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WO2017018129A1 - Procédé de formation de câblage en couches - Google Patents

Procédé de formation de câblage en couches Download PDF

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Publication number
WO2017018129A1
WO2017018129A1 PCT/JP2016/069687 JP2016069687W WO2017018129A1 WO 2017018129 A1 WO2017018129 A1 WO 2017018129A1 JP 2016069687 W JP2016069687 W JP 2016069687W WO 2017018129 A1 WO2017018129 A1 WO 2017018129A1
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WIPO (PCT)
Prior art keywords
forming
surface region
conductive layer
group
radiation
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Ceased
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PCT/JP2016/069687
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English (en)
Japanese (ja)
Inventor
仁 浜口
健朗 田中
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JSR Corp
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JSR Corp
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Publication date
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Priority to JP2017531101A priority Critical patent/JP6799267B2/ja
Publication of WO2017018129A1 publication Critical patent/WO2017018129A1/fr
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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
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • 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
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/288—Deposition of conductive or insulating materials for electrodes conducting electric current from a liquid, e.g. electrolytic deposition
    • 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
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
    • 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
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/03—Use of materials for the substrate
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/40—Forming printed elements for providing electric connections to or between printed circuits

Definitions

  • the present invention relates to a method for forming a laminated wiring.
  • Photolithographic methods are widely used for forming wirings, electrodes and the like used for semiconductor elements and electronic circuits.
  • the photolithography method requires expensive equipment, and the process is complicated, resulting in an increase in manufacturing cost.
  • printed electronics that directly prints the wiring has attracted attention.
  • Each printing method such as ink jet printing, screen printing, and gravure printing used in printed electronics is a simple and low-cost method because a desired pattern of wiring can be directly formed on a substrate.
  • the ink material used flows as a result of these wetting spread and blurring, there is a limit in forming a fine wiring pattern.
  • the conventional general printing method it is not possible to form a laminated wiring in which wirings having a layer structure are connected by vias.
  • a method of forming a laminated wiring by a printing method using a material whose surface energy changes by applying energy has been proposed (see Japanese Patent Application Laid-Open No. 2015-15378).
  • a multilayer wiring is formed by the following steps. First, a wettability changing layer is formed on a substrate having a first wiring formed on the surface, using a material whose surface energy is changed by applying energy. This wettability changing layer becomes an interlayer insulating film. Next, a region having high wettability is formed by irradiating a part of the surface of the wettability changing layer with laser. This region with high wettability becomes a wiring pattern. Next, a via hole is formed by further irradiating a part of the formed region with high wettability with laser. After that, by applying a conductive ink on this highly wettable region, the second wiring and the via can be formed at the same time.
  • the above-described method performs high-energy laser irradiation to form a highly wettable region that becomes a wiring pattern, and it is difficult to say that the efficiency is good.
  • a laser for example, as the wiring pattern becomes complicated, the scanning path becomes complicated and the working time becomes longer.
  • a polymer having a side chain that contains polyimide in the main chain and can generate a hydrophilic group by irradiation with ultraviolet rays is used. Only.
  • the present invention has been made based on the above circumstances, and an object of the present invention is to provide a method for forming a multilayer wiring capable of efficiently forming a multilayer wiring.
  • the invention made in order to solve the above-described problems includes a step of preparing a base material having a first conductive layer as an outermost layer, an insulation having a liquid-repellent surface region and a lyophilic surface region on the surface of the base material.
  • a step of forming a film, and a step of forming a second conductive layer laminated on the lyophilic surface region of the insulating film by contacting the surface of the insulating film with the second conductive layer forming material An insulating film forming step of forming an insulating coating film having a liquid repellent surface with an insulating film forming composition comprising a first polymer having an acid dissociable group and a first acid generator; and It is a formation method of laminated wiring provided with the process of forming the above-mentioned lyophilic surface area in a part of surface area of an insulating coat.
  • an insulating film forming composition including a first polymer having an acid dissociable group and a first acid generator is used for forming an insulating film. For this reason, for example, in the region of the insulating coating that has been heated or irradiated with radiation, an acid is generated, and the acid dissociable group of the first polymer is dissociated by the generation of this acid, thereby changing the wettability. To do. Such heating and radiation irradiation can be performed without using a laser. Therefore, according to the formation method, a multilayer wiring can be formed efficiently.
  • the present invention can provide a method of forming a multilayer wiring that can efficiently form the multilayer wiring.
  • FIG. 1A is an explanatory diagram of the step (A-1) in the method for forming a multilayer wiring according to one embodiment of the present invention
  • FIG. 1B is an explanatory diagram of the step (A-2).
  • 1C is an explanatory diagram of the step (A-3)
  • FIG. 1D is an explanatory diagram of the step (A-4)
  • FIG. 1E is a schematic diagram of the step (A-3).
  • FIG. FIG. 2 (a) is an explanatory diagram of the step (B-1)
  • FIG. 2 (b) is an explanatory diagram of the step (B-2)
  • FIG. 2 (c) is an explanatory diagram of the step (B-3).
  • FIG. 6 is an explanatory diagram of (B-4).
  • FIG. 3 is an explanatory diagram of the step (C).
  • FIG. 4 is an image showing the substrate on which the first conductive layer in the example is formed.
  • FIG. 5 is an image showing a substrate on which a repellent pattern is formed on the second layer in the example.
  • FIG. 6 is an image showing the substrate on which the second conductive layer is formed in the example.
  • FIG. 7 is an enlarged image of the substrate on which the second conductive layer of FIG. 6 is formed.
  • FIG. 8 is an image showing the substrate on which the second conductive layer and the via conductor are formed in the example.
  • FIG. 9 is an SEM image showing the substrate on which the second conductive layer and the via conductor are formed in the example.
  • a method for forming a laminated wiring according to an embodiment of the present invention includes: Preparing a base material having the first conductive layer as the outermost layer (A), Step (B) of forming an insulating film on the surface of the base material, and Step (C) of forming a second conductive layer With The insulating film forming step (B) Step (B-1) for forming an insulating coating, and Step (B-2) for forming a lyophilic surface region Is provided.
  • the insulating film forming step (B) in the forming method includes: Step of forming via hole (B-3) It is preferable to comprise Heating the insulating coating film irradiated with radiation (B-4) It is also preferable to comprise.
  • preparation step (A) A step (A-1) of forming a base coating film, Step of forming lyophilic surface region (A-2) and step of forming first conductive layer (A-4)) It is preferable to provide.
  • the preparation step (A) in the formation method includes: Before the first conductive layer forming step (A-4), Heating the base coating film irradiated with radiation (A-3) It is preferable to provide.
  • the preparation step (A) in the forming method includes: After the first conductive layer forming step (A-4), A step of irradiating the entire surface on the side where the first conductive layer is formed (A-5) It is preferable to provide.
  • the formation method will be described in detail in order. Note that the order of the steps is not limited to the following order. The order of the steps may be different as long as a similar multilayer wiring can be formed, and a plurality of steps may be performed simultaneously.
  • the preparation step (A) is a step of preparing a base material having the first conductive layer as the outermost layer.
  • the preparation step (A) is preferably composed of the following steps (A-1) to (A-5).
  • the undercoat film forming step (A-1) is a step of forming an undercoat film having a liquid repellent surface with the undercoat film forming composition.
  • the composition for forming a base film includes a polymer having an acid dissociable group (second polymer) and an acid generator (second acid generator).
  • the acid dissociable group refers to a group in which a hydrogen atom in an acidic functional group such as a phenolic hydroxyl group, a carboxyl group, or a sulfonic acid group is substituted, and refers to a group that dissociates in the presence of an acid.
  • the composition for forming the base film will be described in detail later. Specifically, in the step (A-1), as shown in FIG. 1A, a base coating film 11 is formed by applying a base film forming composition to the surface of the substrate 10. The base coating film 11 finally becomes the base film 15 (see FIG. 1 (e)).
  • Examples of the material of the substrate 10 include glass, quartz, silicon, and resin.
  • Examples of the resin include polyethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate, polyethersulfone, polycarbonate, polyimide, and a ring-opening polymer (ROMP polymer) of cyclic olefin.
  • the substrate 10 is preferably a resin substrate, a glass substrate, or a semiconductor substrate conventionally used in electronic circuits. By using such a substrate, the obtained laminated wiring can be used as it is in an electronic circuit or the like.
  • the coating method of the undercoat film forming composition is not particularly limited, and is a coating method using a brush or brush, a dipping method, a spray method, a roll coating method, a spin coating method (spin coating method), a slit die coating method, Known methods such as a bar coating method, flexographic printing, offset printing, ink jet printing, and dispensing method can be used.
