or more metal components selected from the group consisting of V, Sn, and Pb, the content of each of the two or more metal components in the chemical solution for semiconductor manufacturing 30 days after container filling is preferably 1 mass ppm or less for each, and the content of at least one of the two or more metal components in the chemical solution for semiconductor manufacturing 30 days after container filling is preferably 1 mass ppt or more. Incidentally, the upper limit of the content of each of the two or more metal components in the chemical solution for semiconductor manufacturing 30 days after container filling is more preferably 900,000 mass ppt or less, still more preferably 100,000 mass ppt or less, even more preferably 500 mass ppt or less, and yet even more preferably 450 mass ppt or less. And the lower limit of this content is preferably greater than 0 mass ppt, more preferably 0.01 mass ppt or more, and still more preferably 0.1 mass ppt or more. Also, the upper limit of the content of at least one metal component among two or more metal components in the chemical solution for semiconductor manufacturing after 30 days have passed since the container was filled is preferably 900,000 mass ppt or less, more preferably 100,000 mass ppt or less, still more preferably 500 mass ppt or less, and even more preferably 450 mass ppt or less. And the lower limit of this content is preferably greater than 0 mass ppt, more preferably 0.01 mass ppt or more, still more preferably 0.1 mass ppt or more, and even more preferably 1 mass ppt or more.

[0030] According to this embodiment, as described above, since the increase in particles over time in the chemical solution can be suppressed, the increase in the concentration of the above-mentioned metal components in the container can be suppressed over a long period. As such a preferred example, for example, the ratio of the concentration of the metal component in the container 30 days after filling the container to the concentration of the metal component in the container at the time of filling the container (30 days after filling / at the time of filling) is 1 or more and 1.5 or less. The lower limit of this ratio of the concentration in the container is preferably 1.00 or more, and more preferably 1.05 or more. Also, the upper limit of this ratio is not particularly limited, but is preferably 10 or less, more preferably 5 or less, still more preferably 3 or less, even more preferably 2.5 or less, and even more preferably 1.5 or less. When the above ratio is within the above numerical range, it is possible to achieve both suppression of the increase in particles over time in the chemical solution due to the passage of the storage days and suppression of the occurrence of defects at a higher level.

[0031] The chemical solution for semiconductor manufacturing contains an organic solvent. The organic solvent is not particularly limited, but one or more selected from the group consisting of alcohol solvents, glycol ether solvents, glycol ester solvents, ketone solvents, lactone solvents, ester solvents, sulfonic acid solvents, amide solvents, and pyrrolidone solvents are preferred.

[0032] Specific examples of the alcohol-based solvents include, for example, aliphatic alcohols such as methanol, ethanol, denatured ethanol, isopropanol, n-propanol, n-butanol, 3-methoxy-3-methyl-1-butanol; glycols such as ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, glycerin, 1,3-propanediol, 1,3-butanediol, 1,4-butanediol, furfuryl alcohol, hexylene glycol, etc.

[0033] Specific examples of the glycol ether-based solvents include alkylene glycol monoalkyl ethers, alkylene glycol dialkyl ethers, high molecular type polyalkylene glycol ether-based solvents, and the like.

[0034] Examples of the alkylene glycol monoalkyl ethers include ethylene-based glycol monoalkyl ethers such as ethylene glycol monomethyl ether, diethylene glycol monomethyl ether, triethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monobutyl ether, triethylene glycol monobutyl ether, ethylene glycol monohexyl ether, diethylene glycol monohexyl ether; propylene-based glycol monoalkyl ethers such as propylene glycol monomethyl ether (PGME), propylene glycol monoethyl ether, propylene glycol monopropyl ether, propylene glycol monobutyl ether, dipropylene glycol monomethyl ether (DPM), dipropylene glycol monoethyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, tripropylene glycol monomethyl ether, tripropylene glycol monoethyl ether, tripropylene glycol monobutyl ether, etc.

