Barrier material forming composition and method for producing the same, barrier material and method for producing the same, and product and method for producing the same

Abstract

To provide a barrier material that has excellent moisture-proofness and can be applied to objects of various shapes, and in which the surface of the object can be clearly seen after application.SOLUTION: Provided is a barrier material forming composition that contains a mixture of a hydrolytic polycondensation product of a silane compound containing a silane oligomer and a silane monomer, a curing catalyst, and a polyether-modified polydimethylsiloxane, and in which the ratio (N2 / N1) of the total number of carbon atoms bonded to oxygen atoms N2 to the total number of carbon atoms bonded to silicon atoms N1 in the polyether-modified polydimethylsiloxane is 2 to 4.SELECTED DRAWING: None

Description

[Technical Field]

[0001] The present invention relates to a barrier material-forming composition and a method for producing the same, a barrier material and a method for producing the same, and a product and a method for producing the same. [Background technology]

[0002] Conventionally, in order to prevent moisture from entering gaps formed in electronic components, sealing electronic components with barrier films etc. has been considered. For example, Patent Document 1 describes a barrier film laminate in which a barrier film having an inorganic oxide layer is laminated. [Prior art documents] [Patent documents]

[0003] [Patent Document 1] Japanese Patent Application Laid-Open No. 2011-093195 Summary of the Invention [Problem to be solved by the invention]

[0004] However, the barrier film laminate described in Patent Document 1 is in the form of a film, and therefore its applicability is limited.

[0005] In addition, with the recent trend toward finer and more diverse electronic components, there is a demand for good visibility of printing, markers, etc. on the surface of an object through the barrier material after the barrier material has been formed on the object.

[0006] Therefore, an object of the present invention is to provide a barrier material that has excellent moisture resistance, can be applied to objects of various shapes, and allows good visibility of the object surface after application. Another object of the present invention is to provide a barrier material-forming composition that can easily form the barrier material. A further object of the present invention is to provide a method for producing the barrier material-forming composition, a method for producing the barrier material, a product including the barrier material, and a method for producing the product. [Means for solving the problem]

[0007] The present invention provides a barrier material-forming composition comprising a mixture of a hydrolysis polycondensate of a silane compound containing a silane oligomer and a silane monomer, a curing catalyst, and a polyether-modified polydimethylsiloxane. By applying this composition to an object, a barrier material with excellent moisture resistance can be easily formed on the object. Furthermore, by appropriately selecting the ratio of polydimethylsiloxane moieties to polyether moieties in the polyether-modified polydimethylsiloxane as described below, the composition can be used to form a barrier material that allows good visibility of the object surface.

[0008] In one embodiment of the composition, the ratio (N2 / N1) of the total number of carbon atoms bonded to oxygen atoms, N2, to the total number of carbon atoms bonded to silicon atoms, N1, in the polyether-modified polydimethylsiloxane is 2 to 4. In such a composition, the ratio of polydimethylsiloxane moieties to polyether moieties is appropriately adjusted, and the polyether-modified polydimethylsiloxane functions well as a leveling material, smoothing the surface of the barrier material formed on the object. This significantly improves the visibility of the object surface after the barrier material is formed.

[0009] The composition according to one embodiment comprises a polyether-modified polydimethylsiloxane. 13 In the C-NMR spectrum, the peak P corresponds to the carbon atom bonded to the silicon atom. C1 Peak area S C1 Peak P corresponding to the carbon atom bonded to the oxygen atom C2 Peak area S C2 The ratio (S C2 / S C1 ) is 2 to 4. In such a composition, the ratio of the polydimethylsiloxane portion to the polyether portion is appropriately adjusted, and the polyether-modified polydimethylsiloxane functions well as a leveling material, smoothing the surface of the barrier material formed on the object. This significantly improves the visibility of the object surface after the barrier material has been formed.

[0010] The composition according to one embodiment comprises a polyether-modified polydimethylsiloxane. 1 In the H-NMR spectrum, the peak P corresponds to the hydrogen atom on the carbon atom bonded to the silicon atom. H1 Peak area S H1 Peak P corresponding to hydrogen atoms on carbon atoms bonded to oxygen atoms H2 Peak area S H2 The ratio (S H2 / S H1 ) is 1.0 to 1.8. In such a composition, the ratio of the polydimethylsiloxane portion to the polyether portion is appropriately adjusted, and the polyether-modified polydimethylsiloxane functions well as a leveling material, smoothing the surface of the barrier material formed on the object. This significantly improves the visibility of the object surface after the barrier material has been formed.