  • the undercoat film 11 is preferably heated (prebaked).
  • the heating conditions vary depending on the composition of the composition for forming a base film, but are, for example, about 60 ° C. to 120 ° C. and about 1 minute to 10 minutes.
  • the average thickness of the obtained base coating film 11 can be appropriately adjusted according to the use and the like, but the lower limit is preferably 0.05 ⁇ m, more preferably 0.1 ⁇ m. On the other hand, the upper limit is preferably 20 ⁇ m, and more preferably 10 ⁇ m.
  • irradiation (exposure) of radiation (h ⁇ ) to a part of the surface region of the base coating film 11 is performed. This is a step of forming the liquid surface region 12.
  • the surface of the base coating film 11 obtained from the base film forming composition has liquid repellency, and the region irradiated with radiation becomes the lyophilic surface region 12.
  • the region not irradiated with radiation is the liquid repellent surface region 13.
  • liquid repellency and lyophilicity are relative concepts.
  • the reason why the lyophilic surface region 12 is formed by irradiation with radiation is as follows.
  • an acid is generated from the radiation-sensitive acid generator in the undercoat film forming composition, whereby the acid-dissociable group of the polymer is dissociated. Due to the dissociation of the acid dissociable group, the surface energy of the irradiated region changes, and wettability increases. In particular, when the acid-dissociable group has a fluorine atom, the expression of this liquid repellency becomes remarkable.
  • the component derived from the dissociated acid dissociable group is preferably volatilized, the lyophilic surface region 12 becomes a recess (concave pattern). Since the lyophilic surface region 12 becomes a recess, as will be described later, the recess (lyophilic surface region 12) can be filled with the conductive layer forming material without bleeding.
  • Irradiation (exposure) of radiation can be performed through a photomask having a predetermined pattern so that the lyophilic surface region 12 having the same shape as the shape of the wiring to be formed is formed.
  • a photomask having a predetermined pattern so that the lyophilic surface region 12 having the same shape as the shape of the wiring to be formed is formed.
  • irradiation can be efficiently performed even when a complicated pattern is formed.
  • a predetermined pattern can be drawn and exposed using a direct drawing type exposure machine or the like.
  • the radiation irradiated in this step (A-2) visible light, ultraviolet light, far ultraviolet light, charged particle beam, X-ray or the like can be used.
  • radiation having a wavelength in the range of 190 nm to 450 nm is preferable, and radiation containing ultraviolet light having a wavelength of 365 nm is more preferable.
  • the exposure dose of radiation in this step (A-2) may be appropriately set within a range in which a sufficient change in wettability and formation of recesses can be formed.
  • the lower limit of the exposure amount is preferably 10 mJ / cm 2 and more preferably 20 mJ / cm 2 as the intensity of radiation at a wavelength of 365 nm.
  • this upper limit 1000 mJ / cm 2 is preferable, and 500 mJ / cm 2 is more preferable.
  • the size and shape of the lyophilic surface region 12 to be formed correspond to the desired size and shape of the wiring, but can be a linear shape having a width of 10 ⁇ m to 300 ⁇ m, for example.
  • the heating step (A-3) is a step of heating the base coating film 11 irradiated with radiation.
  • components dissociated in the region irradiated with radiation can be further volatilized.
  • the lyophilic surface region 12 (concave portion) becomes deeper (see FIG. 1C).
  • the wettability of the lyophilic surface region 12 is further increased by volatilization of the dissociated component.
  • the depth of the lyophilic surface region 12 can be, for example, 0.1 ⁇ m or more and 1 ⁇ m or less. Moreover, as a minimum of the depth of the lyophilic surface area
  • the heating method in this step is not particularly limited, and examples thereof include a method of heating using a hot plate, oven, dryer or the like. In addition, you may heat by vacuum baking.
  • the heating conditions are also appropriately set depending on the composition and film thickness of the composition for forming the base film, but are preferably 60 ° C. or higher and 150 ° C. or lower, and preferably 3 minutes or longer and 30 minutes or shorter.
  • the contact angle difference between the lyophilic surface region 12 thus formed and the liquid repellent surface region 13 with respect to tetradecane contact angle in the liquid repellent surface region 13 ⁇ contact angle in the lyophilic surface region 12.
  • 30 degrees is preferred, 40 degrees is more preferred, and 50 degrees is still more preferred.
  • the upper limit of the contact angle difference is, for example, 70 °.
  • the lower limit of the contact angle difference between water between the lyophilic surface region 12 and the lyophobic surface region 13 (contact angle in the lyophobic surface region 13 ⁇ contact angle in the lyophilic surface region 12) is 20 ° is preferred, and 25 degrees is more preferred.
  • the upper limit of this contact angle difference is, for example, 60 °.
  • the conductive layer forming material in contact with the liquid-repellent surface region 13 can easily move to the lyophilic surface region 12, and the lyophilic property. Wiring can be suitably formed along the surface region 12.
  • the first conductive layer forming step (A-4) is a step of forming the first conductive layer 14 by the contact of the first conductive layer forming material with the surface of the base coating film 11 irradiated with radiation (FIG. 1). (See (d)).
  • the material for forming the first conductive layer is not particularly limited.
  • any conductive material that can form wiring can be used, and examples include conductive film forming ink and conductive film forming paste.
  • first conductive layer forming materials include ink or paste in which metal particles are dispersed, ink or paste containing a metal salt and a reducing agent, and metal oxide particles that can be metallized by heating in a reducing atmosphere. And an ink or paste in which a conductive polymer is dispersed or a solution, an ink or paste in which nanocarbons such as carbon nanotubes and graphene are dispersed, and the like.
  • inks and pastes in which metal particles such as silver particles are dispersed, and inks and pastes containing metal salts and a reducing agent are preferable.
  • These inks or pastes can form a coating film by various printing methods and coating methods. In addition, such a coating film of the first conductive layer forming material is heated to become the first conductive layer 14 (wiring).
  • the contact of the first conductive layer forming material with the surface of the base coating film 11 can be performed by a known method such as coating.
  • a known method such as coating.
  • application method using brush or brush, dipping method, spray method, roll coating method, spin coating method (spin coating method), slit die coating method, bar coating method, flexographic printing, offset printing, inkjet Well-known methods, such as printing and a dispensing method can be mentioned.
  • a dipping method, a spray method, a spin coating method, a slit die coating method, an offset printing method, an ink jet method, and a dispensing method are preferable.
  • a lyophilic surface region 12 and a liquid repellent surface region 13 are formed on the surface of the base coating film 11. For this reason, when the first conductive layer forming material is brought into contact with the surface of the base coating film 11, the first conductive layer forming material is repelled in the liquid repellent surface region 13 and is preferably lyophilic, which is a recess. It flows into the surface region 12. Thereby, the first conductive layer forming material is disposed along the lyophilic surface region 12 which is a recess.
  • the radiation irradiating step (A-5) is a step of irradiating the entire surface of the surface on which the first conductive layer forming material is applied, that is, the side on which the first conductive layer 14 is formed, with radiation (h ⁇ ).
  • the radiation irradiating step (A-5) is a step of irradiating the entire surface of the surface on which the first conductive layer forming material is applied, that is, the side on which the first conductive layer 14 is formed, with radiation (h ⁇ ).
  • Specific examples and preferred examples of radiation irradiated in this step are the same as those in the lyophilic surface region forming step (A-2). Further, the radiation exposure amount in this step can be the same as in the lyophilic surface region forming step (A-2).
  • the base coating film 11 and the like it is preferable to heat the base coating film 11 and the like after irradiation of radiation to the entire surface.
  • the component derived from the acid dissociable group dissociated in the exposed portion (exposed portion) is volatilized, and the exposed portion becomes thinner and more lyophilic.
  • the first conductive layer forming material (first conductive layer 14) is sufficiently cured by this heating.
  • the base coating film 11 becomes the base film 15, and the base material 16 having the first conductive layer 14 (wiring) as the outermost layer can be obtained (see FIG. 1E).
  • This heating method is not particularly limited, and examples thereof include a method of heating using a hot plate, oven, dryer or the like. In addition, you may heat by vacuum baking.
  • the heating conditions are not particularly limited, but may be, for example, 50 ° C. or higher and 200 ° C. or lower and 1 minute or longer and 120 minutes or shorter. However, since it is not necessary to make the undercoat film 15 (the undercoat film 11) thin, the heating conditions may be milder than in the heating step (A-3).
  • ⁇ Insulating film forming step (B)> an insulating film 23 having a lyophobic surface region 19 and a lyophilic surface region 18 provided with via holes 20 is formed on the surface of the substrate 16. It is a process (see FIG. 2C). In FIG. 2C and the like, the via hole 20 is formed in the lyophilic surface region 18 of the insulating film 23, but the via hole 20 may not be formed.