[0035] Examples of the alkylene glycol dialkyl ether include ethylene glycol dialkyl ethers such as ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, ethylene glycol diethyl ether, ethylene glycol dibutyl ether, diethylene glycol dibutyl ether, triethylene glycol dibutyl ether, ethylene glycol dihexyl ether, and diethylene glycol dihexyl ether; propylene glycol dialkyl ethers such as propylene glycol dimethyl ether, propylene glycol diethyl ether, propylene glycol dipropyl ether, propylene glycol dibutyl ether, dipropylene glycol dimethyl ether, dipropylene glycol diethyl ether, dipropylene glycol dipropyl ether, dipropylene glycol dibutyl ether, tripropylene glycol dimethyl ether, tripropylene glycol diethyl ether, and tripropylene glycol dibutyl ether.

[0036] Examples of the polyalkylene glycol ether include polyalkylene glycol ethers such as polyoxypropylene butyl ether, polyoxyethylene polyoxypropylene butyl ether, polyoxyethylene oleyl ether, and polyoxyethylene polyoxypropylene-2-ethylhexyl ether.

[0037] Among these, ethylene glycol monoalkyl ethers, propylene glycol monoalkyl ethers, ethylene glycol dialkyl ethers, propylene glycol dialkyl ethers, etc. are preferable, and propylene glycol monomethyl ether (PGME) etc. are more preferable.

[0038] Specific examples of the glycol ester solvent include alkylene glycol monoalkyl ether acetate etc.

[0039] Examples of alkylene glycol monoalkyl ether acetates include ethylene glycol ether acetates such as ethylene glycol monobutyl ether acetate and diethylene glycol monobutyl ether acetate; propylene glycol ether acetates such as propylene glycol monomethyl ether acetate (PGMEA), dipropylene glycol monomethyl ether acetate, and propylene glycol diacetate.

[0040] Among these, ethylene glycol ether acetates and propylene glycol ether acetates are preferred, and propylene glycol monomethyl ether acetate (PGMEA) and the like are more preferred.

[0041] Specific examples of ketone solvents include acetone, methyl ethyl ketone (MEK), methyl isobutyl ketone (MIBK), diisobutyl ketone, cyclohexanone, cyclopentanone, diacetone alcohol, 1 - hexanone, 2 - hexanone, 4 - heptanone, 2 - heptanone, 1 - octanone, 2 - octanone, 1 - nonanone, 2 - nonanone, acetylacetone, acetonylacetone, phenylacetone, acetophenone, methylnaphthyl ketone, methylcyclohexanone, ionone, isophorone, propylene carbonate (propylene carbonate), diacetonyl alcohol, acetyl carbinol, and the like.

[0042] Among these, cyclohexanone, cyclopentanone, 2 - heptanone and the like are preferred.

[0043] Specific examples of lactone solvents include γ - butyrolactone, α - methyl - γ - butyrolactone, β - propiolactone, γ - valerolactone, δ - valerolactone, γ - caprolactone, ε - caprolactone, γ - laurolactone, hexanolactone, and the like.

[0044] Among these, γ - butyrolactone and the like are preferred.

[0045] Specific examples of the ester solvents include methyl acetate, ethyl acetate, butyl acetate, amyl acetate, propyl acetate, isopropyl acetate, methyl lactate, ethyl lactate, butyl lactate, ethyl methoxyacetate, ethyl ethoxyacetate, 2-methoxybutyl acetate, 3-methoxybutyl acetate, 4-methoxybutyl acetate, 3-methoxy-3-methylbutyl acetate, 3-ethyl-3-methoxybutyl acetate, 4-methyl-4-methoxypentyl acetate, methyl formate, ethyl formate, propyl formate, butyl formate, ethyl lactate, propyl lactate, butyl lactate, ethyl carbonate, propyl carbonate, butyl carbonate, methyl pyruvate, ethyl pyruvate, propyl pyruvate, butyl pyruvate, methyl acetoacetate, ethyl acetoacetate, methyl propionate, ethyl propionate, propyl propionate, isopropyl propionate, methyl 2-hydroxypropionate, ethyl 2-hydroxypropionate, methyl 3-methoxypropionate, ethyl 3-methoxypropionate, ethyl 3-ethoxypropionate, propyl 3-methoxypropionate, and the like.