[0011] In one embodiment, the silane oligomer may have a silicon atom bonded to three oxygen atoms.

[0012] In one embodiment, the ratio of the total number of silicon atoms bonded to three oxygen atoms and silicon atoms bonded to four oxygen atoms to the total number of silicon atoms in the silane oligomer may be 30% or more.

[0013] In one embodiment, the silane monomer may include at least one selected from the group consisting of alkyltrialkoxysilanes, aryltrialkoxysilanes, and tetraalkoxysilanes.

[0014] In one embodiment, the content of the silane monomer in the silane compound may be 5 to 40 parts by mass relative to 100 parts by mass of the silane oligomer.

[0015] In one embodiment, the silane compound may further contain a linear polysiloxane.

[0016] In one embodiment, the linear polysiloxane has a kinematic viscosity of 50 mm at 25°C.2 / s or more.

[0017] In one embodiment, the linear polysiloxane may have a diorganopolysiloxane chain.

[0018] In one embodiment, the linear polysiloxane may have groups selected from the group consisting of silanol groups and alkoxy groups at both ends.

[0019] In one embodiment, the content of the linear polysiloxane in the silane compound may be 1 to 30 parts by mass relative to 100 parts by mass of the silane oligomer.

[0020] The present invention also provides a method for producing the composition, comprising the steps of heating the silane compound in the presence of an acid catalyst to obtain the hydrolysis polycondensate, and mixing the hydrolysis polycondensate, the curing catalyst, and the polyether-modified polydimethylsiloxane.

[0021] In one embodiment, the acid catalyst may include at least one selected from the group consisting of acetic acid, phosphoric acid, hydrochloric acid, and nitric acid.

[0022] The present invention also provides a method for producing a barrier material, comprising the step of curing the composition to form a barrier material.

[0023] The present invention also provides a method for producing a product having a moisture-proof treated member, the method comprising a first step of applying the composition onto the member, and a second step of curing the applied composition to form a barrier material on the member.

[0024] The present invention also provides a method for producing a product having a first member and a second member joined to the first member, wherein the joint between the first member and the second member is moisture-proof treated. The method includes a first step of disposing the composition between the first member and the second member, and a second step of curing the composition to form a barrier material and joining the first member and the second member via the barrier material.

[0025] The present invention also provides a method for manufacturing an article comprising a moisture barrier member, the method comprising a first step of curing the composition to produce a moisture barrier member having a barrier material, and a second step of assembling a plurality of components comprising the moisture barrier member.

[0026] The present invention also provides a barrier material which is a cured product of the above composition.

[0027] The present invention also provides a product comprising a member and the barrier material described above formed on the member.

[0028] The present invention also provides a product comprising a first member, a second member, and the barrier material provided between the first member and the second member, wherein the first member and the second member may be joined via the barrier material.

[0029] The present invention further provides an article of manufacture that is an assembly of multiple components including a moisture-proof component having the above-described barrier material. [Effects of the Invention]

[0030] The present invention provides a barrier material that has excellent moisture resistance, can be applied to objects of various shapes, and allows good visibility of the object surface after application. The present invention also provides a barrier material-forming composition that can easily form the barrier material. Furthermore, the present invention also provides a method for producing the barrier material-forming composition, a method for producing the barrier material, a product including the barrier material, and a method for producing the product. DETAILED DESCRIPTION OF THE INVENTION

[0031] Preferred embodiments of the present invention will be described below. In this specification, a numerical range indicated using "to" indicates a range that includes the numerical values ​​before and after "to" as the minimum and maximum values, respectively. "A or B" may include either A or B, or may include both. Unless otherwise specified, the materials exemplified in this embodiment can be used alone or in combination of two or more.

[0032] <Barrier material forming composition> The barrier material-forming composition of this embodiment contains a mixture of a hydrolysis polycondensate of a silane compound containing a silane oligomer and a silane monomer, a curing catalyst, and a polyether-modified polydimethylsiloxane, in which the ratio of the polydimethylsiloxane moiety to the polyether moiety is adjusted to a predetermined range.