  • the insulating coating film forming step (B-1) is a step of forming the insulating coating film 17 having a liquid-repellent surface with the insulating film forming composition.
  • the composition for forming an insulating film includes a polymer having an acid dissociable group (first polymer) and an acid generator (first acid generator). This insulating film forming composition will be described in detail later.
  • the insulating film forming composition is applied to the surface of the base material 16 on the side where the first conductive layer 14 is formed.
  • the insulating coating film 17 is formed by application.
  • the insulating coating film 17 finally becomes the insulating film 23.
  • the coating method of the insulating film forming composition is the same as the coating method of the base film forming composition in step (A-1) described above.
  • the insulating coating film 17 is preferably heated (pre-baked).
  • the heating condition varies depending on the composition of the composition for forming an insulating film, and is, for example, about 60 ° C. to 120 ° C. and about 1 minute to 10 minutes.
  • the average thickness of the insulating coating 17 to be obtained can be appropriately adjusted according to the use etc., but the lower limit is preferably 0.05 ⁇ m, more preferably 0.1 ⁇ m. On the other hand, the upper limit is preferably 20 ⁇ m, and more preferably 10 ⁇ m.
  • the lyophilic surface region forming step (B-2) is a step of forming a lyophilic surface region by irradiating a part of the surface region of the insulating coating film 17 with radiation (h ⁇ ) (FIG. 2B). )reference). Similar to the base coating film 11 obtained from the base film forming composition, the surface of the insulating coating film 17 has liquid repellency, and the region irradiated with radiation becomes the lyophilic surface region 18. On the other hand, the region not irradiated with radiation is the liquid repellent surface region 19. Moreover, like the base coating film 11, the lyophilic surface region 18 becomes a recess (concave pattern).
  • the radiation irradiation (exposure) method, the type of radiation, specific examples of the exposure dose, and preferred examples are the same as those in the lyophilic surface region forming step (A-2). That is, it is preferable that the irradiation of radiation is performed by exposure through a photomask. Further, the shape and the like of the lyophilic surface region 18 formed can be the same as that of the lyophilic surface region 12 formed in the step (A-2).
  • the via hole forming step (B-3) is a step of forming the via hole 20 (see FIG. 2C).
  • the method for forming the via hole 20 is not particularly limited, but it can be preferably performed by laser irradiation to a part of the lyophilic surface region 18 of the insulating coating film 17. By such laser ablation, a via hole 20 for connecting the first conductive layer 14 and the second conductive layer 21 (see FIG. 3) is formed.
  • the via hole 20 penetrates the insulating coating film 17.
  • the via hole 20 may be formed by a method other than laser ablation.
  • the via hole 20 may be formed by irradiation with a sufficient amount of radiation through a photomask.
  • the wavelength of the laser used in this step (B-3) is not particularly limited, but it is preferable to use radiation (ultraviolet rays) in the range of 190 nm to 450 nm.
  • radiation ultraviolet rays
  • ArF (193 nm) ArF (193 nm), and the like.
  • the size of the via hole 20 to be formed is not particularly limited, but is usually narrower than the width of the linear lyophilic surface region 18.
  • the specific size of the via hole 20 can be, for example, about 1 ⁇ m to 100 ⁇ m.
  • the size of the via hole 20 means the diameter when the opening of the via hole 20 is circular, and the length of one side (long side) when the opening is square.
  • the heating step (B-4) is a step of heating the insulating coating film 17 irradiated with radiation.
  • the dissociated component in the region irradiated with radiation can be further volatilized.
  • the lyophilic surface region 18 (concave portion) is further deepened.
  • the wettability of the lyophilic surface region 18 is further increased by volatilization of the dissociated component.
  • the heating step (B-4) may be performed before the via hole forming step (B-3) as long as it is after the lyophilic surface region forming step (B-2). It may be performed after the hole forming step (B-3). However, the heating step (B-4) is preferably performed before the via hole forming step (B-3). By thinning the lyophilic surface region 18 through the heating step (B-4) and then performing laser ablation, the via hole 20 can be formed efficiently and accurately.
  • ⁇ Second conductive layer forming step (C)> In the second conductive layer forming step (C), the second conductive layer 21 (wiring) laminated on the lyophilic surface region 18 of the insulating film 23 by the contact of the second conductive layer forming material with the surface of the insulating film 23. ). At this time, via conductors 22 that connect the first conductive layer 14 and the second conductive layer 21 are formed together with the second conductive layer 21 by the second conductive layer forming material.
  • Specific examples and preferred examples of the second conductive layer forming material are the same as those of the first conductive layer forming material described above.
  • the contact method of the second conductive layer forming material to the surface of the insulating film 23 is the same as that of the first conductive layer forming material in the first conductive layer forming step (A-4).
  • the second conductive layer forming material is brought into contact with the surface of the insulating film 23, the second conductive layer forming material is repelled in the liquid repellent surface region 19 and preferably in the lyophilic surface region 18 which is a recess. Flows in.
  • the second conductive layer forming material is disposed along the lyophilic surface region 18. Further, the second conductive layer forming material that has flowed into the lyophilic surface region 18 is filled in the via holes 20 formed in the lyophilic surface region 18.
  • the second conductive layer forming material After the contact (application) of the second conductive layer forming material, the second conductive layer forming material is heated together with the substrate 10 and the like. By this heating, the second conductive layer forming material is cured, and the second conductive layer 21 and the via conductor 22 are formed.
  • Examples of the heating method include heating using a hot plate, an oven, a dryer, etc., and vacuum baking.
  • the heating conditions are not particularly limited, but may be, for example, 50 ° C. or higher and 200 ° C. or lower and 1 minute or longer and 120 minutes or shorter.
  • a laminated wiring 24 that is a laminated body of the wiring including the first conductive layer 14 and the second conductive layer 21 can be obtained.
  • a wettability pattern (lyophilic surface region 12 and lyophilic surface region 18) can be formed by exposure through a photomask or the like without using a laser.
  • the laminated wiring 24 can be formed efficiently.
  • composition for forming a base film and the composition for forming an insulating film (hereinafter, both compositions are collectively referred to as “film forming composition”) will be described in detail.
  • the composition for forming the base film and the composition for forming the insulating film may have different compositions or the same composition, but are preferably the same composition. Since these are the same composition, laminated wiring can be manufactured efficiently.
  • the film-forming composition comprises a polymer having an acid-dissociable group (hereinafter also referred to as “polymer (A)”), and an acid generator (hereinafter referred to as “acid generator (B)”). Also called).
  • the film-forming composition usually contains a solvent (C), and other suitable components include a sensitizer (D), a quencher (E), a polymerizable compound (F), and radiation-sensitive polymerization initiation.
  • An agent (G) can be contained.
  • the polymer (A) is not particularly limited as long as it is a polymer having an acid dissociable group, but is usually a polymer having a structural unit (I) having this acid dissociable group.
  • This structural unit (I) is preferably a structure containing either an acetal bond or a hemiacetal ester bond.
  • the structural unit (I) containing an acid dissociable group more preferably contains a group represented by the following formula (5-1) or (5-2).
  • R 4 and R 5 are each independently a hydrogen atom or a methyl group.
  • Rf is independently an organic group having a fluorine atom. * Represents a binding site.
  • —C (R 1 ) (R 2 ) ORf is an acid dissociable group.
  • the acid dissociable group is efficiently dissociated in the exposed portion of the coating film, and the surface energy is increased.
  • the acid-dissociable group contains a fluorine atom as described above, the change in the surface energy of the film before and after the dissociation of the acid-dissociable group, that is, the wettability is increased.
  • Rf is preferably a hydrocarbon group in which one or more hydrogen atoms are substituted with a fluorine atom, and a group having an oxygen atom between the carbon-carbon bonds of such a hydrocarbon group.
  • a more preferred group of Rf includes a group represented by — (R 2 —O) n —R 3 in formulas (1) to (4) described later.
  • the structural unit (I) is preferably a structural unit represented by any one of the following formulas (1) to (4).
  • the structural unit (I) may be composed of only one type of structural unit or may include a plurality of types of structural units.
  • each R 1 is independently a hydrogen atom or a methyl group.
  • R 2 each independently represents a methylene group, an alkylene group having 2 to 12 carbon atoms, an alkenylene group having 2 to 12 carbon atoms, a divalent aromatic hydrocarbon group having 6 to 12 carbon atoms, or 4 to 12 carbon atoms. A divalent alicyclic hydrocarbon group, or a group in which one or more hydrogen atoms of these groups are substituted with a substituent.
  • R 3 is each independently a hydrocarbon group in which one or more hydrogen atoms are substituted with fluorine atoms.