[0046] Among these, ethyl acetate, butyl acetate, ethyl lactate, butyl lactate, 3-methoxybutyl acetate, and the like are preferred.

[0047] Specific examples of the sulfonic acid solvents include, for example, dimethyl sulfone, diethyl sulfone, tetramethylene sulfone, dipropyl sulfone, sulfolane (also known as tetramethylene sulfone), 3-methyl sulfolane, 2,4-dimethyl sulfolane, 3,4-dimethyl sulfolane, diphenyl sulfolane, 3,4-diphenylmethyl sulfolane, sulfolene, 3-methyl sulfolene, 3-ethyl sulfolene, and the like.

[0048] Specific examples of amide solvents include, for example, N,N-dimethylformamide (DMF), diethylformamide (DEF), N,N-dimethylacetamide (DMAc), N-methylpyrrolidine (MPD), hexamethylphosphoric triamide (HMPA), and the like.

[0049] Specific examples of pyrrolidone solvents include, for example, N-methylpyrrolidone (NMP), 2-pyrrolidone, N-vinyl-2-pyrrolidone, and the like.

[0050] Among the above, it is preferable to contain one or more selected from the group consisting of alcohol solvents, glycol ether solvents, glycol ester solvents, ketone solvents, lactone solvents, and ester solvents; more preferably, it contains one or more selected from the group consisting of alkylene glycol monoalkyl ethers, alkylene glycol monoalkyl ether acetates, cyclohexanone, cyclopentanone, 2-heptanone, γ-butyrolactone, ethyl lactate, butyl acetate, and 3-methoxybutyl acetate.

[0051] The chemical solution for semiconductor manufacturing may contain one kind of organic solvent or two or more kinds of organic solvents, but it is preferable to contain two or more kinds of organic solvents. As a preferred example when containing two or more kinds of organic solvents, two or more of the above-mentioned organic solvents can be selected. Further, as a preferable combination when containing two or more kinds of organic solvents, it is preferable to contain two or more selected from the group consisting of alcohol solvents, glycol ether solvents, glycol ester solvents, ketone solvents, lactone solvents, ester solvents, sulfonic acid solvents, amide solvents, and pyrrolidone solvents. As its preferred example, the above-mentioned preferred examples can be selected respectively.

[0052] As an example of a preferred combination when containing two or more organic solvents, for example, (i) at least one glycol ether solvent or glycol ester solvent, and (ii) one or more selected from the group consisting of alcohol solvents, glycol ether solvents, glycol ester solvents, ketone solvents, lactone solvents, and ester solvents are preferably contained; it is more preferable to contain at least (i) a glycol ether solvent and (ii) a glycol ester solvent.

[0053] The preferred content ratios of the above (i) and (ii) are preferably (i):(ii)=1:9 to 9:1 by volume ratio, more preferably 3:7 to 9:1, and even more preferably 5:5 to 9:1. For example, in the case of a mixed solvent containing two organic solvents where (i) is propylene glycol monomethyl ether (PGME) and (ii) is propylene glycol monomethyl ether acetate (PGMEA), the content ratio of PGME to PGMEA (PGME:PGMEA) is preferably 1:9 to 9:1 by volume ratio, more preferably 3:7 to 9:1, and even more preferably 5:5 to 9:1.

[0054] Alternatively, as another aspect, it is preferable to contain two or more selected from the group consisting of alkylene glycol monoalkyl ethers, alkylene glycol monoalkyl ether acetates, cyclohexanone, cyclopentanone, 2-heptanone, γ-butyrolactone, ethyl lactate, butyl acetate, and 3-methoxybutyl acetate, and it is more preferable to contain at least (a) one or more alkylene glycol monoalkyl ethers or alkylene glycol monoalkyl ether acetates, and (b) one or more selected from the group consisting of alkylene glycol monoalkyl ethers, alkylene glycol monoalkyl ether acetates, cyclohexanone, cyclopentanone, 2-heptanone, γ-butyrolactone, ethyl lactate, butyl acetate, and 3-methoxybutyl acetate.