[0033] By applying such a composition to an object, a barrier material with excellent moisture resistance can be easily formed on the object, and the polyether-modified polydimethylsiloxane in the composition functions well as a leveling agent, smoothing the surface of the barrier material formed on the object. Therefore, the composition makes it possible to form a barrier material that allows the surface of the object to be clearly seen.

[0034] Furthermore, conventional siloxane-based barrier materials suffer from weight loss due to hydrolysis under high temperature and humidity conditions, which can result in poor long-term reliability. In contrast, the barrier material formed from the above composition is sufficiently inhibited from weight loss due to hydrolysis, even under high temperature and humidity conditions, and has excellent long-term reliability.

[0035] The ratio of polydimethylsiloxane moieties to polyether moieties can be determined, for example, by the ratio (N2 / N1) of the total number of carbon atoms bonded to oxygen atoms, N2, to the total number of carbon atoms bonded to silicon atoms, N1, in the polyether-modified polydimethylsiloxane. The ratio (N2 / N1) is, for example, 2 to 4, and preferably 2.2 to 3.8.

[0036] The ratio of the polydimethylsiloxane portion to the polyether portion is, for example, 13 Peak P in the C-NMR spectrum corresponds to the carbon atom bonded to the silicon atom C1 Peak area S C1 Peak P corresponding to the carbon atom bonded to the oxygen atom C2 Peak area S C2 The ratio (S C2 / S C1 ) may be specified by the ratio (S C2 / S C1 ) is, for example, 2 to 4, and preferably 2.2 to 3.8.

[0037] The ratio of the polydimethylsiloxane portion to the polyether portion is, for example, 1 In the H-NMR spectrum, the peak P corresponds to the hydrogen atom on the carbon atom bonded to the silicon atom. H1 Peak area S H1 Peak P corresponding to hydrogen atoms on carbon atoms bonded to oxygen atoms H2 Peak area S H2 The ratio (S H2 / S H1 ) may be specified by the ratio (S H2 / S H1 ) is, for example, 0.8 to 2.0, and preferably 1.0 to 1.8.

[0038] That is, the composition of the present embodiment may satisfy the following formula (1). 2 <N2 / N1<4 …(1)

[0039] Furthermore, the composition of the present embodiment may satisfy either the following formula (2) or formula (3), and preferably satisfies both: 2 C2 / S C1 <4 …(2) 0.8 H2 / S H1 <2.0 …(3)

[0040] In this specification, 13 The C-NMR spectrum is measured by the following method. (solution 13 C-NMR measurement conditions) Device name: JEOL RESONANCE ECX400II Observed nucleus: 13C Observation frequency: 10.052MHz Measurement temperature: room temperature (23℃) Measurement solvent: CDCl3 Pulse width: 11.4 μsec (45°) Pulse repetition time: 2.0 seconds Accumulation count: 700 times Sample concentration (sample / measurement solvent): 100 mg / 1.0 ml

[0041] 13 In the C-NMR spectrum, peak P C1 The peak area S may be a peak having a chemical shift in the range of 5 ppm to −5 ppm (preferably 3 ppm to −3 ppm). C1 may be the total value of the peak areas of peaks with chemical shifts in the range of 5 ppm to −5 ppm (preferably 3 ppm to −3 ppm).

[0042] Also, 13 In the C-NMR spectrum, peak P C2 may be a peak having a chemical shift in the range of 47 ppm to 65 ppm (preferably 50 ppm to 65 ppm). That is, the peak area S C2 may be the total value of the peak areas of peaks with chemical shifts in the range of 47 ppm to 65 ppm (preferably 50 ppm to 65 ppm).​​

[0043] In this specification, 1 The H-NMR spectrum is measured by the following method. (solution 1 H-NMR measurement conditions) Device name: JEOL RESONANCE ECX400II Observed nucleus: 1H Observation frequency: 399.78MHz Measurement temperature: room temperature (23℃) Measurement solvent: CDCl3 Pulse width: 6.64 μsec (90°) Pulse repetition time: 5.0 seconds Number of times: 8 Sample concentration (sample / measurement solvent): 10 mg / 1.0 ml

[0044] 1 In the H-NMR spectrum, peak P H1 may be a peak having a chemical shift in the range of 0.5 ppm to −0.5 ppm (preferably 0.3 ppm to −0.3 ppm). That is, the peak area S H1 may be the total value of the peak areas of peaks with chemical shifts in the range of 0.5 ppm to −0.5 ppm (preferably 0.3 ppm to −0.3 ppm).