  • Each m is independently 0 or 1.
  • n is each independently an integer of 0 to 12.
  • Examples of the alkylene group having 2 to 12 carbon atoms represented by R 2 include an ethylene group, a propylene group, and a butylene group.
  • Examples of the alkenylene group having 2 to 12 carbon atoms represented by R 2 include a vinylene group and an ethene-1,2-diyl group.
  • Examples of the divalent aromatic hydrocarbon group having 6 to 12 carbon atoms represented by R 2 include a phenylene group, a tolylene group, a naphthylene group, and a biphenylene group.
  • Examples of the divalent alicyclic hydrocarbon group having 4 to 12 carbon atoms represented by R 2 include a cyclobutanediyl group and a cyclohexanediyl group.
  • substituent for substituting the hydrogen atom of these groups include a halogen atom such as a fluorine atom and a hydroxy group.
  • R 2 is preferably a methylene group, an alkylene group or an aromatic hydrocarbon group, more preferably a methylene group, an ethylene group, a propylene group, a butylene group, a phenylene group or a biphenylene group.
  • Examples of the hydrocarbon group in which one or more hydrogen atoms represented by R 3 are substituted with a fluorine atom include a fluorine-substituted aliphatic hydrocarbon group and a fluorine-substituted aromatic hydrocarbon group. Fluorine-substituted aliphatic hydrocarbon groups are preferred.
  • the lower limit of the number of carbon atoms of the fluorine-substituted hydrocarbon group is preferably 3, and more preferably 4.
  • the upper limit is preferably 30, more preferably 20, and even more preferably 15.
  • the lower limit of the fluorine number of the fluorine-substituted hydrocarbon group is preferably 5 and more preferably 10.
  • the upper limit can be set to 30, for example.
  • fluorine-substituted hydrocarbon group represented by R 3 include groups represented by the following formulas (Rf-1) to (Rf-33).
  • N is an integer from 0 to 12, but the upper limit is preferably 8, preferably 4 and more preferably 2.
  • n is particularly preferably 0.
  • the upper limit may be 100% by mass, or 80% by mass.
  • the polymer (A) can have a structural unit other than the structural unit (I).
  • Other structural units specifically include (meth) acrylic acid chain alkyl ester, (meth) acrylic acid cyclic alkyl ester, (meth) acrylic acid aryl ester, unsaturated aromatic compound, conjugated diene, tetrahydro, which will be described later.
  • Examples include structural units derived from unsaturated compounds having a skeleton, maleimides, other monomers, and the like.
  • the polymer (A) is (1) a method of reacting a compound (a) represented by the following formula (a) with a polymer having a hydroxyl group or a carboxy group as a precursor, and (2) a compound (a). It can be obtained by, for example, a method of polymerizing a monomer obtained by use.
  • R 1 - R 3 and n are the above formula (1) the same meaning as R 1 - R 3 and n in - (4).
  • Examples of the monomer having a hydroxyl group include (meth) acrylic acid ester having a hydroxyl group. Specifically, 2-hydroxyethyl methacrylate, 2-hydroxypropyl methacrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxybutyl methacrylate, 2-hydroxybutyl acrylate, 2-hydroxy-3-phenoxypropyl acrylate 2-acryloyloxyethyl-2-hydroxylethylphthalic acid, dipropylene glycol methacrylate, dipropylene glycol acrylate, 4-hydroxybutyl methacrylate, 4-hydroxybutyl acrylate, cyclohexanedimethanol monoacrylate, cyclohexanedimethanol monomethacrylate, ethyl ⁇ - (Hydroxymethyl) acrylate, polypropylene glycol monomethacrylate, polyp Pyrene glycol monoacrylate, glycerin monomethacrylate, glycerin mono
  • Examples of the monomer having a carboxy group include acrylic acid, methacrylic acid, 2-acryloyloxyethyl succinic acid, 2-methacryloyloxyethyl succinic acid, 2-acryloyloxyethyl phthalic acid, 2-methacryloyloxyethyl phthalic acid, and 2-acryloyloxy.
  • Ethyltetrahydrophthalic acid 2-methacryloyloxyethyltetrahydrophthalic acid, 2-acryloyloxyethylhexahydrophthalic acid, 2-methacryloyloxyethylhexahydrophthalic acid, 2-acryloyloxypropylphthalic acid, 2-methacryloyloxypropylphthalic acid, 2-acryloyloxypropyltetrahydrophthalic acid, 2-methacryloyloxypropyltetrahydrophthalic acid, 2-acryloyloxypropylhexahydrophthalic acid, - it can be exemplified methacryloyloxypropyl hexahydrophthalic acid.
  • the polymer having a hydroxyl group or a carboxy group can be obtained by using only the monomer having a hydroxyl group or a carboxy group as described above, or a monomer other than the monomer having a hydroxyl group or a carboxy group and a monomer having a hydroxyl group or a carboxy group. It can be obtained by copolymerizing with a monomer.
  • Examples of the monomer other than the monomer having a hydroxyl group or a carboxy group include (meth) acrylic acid chain alkyl ester, (meth) acrylic acid cyclic alkyl ester, (meth) acrylic acid aryl ester, unsaturated aromatic compound, conjugated diene, tetrahydrofuran Examples thereof include unsaturated compounds containing a skeleton, maleimides, and other monomers.
  • Examples of the (meth) acrylic acid chain alkyl ester include methyl methacrylate, ethyl methacrylate, n-butyl methacrylate, sec-butyl methacrylate, t-butyl methacrylate, 2-ethylhexyl methacrylate, isodecyl methacrylate, methacrylic acid.
  • N-lauryl acid tridecyl methacrylate, n-stearyl methacrylate, methyl acrylate, ethyl acrylate, n-butyl acrylate, sec-butyl acrylate, t-butyl acrylate, 2-ethylhexyl acrylate, isodecyl acrylate And n-lauryl acrylate, tridecyl acrylate, and n-stearyl acrylate.
  • Examples of (meth) acrylic acid cyclic alkyl esters include cyclohexyl methacrylate, 2-methylcyclohexyl methacrylate, tricyclo [5.2.1.0 2,6 ] decan-8-yl methacrylate, isobornyl methacrylate, cyclohexyl acrylate. 2-methylcyclohexyl acrylate, tricyclo [5.2.1.0 2,6 ] decan-8-yl acrylate, isobornyl acrylate, and the like.
  • (meth) acrylic acid aryl esters examples include phenyl methacrylate, benzyl methacrylate, phenyl acrylate, and benzyl acrylate.
  • Examples of the unsaturated aromatic compound include styrene, ⁇ -methylstyrene, o-methylstyrene, m-methylstyrene, p-methylstyrene, p-methoxystyrene and the like.
  • conjugated diene examples include 1,3-butadiene, isoprene, 2,3-dimethyl-1,3-butadiene and the like.
  • Examples of the unsaturated compound containing a tetrahydrofuran skeleton include tetrahydrofurfuryl (meth) acrylate, 2-methacryloyloxy-propionic acid tetrahydrofurfuryl ester, 3- (meth) acryloyloxytetrahydrofuran-2-one, and the like. .
  • maleimide examples include N-phenylmaleimide, N-cyclohexylmaleimide, N-tolylmaleimide, N-naphthylmaleimide, N-ethylmaleimide, N-hexylmaleimide, N-benzylmaleimide and the like.
  • Examples of other monomers include (meth) acrylic acid ester having an epoxy group (cyclic ether group). Specifically, glycidyl methacrylate, 3,4-epoxycyclohexyl methacrylate, 3,4-epoxycyclohexyl acrylate, 3- (methacryloyloxymethyl) -3-ethyloxetane, 3- (acryloyloxymethyl) -3- Examples include ethyl oxetane, tricyclo [5.2.1.0 2,6 ] decan-8-yloxyethyl methacrylate, tricyclo [5.2.1.0 2,6 ] decan-8-yloxyethyl acrylate, and the like. be able to.
  • Examples of the solvent used in the polymerization reaction for synthesizing a polymer having a hydroxyl group or a carboxy group include glycol ether, ethylene glycol alkyl ether acetate, diethylene glycol monoalkyl ether, diethylene glycol dialkyl ether, dipropylene glycol dialkyl ether, propylene glycol mono Examples include alkyl ether, propylene glycol alkyl ether acetate, propylene glycol monoalkyl ether propionate and the like. Other alcohols, ethers, ketones, esters and the like can also be used.
  • a molecular weight modifier can be used to adjust the molecular weight.