[0055] The preferred content ratios of (a) and (b) described above are preferably (a):(b) = 1:9 to 9:1, more preferably 3:7 to 9:1, and even more preferably 5:5 to 9:1 in terms of volume ratio. For example, when the mixed solvent contains two organic solvents where (a) is propylene glycol monomethyl ether (PGME) and (b) is alkylene glycol monoalkyl ether propylene glycol monomethyl ether acetate (PGMEA), the content ratio of PGME to PGMEA (PGME:PGMEA) is preferably 1:9 to 9:1, more preferably 3:7 to 9:1, and even more preferably 5:5 to 9:1 in terms of volume ratio.

[0056] By using the combination of organic solvents as described above, it is possible to further achieve a high level of compatibility between the suppression of the increase in particles over time in the chemical solution and the suppression of the occurrence of defects.

[0057] The content of the organic solvent is preferably 90 to 100% by mass based on the total amount of the chemical solution. The lower limit is more preferably 95% by mass or more, and even more preferably 99% by mass or more. The upper limit is preferably less than 100% by mass.

[0058] The chemical solution according to this embodiment may contain water. Water may be added to the chemical solution, or may be mixed into the chemical solution unintentionally during the manufacturing process of the chemical solution. For example, when a water-soluble organic solvent is contained as the organic solvent, it can be expected to sufficiently suppress the increase in particles over time and the occurrence of defects in the chemical solution even when used in combination with water. The content of water may be included as the remainder of the components other than water. The content of water may be, for example, 0.001% to 2.0% by mass based on the total amount of the chemical solution. The lower limit may be 0.005% by mass or more, or 0.01% by mass or more. The upper limit may be 1.5% by mass or less, or 1.0% by mass or less. Note that the water content in the chemical solution can be measured by the Karl Fischer titration method.

[0059] The chemical solution according to this embodiment may further contain other components according to the intended use, as long as the effects of this embodiment can be obtained. For example, antioxidants (such as dibutylhydroxytoluene, etc.), acid generators, basic compounds, acid diffusion control agents, stabilizers, hydrophobic resins, surfactants, etc. can be mentioned. These can be appropriately selected from publicly known ones according to the intended use.

[0060] The chemical solution according to this embodiment can be used in various chemical solutions used in the manufacturing process of semiconductor devices. For example, it can be suitably used as a resist solution, developer, stripper, cleaning solution, pre-rinse solution, rinse solution, chemical mechanical polishing (CMP) slurry, etc. In particular, it can be more suitably used as a developer for semiconductor manufacturing or a rinse solution for semiconductor manufacturing (including the above-mentioned pre-rinse solution). Since these are applications where fine components other than the metal components of V, Sn, and Pb do not need to be added, the advantages of this embodiment, namely, the ability to suppress the increase in particles over time in the chemical solution and the occurrence of defects, can be particularly effectively utilized. In addition, there is also the advantage that the product life can be extended in terms of suppressing changes over time.

[0061] The chemical solution according to this embodiment can be used as a container for storing the chemical solution for semiconductor manufacturing stored in the above-described container. That is, it can be made into a container for a chemical solution for semiconductor manufacturing that includes the chemical solution for semiconductor manufacturing according to this embodiment and a container for storing the chemical solution for semiconductor manufacturing.

[0062] <Method for manufacturing a chemical solution for semiconductor manufacturing in a container>

[0063] As a preferred embodiment of the method for manufacturing a chemical solution for semiconductor manufacturing contained in a container, there is provided a method for manufacturing a chemical solution for semiconductor manufacturing contained in a container, the chemical solution for semiconductor manufacturing being contained in a container, the method including: a step of preparing a container containing, as a base material, a passivated austenitic stainless steel and having a passivated surface as an inner surface; and a step of filling the container with the chemical solution for semiconductor manufacturing. The chemical solution for semiconductor manufacturing contains at least one metal component selected from the group consisting of V, Sn, and Pb and an organic solvent, and the content of the metal component in the chemical solution for semiconductor manufacturing 30 days after filling the container is from 0.1 mass ppt to 1 mass ppm. Note that components to be blended in the chemical solution for semiconductor manufacturing may be appropriately selected from those described above. Also, numerical values such as content related to the chemical solution for semiconductor manufacturing may be appropriately selected from the conditions described above. The method for mixing the components is not particularly limited, and known methods can be appropriately employed. Further, if necessary, purification treatments such as a distillation step, a filtration step using a filter or the like, and a degassing step may be performed.