[0045] Also, 1 In the H-NMR spectrum, peak P H2 may be a peak having a chemical shift in the range of 4.5 ppm to 2.5 ppm (preferably 4 ppm to 2 ppm). That is, the peak area S H2 may be the total value of the peak areas of peaks with chemical shifts in the range of 4.5 ppm to 2.5 ppm (preferably 4 ppm to 2 ppm).

[0046] The barrier material-forming composition may be in a liquid or paste form, and is preferably in a liquid form from the viewpoint of easier application to an object.

[0047] A silane oligomer has a structure in which multiple silicon atoms are linked via oxygen atoms, and can also be called a polymer of silane monomers. In this specification, the term "silane oligomer" refers to a polymer having a molecular weight of 100,000 or less.

[0048] The silicon atoms contained in the silane oligomer can be classified into silicon atoms bonded to one oxygen atom (M unit), silicon atoms bonded to two oxygen atoms (D unit), silicon atoms bonded to three oxygen atoms (T unit), and silicon atoms bonded to four oxygen atoms (Q unit). Examples of M units, D units, T units, and Q units are represented by the following formulae (M), (D), (T), and (Q), respectively.

[0049] [ka]

[0050] In the above formula, R represents an atom (such as a hydrogen atom) or an atomic group (such as an alkyl group) other than an oxygen atom bonded to silicon. Information about the content of these units can be obtained by Si-NMR.

[0051] In the silane oligomer, the ratio of the total number of T units and Q units to the total number of silicon atoms may be, for example, 30% or more, preferably 50% or more, more preferably 70% or more, even more preferably 90% or more, or even 100%. Such a silane oligomer provides a barrier material with even better moisture resistance.

[0052] In a preferred embodiment, the silane oligomer preferably contains T units. The content of T units in the silane oligomer is, for example, 10% or more, preferably 20% or more, 30% or more, 40% or more, 50% or more, 70% or more, 80% or more, or 90% or more, or even 100%, based on the total number of silicon atoms. Such a silane oligomer tends to further improve the flexibility of the barrier material.

[0053] In another preferred embodiment, the content of Q units in the silane oligomer is, for example, 50% or more, preferably 70% or more, more preferably 80% or more, and even more preferably 90% or more, relative to the total number of silicon atoms, and may be 100%. Such a silane oligomer tends to further improve the moisture resistance and transparency of the barrier material.

[0054] The silane oligomer preferably has an alkyl group or an aryl group as R in the above formulas (M), (D), (T) and (Q).

[0055] The alkyl group is preferably an alkyl group having 6 or less carbon atoms, more preferably an alkyl group having 4 or less carbon atoms. Specific examples of the alkyl group include a methyl group, an ethyl group, a propyl group, and a butyl group, and of these, a methyl group, an ethoxy group, and a propyl group are preferred, and a methyl group is more preferred.

[0056] Examples of the aryl group include a phenyl group and a substituted phenyl group. Examples of the substituent of the substituted phenyl group include an alkyl group, a vinyl group, a mercapto group, an amino group, a nitro group, a cyano group, etc. The aryl group is preferably a phenyl group.

[0057] The weight-average molecular weight of the silane oligomer may be, for example, 400 or more, preferably 600 or more, and more preferably 1,000 or more. The weight-average molecular weight of the silane oligomer may be, for example, 30,000 or less, preferably 10,000 or less, and more preferably 6,000 or less. A higher weight-average molecular weight of the silane oligomer tends to improve flexibility, while a lower weight-average molecular weight tends to improve moisture resistance and transparency. In this specification, the weight-average molecular weight of the silane oligomer refers to the weight-average molecular weight expressed in terms of polystyrene measured by gel permeation chromatography (GPC).

[0058] The content of the silane oligomer in the silane compound may be, for example, 30% by mass or more, preferably 40% by mass or more, more preferably 45% by mass or more, and even more preferably 50% by mass or more, based on the total amount of the silane compound. This more significantly enhances the effects of the invention described above. Furthermore, the content of the silane oligomer in the silane compound may be, for example, 95% by mass or less, 90% by mass or less, 85% by mass or less, or 80% by mass or less, based on the total amount of the silane compound.