  • molecular weight modifiers include halogenated hydrocarbons such as chloroform and carbon tetrabromide; mercaptans such as n-hexyl mercaptan, n-octyl mercaptan, n-dodecyl mercaptan, t-dodecyl mercaptan, and thioglycolic acid; Xanthogens such as xanthogen sulfide and diisopropylxanthogen disulfide; terpinolene, ⁇ -methylstyrene dimer and the like can be mentioned.
  • polystyrene conversion weight average molecular weight (Mw) by gel permeation chromatography (GPC) of a polymer which has a hydroxyl group or a carboxy group 1000 is preferred and 5000 is more preferred. On the other hand, as this upper limit, 50000 is preferable and 30000 is more preferable.
  • An acetal bond is formed by the hydroxyl group of the polymer having a hydroxyl group and the vinyl ether group of the compound (a), and the carboxy group of the polymer having a carboxy group and the vinyl ether group of the compound (a)
  • a hemiacetal ester bond is formed to form the polymer (A).
  • a polymer having a hydroxyl group or a carboxy group is dissolved in an organic solvent, and then an equimolar or excess amount of the compound (a) is added to the hydroxyl group or carboxy group of the polymer. .
  • an acid eg, oxalic acid
  • the target polymer (A) can be obtained by removing the organic solvent.
  • an acetal bond is formed by the hydroxyl group of the polymerizable compound having a hydroxyl group and the vinyl ether group of the vinyl ether compound (compound (a)), or the carboxy group of the polymerizable compound having a carboxy group.
  • a hemiacetal ester bond is formed by the group and the vinyl ether group of the vinyl ether compound (compound (a)) to obtain a desired monomer.
  • the polymer (A) can be obtained by polymerizing the obtained monomer in the same manner as in the method for producing a polymer having a hydroxyl group or a carboxy group.
  • the acid generator (B) has a function of generating an acid in response to, for example, heating or radiation.
  • the acid generator (B) is preferably a radiation-sensitive acid generator.
  • the acid generator (B) may be contained in the form of a compound as a so-called acid generator, or may be incorporated in a part of the polymer such as the polymer (A). When the composition for film formation contains the acid generator (B), the acid dissociable group can be eliminated from the polymer (A).
  • Examples of the acid generator that is a radiation-sensitive acid generator include oxime sulfonate compounds, onium salts, sulfonimide compounds, halogen-containing compounds, diazomethane compounds, sulfone compounds, sulfonic acid ester compounds, and carboxylic acid ester compounds. it can. You may use an acid generator individually or in combination of 2 or more types. These radiation-sensitive acid generators may function as a heat-sensitive acid generator.
  • oxime sulfonate compound As said oxime sulfonate compound, the compound containing the oxime sulfonate group represented by following formula (6) is preferable.
  • R 11 is an alkyl group having 1 to 12 carbon atoms, a fluoroalkyl group having 1 to 12 carbon atoms, an alicyclic hydrocarbon group having 4 to 12 carbon atoms, or an aryl having 6 to 20 carbon atoms. Or a group in which some or all of the hydrogen atoms of the alkyl group, alicyclic hydrocarbon group and aryl group are substituted with a substituent.
  • alkyl group, alicyclic hydrocarbon group, and aryl group may have include an alkoxy group having 1 to 10 carbon atoms, a hydroxyl group, and a halogen atom.
  • Examples of the compound containing an oxime sulfonate group represented by the above formula (6) include oxime sulfonate compounds represented by the following formulas (6-1) to (6-3).
  • R 11 has the same meaning as R 11 in the formula (6).
  • R 15 is an alkyl group having 1 to 12 carbon atoms or a fluoroalkyl group having 1 to 12 carbon atoms.
  • X is an alkyl group, an alkoxy group, or a halogen atom.
  • m is an integer of 0 to 3. However, when there are a plurality of Xs, the plurality of Xs may be the same or different.
  • Examples of the oxime sulfonate compound represented by the above formula (6-3) include compounds represented by the following formulas (6-3-1) to (6-3-5).
  • the compounds represented by the above formulas (6-3-1) to (6-3-5) are sequentially (5-propylsulfonyloxyimino-5H-thiophen-2-ylidene)-(2-methylphenyl) acetonitrile, (5-octylsulfonyloxyimino-5H-thiophen-2-ylidene)-(2-methylphenyl) acetonitrile, (camphorsulfonyloxyimino-5H-thiophen-2-ylidene)-(2-methylphenyl) acetonitrile, (5 -P-toluenesulfonyloxyimino-5H-thiophen-2-ylidene)-(2-methylphenyl) acetonitrile and (5-octylsulfonyloxyimino)-(4-methoxyphenyl) acetonitrile.
  • Examples of other compounds containing the oxime sulfonate group represented by the above formula (6) include (5-octylsulfonyloxyimino)-(4-methoxyphenyl) acetonitrile.
  • onium salt examples include diphenyliodonium salt, triphenylsulfonium salt, alkylsulfonium salt, benzylsulfonium salt, dibenzylsulfonium salt, substituted benzylsulfonium salt, benzothiazonium salt, and tetrahydrothiophenium salt. it can.
  • diphenyliodonium salt examples include diphenyliodonium tetrafluoroborate, diphenyliodonium hexafluorophosphonate, diphenyliodonium hexafluoroarsenate, diphenyliodonium trifluoromethanesulfonate, diphenyliodonium trifluoroacetate, diphenyliodonium-p-toluenesulfonate, diphenyl Iodonium butyltris (2,6-difluorophenyl) borate, 4-methoxyphenylphenyliodonium tetrafluoroborate, bis (4-t-butylphenyl) iodonium tetrafluoroborate, bis (4-t-butylphenyl) iodonium hexafluoroarce Bis (4-tert-butylphenyl) iodonium triflate Romethanesulf
  • triphenylsulfonium salt examples include triphenylsulfonium trifluoromethanesulfonate, triphenylsulfonium camphorsulfonic acid, triphenylsulfonium tetrafluoroborate, triphenylsulfonium trifluoroacetate, triphenylsulfonium-p-toluenesulfonate, and triphenyl. And sulfonium butyl tris (2,6-difluorophenyl) borate.
  • alkylsulfonium salt examples include 4-acetoxyphenyldimethylsulfonium hexafluoroantimonate, 4-acetoxyphenyldimethylsulfonium hexafluoroarsenate, dimethyl-4- (benzyloxycarbonyloxy) phenylsulfonium hexafluoroantimonate, dimethyl-4 -(Benzoyloxy) phenylsulfonium hexafluoroantimonate, dimethyl-4- (benzoyloxy) phenylsulfonium hexafluoroarsenate, dimethyl-3-chloro-4-acetoxyphenylsulfonium hexafluoroantimonate, and the like.
  • benzylsulfonium salt examples include benzyl-4-hydroxyphenylmethylsulfonium hexafluoroantimonate, benzyl-4-hydroxyphenylmethylsulfonium hexafluorophosphate, 4-acetoxyphenylbenzylmethylsulfonium hexafluoroantimonate, benzyl-4-methoxy Phenylmethylsulfonium hexafluoroantimonate, benzyl-2-methyl-4-hydroxyphenylmethylsulfonium hexafluoroantimonate, benzyl-3-chloro-4-hydroxyphenylmethylsulfonium hexafluoroarsenate, 4-methoxybenzyl-4-hydroxy Examples thereof include phenylmethylsulfonium hexafluorophosphate.
  • dibenzylsulfonium salt examples include dibenzyl-4-hydroxyphenylsulfonium hexafluoroantimonate, dibenzyl-4-hydroxyphenylsulfonium hexafluorophosphate, 4-acetoxyphenyl dibenzylsulfonium hexafluoroantimonate, and dibenzyl-4-methoxyphenyl.
  • Sulfonium hexafluoroantimonate dibenzyl-3-chloro-4-hydroxyphenylsulfonium hexafluoroarsenate, dibenzyl-3-methyl-4-hydroxy-5-tert-butylphenylsulfonium hexafluoroantimonate, benzyl-4-methoxybenzyl Examples include -4-hydroxyphenylsulfonium hexafluorophosphate.
  • substituted benzylsulfonium salt examples include p-chlorobenzyl-4-hydroxyphenylmethylsulfonium hexafluoroantimonate, p-nitrobenzyl-4-hydroxyphenylmethylsulfonium hexafluoroantimonate, and p-chlorobenzyl-4-hydroxyphenyl.
  • Methylsulfonium hexafluorophosphate p-nitrobenzyl-3-methyl-4-hydroxyphenylmethylsulfonium hexafluoroantimonate, 3,5-dichlorobenzyl-4-hydroxyphenylmethylsulfonium hexafluoroantimonate, o-chlorobenzyl-3 And -chloro-4-hydroxyphenylmethylsulfonium hexafluoroantimonate.