[0064] <Method for Storing Chemical Solution for Semiconductor Manufacturing>

[0065] As described above, according to the present embodiment, there is at least an advantage that an increase in particles over time in the chemical solution can be suppressed so that a sufficient effect of suppressing the generation of defects can be exhibited so that no defects occur when used for film formation or the like. From such a viewpoint, the present embodiment is suitable as a method for storing a chemical solution for semiconductor manufacturing.

[0066] As a preferred embodiment of the method for storing a chemical solution for semiconductor manufacturing according to the present embodiment, a step of preparing a container containing a passivated austenitic stainless steel as a base material and having a passivated surface as an inner surface, and a step of filling the container with the chemical solution for semiconductor manufacturing are included. The chemical solution for semiconductor manufacturing contains at least one metal component selected from the group consisting of V, Sn, and Pb and an organic solvent. The content of the metal component in the chemical solution for semiconductor manufacturing after 30 days from the time of container filling is 0.1 mass ppt to 1 mass ppm. A method for storing a chemical solution for semiconductor manufacturing is provided. During storage, known treatments such as filling the inside of the container with an inert gas such as nitrogen gas may be performed as necessary. The components of the chemical solution for semiconductor manufacturing may be appropriately selected from those described above. Also, the numerical values such as the content of the chemical solution for semiconductor manufacturing can be appropriately selected according to the above-described conditions.

[0067] As described above, according to the present embodiment, by controlling the content of trace metal components such as V, Sn, and Pb that cause the generation of defects, an increase in particles over time in the chemical solution can be suppressed, and the generation of defects can also be suppressed. A chemical solution for semiconductor manufacturing in a container, a method for manufacturing a chemical solution for semiconductor manufacturing in a container, and a method for storing a chemical solution for semiconductor manufacturing can be realized.

Examples

[0068] The present invention will be described in more detail with reference to the following examples and comparative examples, but the present invention is not limited to the following examples. Unless otherwise specified, the quantities are based on mass, and the experiments were conducted under conditions of 25°C and atmospheric pressure.

[0069] In the preparation of the chemical solution, unless otherwise specified, the handling of containers, the preparation of the chemical solution, the storage in containers, the storage, and the analytical measurement were carried out in a clean room. The operation of sampling the sample from the container was carried out in a clean room of ISO class 1000, and the other operations were carried out in a clean room of ISO class 5. Then, in order to improve the measurement accuracy, in the measurement of the content of metal components, when measuring components below the detection limit in normal measurement, the chemical solution was concentrated for measurement, and the content was calculated by converting it to the concentration of the solution before concentration.

[0070] <Organic solvent>

[0071] As the organic solvent of the chemical solution, the organic solvents listed in Table 1 were used. The abbreviations are as follows. ·PGMEA: Propylene glycol monomethyl ether acetate ·PGME: Propylene glycol monomethyl ether ·PGME / PGMEA(7:3): A mixture of PGME and PGMEA at a volume ratio of 7:3

[0072] <Purification>

[0073] The above organic solvents were purified by performing a filtration step using the filter shown in Table 1 after the distillation step shown below. The number of times the solution was passed through the filter in the filtration step was appropriately changed for purification. In the case of the mixture (PGME / PGMEA(7:3, volume ratio)), the organic solvents before mixing (each liquid) were individually distilled and then mixed at a predetermined ratio to form a mixture, and the mixture was filtered using a filter.

[0074] (Distillation step)

[0075] For commercially available organic solvents, a distillation treatment including dehydration was performed one or more times to prepare an organic solvent with reduced impurities. The water content in the organic solvent after distillation was all 100 ppm or less.