[0059] In this embodiment, the silane compound contains a silane monomer. By incorporating the silane monomer, for example, the contents of T units and Q units in the barrier material can be easily adjusted, and effects such as transparency and flexibility can be imparted to the barrier material depending on the application. Furthermore, by incorporating the silane monomer, a barrier material with even more excellent moisture resistance tends to be obtained.

[0060] The silane monomer may be, for example, at least one silane monomer (hereinafter also referred to as a first silane monomer) selected from the group consisting of alkyltrialkoxysilane, aryltrialkoxysilane, and tetraalkoxysilane.

[0061] By incorporating the first silane monomer, for example, it is possible to adjust the contents of T units and Q units in the barrier material, and to impart effects such as transparency and flexibility to the barrier material depending on the application. Furthermore, by incorporating the first silane monomer, a barrier material with even more excellent moisture resistance tends to be obtained.

[0062] When the silane compound contains a first silane monomer, the content of the first silane monomer in the silane compound is not particularly limited, and may be, for example, 5 parts by mass or more, preferably 8 parts by mass or more, and more preferably 10 parts by mass or more, relative to 100 parts by mass of the silane oligomer. This tends to further improve the flexibility of the cured product. Furthermore, the content of the first silane monomer may be, for example, 40 parts by mass or less, preferably 35 parts by mass or less, and more preferably 30 parts by mass or less. This tends to reduce the volatility of the coating liquid and further improve workability.

[0063] Alkyltrialkoxysilane is a silane compound in which one alkyl group and three alkoxy groups are bonded to a silicon atom.

[0064] The alkyl group of the alkyltrialkoxysilane is preferably an alkyl group having 6 or less carbon atoms, and more preferably an alkyl group having 4 or less carbon atoms. Specific examples of the alkyl group include a methyl group, an ethyl group, a propyl group, and a butyl group. Of these, a methyl group, an ethyl group, and a propyl group are preferred, and a methyl group is more preferred. Furthermore, the alkoxy group of the alkyltrialkoxysilane is preferably an alkoxy group having 6 or less carbon atoms, and more preferably an alkoxy group having 4 or less carbon atoms. Specific examples of the alkoxy group include a methoxy group, an ethoxy group, a propoxy group, and a butoxy group. Of these, a methoxy group, an ethoxy group, and a propoxy group are preferred, and a methoxy group and an ethoxy group are more preferred.

[0065] Aryltrialkoxysilanes are silane compounds in which one aryl group and three alkoxy groups are bonded to a silicon atom.

[0066] Examples of the aryl group of the aryltrialkoxysilane include a phenyl group and a substituted phenyl group. Examples of the substituent of the substituted phenyl group include an alkyl group, a vinyl group, a mercapto group, an amino group, a nitro group, and a cyano group. The aryl group is preferably a phenyl group. The alkoxy group of the aryltrialkoxysilane is preferably an alkoxy group having 6 or less carbon atoms, more preferably an alkoxy group having 4 or less carbon atoms. Specific examples of the alkoxy group include a methoxy group, an ethoxy group, a propoxy group, and a butoxy group. Of these, a methoxy group, an ethoxy group, and a propoxy group are preferred, and a methoxy group and an ethoxy group are more preferred.

[0067] Tetraalkoxysilane is a silane compound in which four alkoxy groups are bonded to a silicon atom.

[0068] The alkoxy group of the tetraalkoxysilane is preferably an alkoxy group having 6 or less carbon atoms, and more preferably an alkoxy group having 4 or less carbon atoms. Specific examples of the alkoxy group include a methoxy group, an ethoxy group, a propoxy group, and a butoxy group. Of these, a methoxy group, an ethoxy group, and a propoxy group are preferred, and a methoxy group and an ethoxy group are more preferred.

[0069] Specific examples of the first silane monomer include methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, and tetrabutoxysilane.

[0070] Examples of the silane monomer include a silane monomer having at least one reactive functional group selected from the group consisting of a vinyl group, an epoxy group, a glycidyl group, a (meth)acryloyl group, an amino group, an isocyanate group, an isocyanurate group, and a mercapto group (hereinafter also referred to as a second silane monomer). When the composition contains such a silane monomer, a barrier material with even better conformability and adhesion to the target object tends to be formed.

[0071] Although the reason why the second silane monomer exhibits the above-mentioned effects is not entirely clear, it is believed that during the formation of the barrier material, crosslinked structures other than siloxane bonds are formed by reactions between reactive functional groups, or between reactive functional groups and silanol groups, etc., which results in excellent moisture resistance and flexibility. It is also believed that during the formation of the barrier material, the reactive functional groups of the second silane monomer bond with functional groups present on the surface of the object, thereby achieving even better moisture resistance and flexibility.