  • benzothiazonium salt examples include 3-benzylbenzothiazonium hexafluoroantimonate, 3-benzylbenzothiazonium hexafluorophosphate, 3-benzylbenzothiazonium tetrafluoroborate, 3- (p-methoxy).
  • Benzyl) benzothiazonium hexafluoroantimonate 3-benzyl-2-methylthiobenzothiazonium hexafluoroantimonate, 3-benzyl-5-chlorobenzothiazonium hexafluoroantimonate, and the like.
  • tetrahydrothiophenium salt examples include 4,7-di-n-butoxy-1-naphthyltetrahydrothiophenium trifluoromethanesulfonate, 1- (4-n-butoxynaphthalen-1-yl) tetrahydrothiophenium trifluoro.
  • sulfonimide compound examples include N- (trifluoromethylsulfonyloxy) succinimide, N- (camphorsulfonyloxy) succinimide, N- (4-methylphenylsulfonyloxy) succinimide, N- (2-trifluoromethylphenylsulfonyl).
  • Halogen-containing compounds examples include haloalkyl group-containing hydrocarbon compounds and haloalkyl group-containing heterocyclic compounds.
  • diazomethane compounds examples include bis (trifluoromethylsulfonyl) diazomethane, bis (cyclohexylsulfonyl) diazomethane, bis (phenylsulfonyl) diazomethane, bis (p-tolylsulfonyl) diazomethane, and bis (2,4-xylylsulfonyl) diazomethane.
  • sulfone compound examples include ⁇ -ketosulfone compounds, ⁇ -sulfonylsulfone compounds, diaryldisulfone compounds, and the like.
  • sulfonic acid ester compounds examples include alkyl sulfonic acid esters, haloalkyl sulfonic acid esters, aryl sulfonic acid esters, and imino sulfonates.
  • carboxylic acid ester compound examples include carboxylic acid o-nitrobenzyl ester.
  • thermosensitive acid generator examples include diphenyliodonium salts, triphenylsulfonium salts, sulfonium salts, benzothiazonium salts, ammonium salts, phosphonium salts, onium salts such as tetrahydrothiophenium salts, and sulfonimides. Compounds and the like. These heat-sensitive acid generators may function as a radiation-sensitive acid generator.
  • an oxime sulfonate compound, an onium salt and a sulfonate compound are preferable, and an oxime sulfonate compound is more preferable.
  • the film-forming composition can further improve the sensitivity, and can also improve the solubility.
  • the lower limit of the content of the acid generator is preferably 0.1 parts by weight and more preferably 1 part by weight with respect to 100 parts by weight of the polymer (A). preferable.
  • the upper limit 10 mass parts is preferable and 5 mass parts is more preferable.
  • solvent (C) Although it does not specifically limit as a solvent (C), The solvent which can melt
  • Solvents (C) include alcohols, ethers, diethylene glycol alkyl ethers, ethylene glycol alkyl ether acetates, propylene glycol monoalkyl ether acetates, propylene glycol monoalkyl ether propionates, aliphatic hydrocarbons, aromatics Group hydrocarbons, ketones, esters and the like.
  • alcohols examples include long-chain alkyl alcohols such as 1-hexanol, 1-octanol, 1-nonanol, 1-dodecanol, 1,6-hexanediol, 1,8-octanediol; Aromatic alcohols such as benzyl alcohol; Ethylene glycol monoalkyl ethers such as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobutyl ether; Propylene glycol monoalkyl ethers such as propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monopropyl ether, propylene glycol monobutyl ether; Examples include dipropylene glycol monoalkyl ethers such as dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, dipropylene glycol monopropyl
  • ethers examples include tetrahydrofuran, hexyl methyl ether, triethylene glycol dimethyl ether, triethylene glycol diethyl ether, 1,4-dioxane, and the like.
  • diethylene glycol alkyl ethers examples include diethylene glycol dimethyl ether, diethylene glycol diethyl ether, and diethylene glycol ethyl methyl ether.
  • ethylene glycol alkyl ether acetates examples include methyl cellosolve acetate, ethyl cellosolve acetate, ethylene glycol monobutyl ether acetate, and ethylene glycol monoethyl ether acetate.
  • propylene glycol monoalkyl ether acetates examples include propylene glycol monomethyl ether acetate, propylene glycol monoethyl ether acetate, propylene glycol monopropyl ether acetate, propylene glycol monobutyl ether acetate and the like.
  • propylene glycol monoalkyl ether propionates examples include propylene glycol monomethyl ether propionate, propylene glycol monoethyl ether propionate, propylene glycol monopropyl ether propionate, and propylene glycol monobutyl ether propionate. be able to.
  • Examples of the aliphatic hydrocarbons include n-pentane, n-hexane, n-heptane, n-octane, n-nonane, n-decane, n-undecane, n-dodecane, cyclohexane, decalin and the like. it can.
  • aromatic hydrocarbons examples include benzene, toluene, xylene, ethylbenzene, n-propylbenzene, i-propylbenzene, n-butylbenzene, mesitylene, chlorobenzene, dichlorobenzene and the like.
  • ketones examples include methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, 2-heptanone, 4-hydroxy-4-methyl-2-pentanone, and the like.
  • esters examples include methyl acetate, ethyl acetate, propyl acetate, i-propyl acetate, butyl acetate, ethyl 2-hydroxypropionate, methyl 2-hydroxy-2-methylpropionate, 2-hydroxy-2-methylpropion Ethyl acetate, methyl hydroxyacetate, ethyl hydroxyacetate, butyl hydroxyacetate, methyl lactate, ethyl lactate, propyl lactate, butyl lactate, methyl 3-hydroxypropionate, ethyl 3-hydroxypropionate, propyl 3-hydroxypropionate, 3- Butyl hydroxypropionate, methyl 2-hydroxy-3-methylbutanoate, methyl methoxyacetate, ethyl methoxyacetate, propyl methoxyacetate, butyl methoxyacetate, methyl ethoxyacetate, ethyl ethoxyacetate, propyl ethoxyacetate, Butyl acetate
  • a solvent (C) may be used individually by 1 type, and 2 or more types may be mixed and used for it.
  • the content of the solvent (C) within the above range, the coating property is improved, and the occurrence of coating unevenness (such as streaky unevenness, pin mark unevenness, and mottled unevenness) is suppressed, and the film thickness uniformity is improved. Can be obtained.
  • the sensitizer (D) has a function of improving the radiation sensitivity of the film-forming composition.
  • the sensitizer (D) is preferably a compound that absorbs radiation and becomes an electronically excited state.
  • the sensitizer (D) in the electronically excited state comes into contact with the acid generator (B) to cause electron transfer, energy transfer, heat generation, etc., and the acid generator (B) undergoes a chemical change. Decomposes to produce acid.
  • Examples of the sensitizer (D) include compounds belonging to the following compounds and having an absorption wavelength in the region of 350 nm to 450 nm.
  • Examples of the sensitizer (D) include pyrene, perylene, triphenylene, anthracene, 9,10-dibutoxyanthracene, 9,10-diethoxyanthracene, 3,7-dimethoxyanthracene, 9,10-dipropyloxyanthracene and the like.
  • Xanthenes such as fluorescein, eosin, erythrosine, rhodamine B, rose bengal;
  • Xanthones such as xanthone, thioxanthone, dimethylthioxanthone, diethylthioxanthone (2,4-diethylthioxanthen-9-one, etc.), isopropylthioxanthone (2-isopropylthioxanthone, etc.); Cyanines such as thiacarbocyanine, oxacarbocyanine; Merocyanines such as merocyanine and carbomerocyanine; Rhodocyanines; Oxonols; Thiazines such as thionine, methylene blue and toluidine blue; Acridines such as acridine orange, chloroflavin, acriflavine; Acridones such as acridone, 10-butyl-2-ch
  • sensitizers (D) polynuclear aromatics, acridones, styryls, base styryls, coumarins and xanthones are preferred, and xanthones are more preferred.
  • a sensitizer (D) may be used individually by 1 type, and may mix and use 2 or more types.
  • a sensitizer (D) As a minimum of content of a sensitizer (D), 0.1 mass part is preferable with respect to 100 mass parts of polymers (A), and 0.3 mass part is more preferable. On the other hand, as this upper limit, 8 mass parts is preferable and 4 mass parts is more preferable.
  • the quencher (E) has a function of controlling the diffusion of the acid from the acid generator (B).
  • Examples of the quencher (E) include amine compounds, amide group-containing compounds, urea compounds, nitrogen-containing heterocyclic compounds, and the like.