[0076] (Filtration step)

[0077] After the distillation process, filtration was performed using the following filters. Before use for filtration, 8 L of each organic solvent was passed through each filter under a pressure condition of 0.1 MPa to pre-wet the filter. The filters used in each example and each comparative example are shown in Table 1. In Comparative Example 2, filtration in the first stage was performed using Filter 1, and then filtration in the second stage was performed using Filter 2. · Filter 1: "Microgard(TM) UPE" (filter name), manufactured by Entegris, 1 nm (pore size) · Filter 2: "Purasol(TM) SP" (filter name), manufactured by Entegris, 200 nm (pore size) · Filter 3: "Microgard UPE" (filter name), manufactured by Entegris, 10 nm (pore size)

[0078]

Table 1

[0079] <Container> As the container for accommodating the chemical solution, a container whose wetted part is made of the following materials was used. · "GEP": Passivated austenitic stainless steel (as the passivation treatment, electrolytic polishing (EP) was performed and then thermal oxidation treatment (GEP treatment) was performed. That is, it is a container containing austenitic stainless steel with thermal oxidation treatment as the passivation treatment as the base material, and the passivated surface (thermal oxidation treatment surface) is the inner surface of the container. · "SUS": Austenitic stainless steel without passivation treatment (without passivation treatment, without thermal oxidation treatment, with electrolytic polishing). That is, it is a container containing austenitic stainless steel without passivation treatment as the base material, and that is the inner surface of the container.

[0080] <Measurement Conditions> [Content of Metal Components] The content of metal components in the chemical solution immediately after containing the chemical solution (meaning immediately after containing the chemical solution in the container and sealing the chemical solution), and after 30 days elapsed (stored for 30 days from filling), was measured using inductively coupled plasma mass spectrometry (ICP-MS, apparatus name "Agilent 8900 ICP-QQQ", manufactured by Agilent).

[0081] (Evaluation of the increase rate of particles in the solution)

[0082] The measured values (LPC values) of particles in the chemical solutions of the examples and comparative examples were measured using a particle counter in the solution ("KS-19F", manufactured by RION) at 25°C to measure the number of particles with a diameter of 30 nm or more (number per mL (particles / mL)). The LPC value (X) immediately after containing the chemical solution in the container and the LPC value (Y) after a predetermined number of days elapsed were measured respectively, and the increase rate (increase rate of particles in the solution) of the LPC value (Y / X) after a predetermined number of days elapsed with respect to the LPC value immediately after filling the chemical solution was calculated. When the shape of the particle is not circular, for example, in the case of an irregular shape, the above diameter was taken as the maximum major axis of the irregular shape.

[0083] Then, based on the following criteria, the increase rate of particles in the solution was evaluated. A: The increase rate of the number of particles was 500% or less. B: The increase rate of the number of particles exceeded 500% and was less than 1000%. C: The increase rate of the number of particles was 1000% or more.

[0084] (Evaluation of defect suppression)

[0085] Defect inspection of a 12-inch (diameter 300 mm) silicon wafer used for inspection was carried out using a dark field defect inspection apparatus ("Surfscan(TM) SP5", manufactured by KLA-Tencor). First, the number of defects (defect number) with a size of 17 nm or more in diameter existing on the surface of the silicon wafer was measured using a dark field defect inspection apparatus (this was taken as the "initial value"). Next, the above substrate was set in a spin ejection device, and while rotating the substrate at a rotational speed of 1000 rpm, 5 mL of the chemical solution contained in the container was ejected onto the surface of the substrate at a flow rate of 1 mL / s. After the ejection, the substrate was spin-dried. Subsequently, using a dark-field defect inspection device, the number of defects having a diameter of 17 nm or more present on the substrate after the chemical solution application was measured (this was defined as the "measurement value"). When the shape of the defect was not circular, for example, in the case of an irregular shape, the above diameter was taken as the maximum major axis of the irregular shape.

[0086] Then, by obtaining the difference between the "initial value" and the "measurement value" (measurement value - initial value), the number of generated defects was determined. And based on the following evaluation criteria, the defect suppression property was evaluated. The measurement area was the total surface area of the 12-inch (diameter 300 mm) silicon wafer used in the inspection, approximately 70650 mm 2 (=150 mm × 150 mm × 3.14), and the number of defects observed therein was counted. A: The number of defects within the measurement area was 100 or less. B: The number of defects within the measurement area was 101 or more and 500 or less. C: The number of defects within the measurement area was 501 or more and 1000 or less. D: The number of defects within the measurement area was 1001 or more.