[0072] From the viewpoint of further improving the flexibility of the barrier material and the adhesion to the member, the reactive functional group of the second silane monomer is preferably selected from the group consisting of a vinyl group, an epoxy group (more preferably a glycidyl group), a (meth)acryloyl group, an amino group, an isocyanate group, an isocyanurate group and a mercapto group, and an amino group is more preferred.

[0073] The second silane monomer preferably has a silicon atom bonded to three oxygen atoms.

[0074] As the second silane monomer, for example, a silane monomer represented by the following formula (A-1) can be suitably used.

[0075] [ka]

[0076] In the formula, R A1 indicates a reactive functional group, and L 1 is an alkanediyl group or an oxyalkanediyl group (-OL 2 a group represented by -, L 2 represents an alkanediyl group, p represents an integer of 0 or more (preferably an integer of 0 to 3), and R A2 represents an alkyl group or an aryl group.

[0077] R A1When is a vinyl group, p is preferably 0 to 3, and more preferably 0.

[0078] R A1 When is an epoxy group, a glycidyl group, a (meth)acryloyl group, an amino group, an isocyanate group, an isocyanurate group, or a mercapto group, p is preferably an integer of 1 or more, more preferably 1 to 3, and even more preferably 1.

[0079] R A1 is a vinyl group, a glycidyl group, or a (meth)acryloyl group, L 1 is preferably an oxyalkanediyl group.

[0080] R A1 is an amino group, an isocyanate group, an isocyanurate group, or a mercapto group, L 1 is preferably an alkanediyl group.

[0081] L 1 and L 2 The alkanediyl group in the formula (I) is preferably an alkanediyl group having 2 to 10 carbon atoms, and more preferably an alkanediyl group having 2 to 8 carbon atoms.

[0082] R A2 The alkyl group in the formula (I) is preferably an alkyl group having 6 or less carbon atoms, more preferably an alkyl group having 4 or less carbon atoms. Specific examples of the alkyl group include a methyl group, an ethyl group, a propyl group (n-propyl group, isopropyl group), a butyl group (n-butyl group, sec-butyl group, isobutyl group, tert-butyl group), etc.

[0083] R A2 The aryl group in is preferably a phenyl group.

[0084] R A2 is preferably an alkyl group.

[0085] When the silane compound contains a silane monomer, the content of the second silane monomer in the silane compound may be, for example, 0.01 parts by mass or more, preferably 0.05 parts by mass or more, and more preferably 0.1 parts by mass or more, per 100 parts by mass of the silane oligomer. This tends to further improve conformability and adhesion. Furthermore, the content of the second silane monomer in the silane compound may be, for example, 5 parts by mass or less, preferably 4 parts by mass or less, and more preferably 2 parts by mass or less. This tends to further improve the thermal stability of the cured product.

[0086] In this embodiment, the silane compound may further contain a linear polysiloxane, which allows the formation of a barrier material that is more conformable to the target object and has fewer defects such as cracks.

[0087] The linear polysiloxane can be said to be a compound having a linear main chain formed by siloxane bonds, and the main chain is preferably a diorganopolysiloxane chain. That is, the linear polysiloxane preferably has a polysiloxane chain composed of repeating D units.

[0088] The organic group bonded to the silicon atom in the main chain of the linear polysiloxane (that is, R in formula (D)) is preferably an alkyl group or an aryl group.

[0089] The alkyl group is preferably an alkyl group having 6 or less carbon atoms, more preferably an alkyl group having 4 or less carbon atoms. Specific examples of the alkyl group include a methyl group, an ethyl group, a propyl group, and a butyl group, and of these, a methyl group, an ethoxy group, and a propyl group are preferred, and a methyl group is more preferred.

[0090] Examples of the aryl group include a phenyl group and a substituted phenyl group. Examples of the substituent of the substituted phenyl group include an alkyl group, a vinyl group, a mercapto group, an amino group, a nitro group, a cyano group, etc. The aryl group is preferably a phenyl group.

[0091] The linear polysiloxane preferably has a group selected from the group consisting of a silanol group and an alkoxy group at at least one end, more preferably at both ends, and the silicon atom at the end bonded to the group is preferably a Q unit or a D unit, more preferably a D unit.