  • Examples of the amine compound include mono (cyclo) alkylamines; di (cyclo) alkylamines; tri (cyclo) alkylamines; substituted alkylanilines or derivatives thereof; ethylenediamine, N, N, N ′, N′-tetra Methylethylenediamine, tetramethylenediamine, hexamethylenediamine, 4,4′-diaminodiphenylmethane, 4,4′-diaminodiphenyl ether, 4,4′-diaminobenzophenone, 4,4′-diaminodiphenylamine, 2,2-bis (4 -Aminophenyl) propane, 2- (3-aminophenyl) -2- (4-aminophenyl) propane, 2- (4-aminophenyl) -2- (3-hydroxyphenyl) propane, 2- (4-amino) Phenyl) -2- (4-hydroxyphenyl) propane, 1 4-bis (1- (4-a
  • amide group-containing compounds include Nt-butoxycarbonyl group-containing amino compounds, formamide, N-methylformamide, N, N-dimethylformamide, acetamide, N-methylacetamide, N, N-dimethylacetamide, propionamide, Examples thereof include benzamide, pyrrolidone, N-methylpyrrolidone, N-acetyl-1-adamantylamine, and isocyanuric acid tris (2-hydroxyethyl).
  • urea compounds include urea, methylurea, 1,1-dimethylurea, 1,3-dimethylurea, 1,1,3,3-tetramethylurea, 1,3-diphenylurea, tri-n-butylthiourea, etc. Is mentioned.
  • nitrogen-containing heterocyclic compound examples include imidazoles such as 2-phenylbenzimidazole; pyridines such as 4- (dimethylamino) pyridine; piperazines; pyrazine, pyrazole, pyridazine, quinosaline, purine, pyrrolidine, piperidine, piperidine ethanol 3-piperidino-1,2-propanediol, morpholine, 4-methylmorpholine, 1- (4-morpholinyl) ethanol, 4-acetylmorpholine, 3- (N-morpholino) -1,2-propanediol, 1, 4-dimethylpiperazine, 1,4-diazabicyclo [2.2.2] octane and the like.
  • imidazoles such as 2-phenylbenzimidazole
  • pyridines such as 4- (dimethylamino) pyridine
  • piperazines pyrazine, pyrazole, pyridazine, quinosa
  • a photodegradable base can be used as the quencher (E).
  • the photodegradable base include sulfonium salt compounds and onium salt compounds such as iodonium salt compounds.
  • quencher (E) a nitrogen-containing heterocyclic compound is preferable, and imidazoles and pyridines are more preferable.
  • a quencher (E) may be used individually by 1 type, and 2 or more types may be mixed and used for it.
  • quencher (E) As a minimum of content of quencher (E), 0.001 mass part is preferred to 100 mass parts of polymer (A), and 0.01 mass part is more preferred. On the other hand, as this upper limit, 3 mass parts is preferable and 1 mass part is more preferable.
  • the film forming composition can improve curability by containing the polymerizable compound (F).
  • the polymerizable compound (F) is usually a polymerizable compound having an ethylenically unsaturated bond.
  • the polymerizable compound (F) a monofunctional, bifunctional, or trifunctional (meth) acrylic acid ester is preferable from the viewpoints of good polymerizability and improved strength of the obtained film.
  • the monofunctional compound refers to a compound having one (meth) acryloyl group
  • the bifunctional or trifunctional or higher functional compound is a compound having two or three (meth) acryloyl groups, respectively. I mean.
  • Examples of the monofunctional (meth) acrylic acid ester include 2-hydroxyethyl acrylate, 2-hydroxyethyl methacrylate, diethylene glycol monoethyl ether acrylate, diethylene glycol monoethyl ether methacrylate, (2-acryloyloxyethyl) (2-hydroxypropyl)
  • Examples include phthalate, (2-methacryloyloxyethyl) (2-hydroxypropyl) phthalate, and ⁇ -carboxypolycaprolactone monoacrylate.
  • bifunctional (meth) acrylic acid ester examples include ethylene glycol diacrylate, propylene glycol diacrylate, propylene glycol dimethacrylate, ethylene glycol dimethacrylate, diethylene glycol diacrylate, diethylene glycol dimethacrylate, tetraethylene glycol diacrylate, and tetraethylene glycol.
  • Examples include dimethacrylate, 1,6-hexanediol diacrylate, 1,6-hexanediol dimethacrylate, 1,9-nonanediol diacrylate, and 1,9-nonanediol dimethacrylate.
  • trifunctional or higher functional (meth) acrylic acid ester examples include trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, pentaerythritol triacrylate, pentaerythritol trimethacrylate, pentaerythritol tetraacrylate, pentaerythritol tetramethacrylate, and dipentaerythritol.
  • the polymerizable compound (F) is preferably a bifunctional or trifunctional or higher (meth) acrylic acid ester, 1,9-nonanediol dimethacrylate, trimethylolpropane triacrylate, pentaerythritol triacrylate, pentaerythritol tetraacrylate, Dipentaerythritol pentaacrylate, dipentaerythritol hexaacrylate, mixture of dipentaerythritol hexaacrylate and dipentaerythritol pentaacrylate, ethylene oxide modified dipentaerythritol hexaacrylate, succinic acid modified pentaerythritol triacrylate, succinic acid modified dipentaerythritol More preferred are pentaacrylate and polyfunctional urethane acrylate compounds.
  • a polymeric compound (F) may be used individually by 1 type, and 2 or more types may be mixed and used for it.
  • a polymeric compound (F) As a minimum of content of a polymeric compound (F), 1 mass part is preferable with respect to 100 mass parts of polymers (A), 3 mass parts is more preferable, and 5 mass parts is further more preferable. On the other hand, as this upper limit, 100 mass parts is preferable, 50 mass parts is more preferable, 20 mass parts is further more preferable, 10 mass parts is especially preferable.
  • the radiation sensitive polymerization initiator (G) is a compound that starts or accelerates the polymerization of the polymerizable compound (F) upon irradiation with radiation. Therefore, when the film-forming composition contains a polymerizable compound (F), it is preferable to use a radiation-sensitive polymerization initiator (G).
  • Examples of the radiation sensitive polymerization initiator (G) include O-acyloxime compounds, acetophenone compounds, biimidazole compounds and the like.
  • O-acyloxime compound examples include ethanone-1- [9-ethyl-6- (2-methylbenzoyl) -9H-carbazol-3-yl] -1- (O-acetyloxime), 1- [9 -Ethyl-6-benzoyl-9. H. -Carbazol-3-yl] -octane-1-one oxime-O-acetate, 1- [9-ethyl-6- (2-methylbenzoyl) -9. H. -Carbazol-3-yl] -ethane-1-one oxime-O-benzoate, 1- [9-n-butyl-6- (2-ethylbenzoyl) -9. H.
  • acetophenone compound examples include ⁇ -aminoketone compounds and ⁇ -hydroxyketone compounds.
  • amino ketone compound examples include 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) -butan-1-one, 2-dimethylamino-2- (4-methylbenzyl) -1- (4 -Morpholin-4-yl-phenyl) -butan-1-one, 2-methyl-1- (4-methylthiophenyl) -2-morpholinopropan-1-one, and the like.
  • Examples of the ⁇ -hydroxyketone compound include 1-phenyl-2-hydroxy-2-methylpropan-1-one and 1- (4-i-propylphenyl) -2-hydroxy-2-methylpropan-1-one. 4- (2-hydroxyethoxy) phenyl- (2-hydroxy-2-propyl) ketone, 1-hydroxycyclohexyl phenylketone and the like.
  • biimidazole compound examples include 2,2′-bis (2-chlorophenyl) -4,4 ′, 5,5′-tetrakis (4-ethoxycarbonylphenyl) -1,2′-biimidazole, 2,2 '-Bis (2-chlorophenyl) -4,4', 5,5'-tetraphenyl-1,2'-biimidazole, 2,2'-bis (2,4-dichlorophenyl) -4,4 ', 5 , 5′-tetraphenyl-1,2′-biimidazole, 2,2′-bis (2,4,6-trichlorophenyl) -4,4 ′, 5,5′-tetraphenyl-1,2′- Biimidazole etc. can be mentioned.
  • an aliphatic or aromatic compound having a dialkylamino group can be used in combination in order to sensitize it.
  • the aliphatic or aromatic compound having a dialkylamino group include 4,4'-bis (dimethylamino) benzophenone and 4,4'-bis (diethylamino) benzophenone.
  • an O-acyloxime compound and an acetophenone compound are preferable.
  • an acetophenone compound an aminoketone compound is preferable.
  • a radiation sensitive polymerization initiator (G) may be used individually by 1 type, and 2 or more types may be mixed and used for it.