[0087] The conditions and evaluation results of each example and each comparative example are shown in Table 2. Note that 1 mass ppm = 1,000,000 mass ppt.

[0088]

Table 2

[0089] From the above, it was at least confirmed that the chemical solution of this example has a low increase rate of in-liquid particles and is also excellent in defect suppression property.

Claims

1. A chemical solution for semiconductor manufacturing contained in a container, wherein the container contains, as a base material, a passivated austenitic stainless steel, and the passivated surface is the inner surface of the container, the chemical solution for semiconductor manufacturing contains one or more metal components selected from the group consisting of V, Sn, and Pb, and an organic solvent, the content of the metal component in the chemical solution for semiconductor manufacturing after 30 days from the time of container filling is from 0.1 mass ppt to 1 mass ppm, A chemical solution for semiconductor manufacturing contained in a container.

2. the chemical solution for semiconductor manufacturing contains two or more metal components selected from the group consisting of V, Sn, and Pb, after 30 days from the time of container filling, the content of each of the two or more metal components in the chemical solution for semiconductor manufacturing is 1 mass ppm or less, and after 30 days from the time of container filling, the content of at least one of the two or more metal components in the chemical solution for semiconductor manufacturing is 1 mass ppt or more, The chemical solution for semiconductor manufacturing contained in a container according to Claim 1.

3. The ratio (after 30 days from the time of filling / at the time of filling) of the concentration of the metal component in the container after 30 days from the time of filling the container to the concentration of the metal component in the container at the time of filling the container is 1 or more and 1.5 or less, The chemical solution for semiconductor manufacturing contained in a container according to Claim 1 or 2.

4. the chemical solution for semiconductor manufacturing contains, as the organic solvent, one or more selected from the group consisting of alkylene glycol monoalkyl ether, alkylene glycol monoalkyl ether acetate, cyclohexanone, cyclopentanone, 2-heptanone, γ-butyrolactone, ethyl lactate, butyl acetate, and 3-methoxybutyl acetate, The chemical solution for semiconductor manufacturing contained in a container according to Claim 1 or 2.

5. the chemical solution for semiconductor manufacturing contains two or more of the organic solvents, The chemical solution for semiconductor manufacturing contained in a container according to Claim 1 or 2.

6. the passivation treatment is a GEP treatment or a GEPW treatment, The chemical solution for semiconductor manufacturing contained in a container according to Claim 1 or 2.

7. the chemical solution for semiconductor manufacturing is a developing solution for semiconductor manufacturing or a rinsing solution for semiconductor manufacturing, The chemical solution for semiconductor manufacturing contained in a container according to Claim 1 or 2.

8. A method for manufacturing a chemical solution for semiconductor manufacturing contained in a container, in which the chemical solution for semiconductor manufacturing is contained in a container A step of preparing a container containing a passivated austenitic stainless steel as a base material and having a passivated surface as an inner surface; A step of filling the container with the chemical solution for semiconductor manufacturing, the method comprising: The chemical solution for semiconductor manufacturing contains one or more metal components selected from the group consisting of V, Sn, and Pb, and an organic solvent; The content of the metal component in the chemical solution for semiconductor manufacturing 30 days after filling the container is 0.1 mass ppt to 1 mass ppm; A method for manufacturing a chemical solution for semiconductor manufacturing in a container.

9. A step of preparing a container containing a passivated austenitic stainless steel as a base material and having a passivated surface as an inner surface; A step of filling the container with the chemical solution for semiconductor manufacturing, the method comprising: The chemical solution for semiconductor manufacturing contains one or more metal components selected from the group consisting of V, Sn, and Pb, and an organic solvent; The content of the metal component in the chemical solution for semiconductor manufacturing 30 days after filling the container is 0.1 mass ppt to 1 mass ppm; A method for storing a chemical solution for semiconductor manufacturing.

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