  • a radiation sensitive polymerization initiator (G) As a minimum of content of a radiation sensitive polymerization initiator (G), 0.05 mass part is preferred to 100 mass parts of polymer (A), and 0.1 mass part is more preferred. On the other hand, as this upper limit, 10 mass parts is preferable and 2 mass parts is more preferable.
  • the film-forming composition may further contain other optional components as long as the effects of the present invention are not impaired.
  • other optional components include a surfactant, a storage stabilizer, an adhesion aid, and a heat resistance improver.
  • Other optional components may be used alone or in combination of two or more.
  • a multilayer wiring according to an embodiment of the present invention is a multilayer wiring obtained by the method for forming a multilayer wiring. Since the multilayer wiring is obtained by the above-described forming method, it is excellent in productivity and can be reduced in cost.
  • the laminated wiring can be suitably used for semiconductor elements and electronic circuits. Moreover, this semiconductor element and electronic circuit can be used suitably for an electronic device etc.
  • An electronic device using the multilayer wiring can be downsized, thinned, enhanced in functionality, and the like. Examples of the electronic device include a liquid crystal display, a portable information device, a digital camera, an organic display, an organic EL lighting, a sensor, and a wearable device.
  • a multilayer multilayer wiring having three or more conductive layers (wirings) can be formed.
  • a multilayer wiring can be formed by repeating the step (B) and the step (C) a plurality of times.
  • a step (A) of preparing a base material having the first conductive layer as the outermost layer an existing substrate with a conductive layer is prepared instead of forming the first conductive layer using a base film forming composition or the like. You can also use it as it is.
  • the formation method of the said multilayer wiring is a method which can obtain a pattern, without passing through the image development process using a developing solution after irradiation.
  • a development process or a cleaning process can be performed instead of or together with the heating after radiation irradiation.
  • thermosensitive acid generator As the acid generator contained in the insulating film forming composition or the base film forming composition, a thermosensitive acid generator or the like can be used. In this case, instead of irradiation with radiation, an acid can be generated by heating a part of the surface region to form a lyophilic surface region. Part of the surface region can be heated, for example, with a laser. Further, a part of the surface region may be heated by radiation irradiation.
  • the insulating film may not have a via hole.
  • a laminated wiring in which the first conductive layer and the second conductive layer are not conductive (insulated) can be formed.
  • Weight average molecular weight (Mw) and molecular weight distribution (Mw / Mn) The weight average molecular weight (Mw) and molecular weight distribution (Mw / Mn) in terms of polystyrene of the polymers obtained in the following synthesis examples were measured under the following conditions.
  • solid content concentration 34.6% by mass.
  • solid content concentration means the ratio of the copolymer mass which occupies for the total mass of a copolymer solution.
  • the obtained reaction solution was added dropwise to an excessive amount of methanol for reprecipitation purification. Subsequently, the precipitate was dissolved again in 30 parts by mass of tetrahydrofuran, and then reprecipitated and purified by dropwise addition to hexane, and the precipitate was dried to obtain a polymer (P-5) as a white solid copolymer. ) The obtained polymer (P-5) was analyzed using 1 H-NMR to confirm that acetalization had progressed (chemical shift: 5.48 ppm, acetal group C—H).
  • reaction solution was cooled to room temperature, and 0.5 parts by mass of pyridine was added to quench the reaction.
  • the obtained reaction solution was added dropwise to an excessive amount of methanol for reprecipitation purification.
  • the precipitate was dissolved again in 30 parts by mass of tetrahydrofuran, and then purified by reprecipitation by dropwise addition to hexane, and the precipitate was dried to obtain a polymer (P-6) as a white solid copolymer. ) 12.1 parts by mass were obtained.
  • the obtained polymer (P-6) was analyzed using 1 H-NMR to confirm that acetalization had progressed (chemical shift: 5.49 ppm, acetal group C—H).
  • first layer wiring first conductive layer
  • the film-forming compositions prepared in Preparation Examples 1 to 9 or Comparative Preparation Examples 1 and 2 were applied on a glass substrate (Corning “EAGLE-XG”) with a spinner, respectively, in a clean oven at 90 ° C.
  • a coating film having a thickness of 0.2 ⁇ m was formed by pre-baking for 5 minutes.
  • a high-pressure mercury lamp (“MA-1400” from Dainippon Kaken Co., Ltd.) is used to apply a quartz mask (contact) to the coating film formed by the above-mentioned “coatability of the second layer film-forming composition”.
  • the exposure dose was 250 mJ / cm 2 and the irradiation was performed. Thereafter, baking was performed at 110 ° C. for 15 minutes using a hot plate to form a lyophilic surface region (exposed portion) and a liquid repellent surface region (non-exposed portion).
  • FIG. 5 shows an image of “a substrate on which a repellent pattern is formed on the second layer” in Example 1.
  • a second layer repellent pattern is formed in the left-right direction.
  • a 20 ⁇ m square hole was formed in the lyophilic portion (lyophilic surface region) of the obtained lyophilic / repellent patterning substrate with a YAG laser thin film processing apparatus (“VL-C” of TNS Systems LLC, oscillation wavelength: 266 nm). .
  • VL-C YAG laser thin film processing apparatus
  • the method for forming a laminated wiring according to the present invention can efficiently form a three-dimensional wiring pattern and can be used for printed electronics or the like.
  • the multilayer wiring obtained by the method for forming a multilayer wiring according to the present invention is suitable for an electronic circuit provided in an electronic device such as a liquid crystal display, a portable information device, a digital camera, an organic display, an organic EL lighting, a sensor, and a wearable device. Can be used.

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  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Manufacturing Of Printed Wiring (AREA)
  • Printing Elements For Providing Electric Connections Between Printed Circuits (AREA)
  • Internal Circuitry In Semiconductor Integrated Circuit Devices (AREA)
  • Formation Of Insulating Films (AREA)

Abstract

L'invention concerne un procédé de formation de câblage en couches qui permet de former efficacement un câblage en couches. La présente invention est un procédé de formation de câblage en couches comprenant : une étape de préparation d'un substrat ayant une première couche conductrice comme couche la plus à l'extérieur ; une étape de formation, sur la surface du substrat, d'un film d'isolation ayant une région à surface repoussant un liquide et une région à surface attirant un liquide ; et une étape de formation d'une deuxième couche conductrice déposée en couches sur la région à surface attirant un liquide du film d'isolation en amenant un matériau formant une deuxième couche conductrice à entrer en contact avec la surface du film d'isolation. L'étape de formation du film d'isolation comprend une étape de formation d'un film de revêtement isolant ayant une surface repoussant un liquide, au moyen d'une composition de formation d'un film d'isolation contenant un premier générateur d'acide et un premier polymère ayant un groupe dissociable à l'acide, et une étape de formation de la région à surface attirant un liquide sur une portion de la région de surface du film de revêtement isolant.
PCT/JP2016/069687 2015-07-28 2016-07-01 Procédé de formation de câblage en couches Ceased WO2017018129A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020012753A1 (fr) * 2018-07-11 2020-01-16 Jsr株式会社 Composition durcissable, structure et procédé de formation associé
US11604412B2 (en) * 2017-08-31 2023-03-14 Fujifilm Corporation Actinic ray-sensitive or radiation-sensitive resin composition, resist film, pattern forming method, and method for manufacturing electronic device

Citations (3)

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Publication number Priority date Publication date Assignee Title
JP2011091380A (ja) * 2005-06-03 2011-05-06 Daikin Industries Ltd パターン基板の製造方法
JP2011221471A (ja) * 2010-04-14 2011-11-04 Jsr Corp ポジ型感放射線性組成物、層間絶縁膜及びその形成方法
JP2015015378A (ja) * 2013-07-05 2015-01-22 株式会社リコー 積層配線の形成方法、積層配線、及び電子素子

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Publication number Priority date Publication date Assignee Title
TWI617629B (zh) * 2013-05-01 2018-03-11 Jsr股份有限公司 具有凹圖案的基材的製造方法、組成物、導電膜的形成方法、電子電路及電子元件

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011091380A (ja) * 2005-06-03 2011-05-06 Daikin Industries Ltd パターン基板の製造方法
JP2011221471A (ja) * 2010-04-14 2011-11-04 Jsr Corp ポジ型感放射線性組成物、層間絶縁膜及びその形成方法
JP2015015378A (ja) * 2013-07-05 2015-01-22 株式会社リコー 積層配線の形成方法、積層配線、及び電子素子

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11604412B2 (en) * 2017-08-31 2023-03-14 Fujifilm Corporation Actinic ray-sensitive or radiation-sensitive resin composition, resist film, pattern forming method, and method for manufacturing electronic device
WO2020012753A1 (fr) * 2018-07-11 2020-01-16 Jsr株式会社 Composition durcissable, structure et procédé de formation associé

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