[0092] The alkoxy group is preferably an alkoxy group having 6 or less carbon atoms, more preferably an alkoxy group having 4 or less carbon atoms. Specific examples of the alkoxy group include a methoxy group, an ethoxy group, a propoxy group, and a butoxy group. Of these, a methoxy group, an ethoxy group, and a propoxy group are preferred, and a methoxy group and an ethoxy group are more preferred.

[0093] The kinematic viscosity of linear polysiloxane at 25°C is 50mm 2 Since such a linear polysiloxane has a sufficient chain length, the above-mentioned effects of blending the linear polysiloxane can be significantly obtained.

[0094] The kinematic viscosity of the linear polysiloxane at 25°C is preferably 60 mmHg, from the viewpoint of obtaining the above-mentioned effects more significantly. 2 / s or more, and more preferably 70 mm 2 / s or more.

[0095] The kinematic viscosity of linear polysiloxane at 25°C is 500mm 2 / s or less. This makes the linear polysiloxane highly compatible with other components in the composition, improving the transparency of the barrier material-forming composition and the barrier material that is the cured product thereof. From the viewpoint of obtaining this effect more significantly, the kinematic viscosity of the linear polysiloxane at 25°C is preferably 300 mm 2 / s or less is more preferable, and 100 mm 2 / s or less is more preferable.

[0096] When the silane compound contains a linear polysiloxane, the content of the linear polysiloxane in the silane compound may be, for example, 0.1 parts by mass or more, preferably 0.5 parts by mass or more, more preferably 1 part by mass or more, and even more preferably 2 parts by mass or more, relative to 100 parts by mass of the silane oligomer. This more significantly exhibits the above-mentioned effects. Furthermore, the content of the linear polysiloxane in the silane compound may be, for example, 40 parts by mass or less, preferably 30 parts by mass or more, more preferably 20 parts by mass or less, and even more preferably 10 parts by mass or less, relative to 100 parts by mass of the silane oligomer. This further improves the density of the coating film, and tends to result in particularly excellent moisture resistance.

[0097] The composition according to this embodiment contains a hydrolysis polycondensate of a silane compound. In this specification, the hydrolysis polycondensate of a silane compound can be referred to as a silane mixture obtained by subjecting a silane compound to a hydrolysis-polycondensation reaction (hereinafter simply referred to as a hydrolysis reaction). The hydrolysis polycondensate of a silane compound can also be referred to as a silane mixture formed by polycondensation of a hydrolyzate obtained by hydrolyzing a hydrolyzable group in a silane compound.

[0098] The hydrolyzable group may be any group that can generate a silanol group by hydrolysis, such as an alkoxy group such as a methoxy group or an ethoxy group. The hydrolyzable group is preferably a group that is directly bonded to a silicon atom in the silane compound.

[0099] The reaction conditions for the hydrolysis reaction are not particularly limited as long as the hydrolyzable group is converted into a silanol group. The hydrolysis reaction is preferably carried out, for example, by heating the silane compound in the presence of an acid catalyst.

[0100] Examples of the acid catalyst include acetic acid, phosphoric acid, hydrochloric acid, nitric acid, carbonic acid, and sulfuric acid, and at least one selected from the group consisting of acetic acid, phosphoric acid, hydrochloric acid, and nitric acid is preferred.

[0101] The amount of the acid catalyst may be, for example, 0.001 part by mass or more, preferably 0.005 part by mass or more, more preferably 0.01 part by mass or more, and even more preferably 0.05 part by mass or more, relative to 100 parts by mass of the silane compound. The amount of the acid catalyst may be, for example, 5 parts by mass or less, preferably 4 parts by mass or less, more preferably 3 parts by mass or less, and even more preferably 2 parts by mass or less, relative to 100 parts by mass of the silane compound.

[0102] The heating temperature during the hydrolysis reaction may be, for example, 40° C. or higher, and preferably 60° C. or lower. The heating temperature during the hydrolysis reaction may be, for example, 100° C. or lower, and preferably 90° C. or lower.

[0103] The reaction time of the hydrolysis reaction may be, for example, 30 minutes or more, preferably 1 hour or more, and may be, for example, 10 hours or less, preferably 5 hours or less.

[0104] The hydrolysis reaction is preferably carried out in a liquid medium. Examples of the liquid medium include water and organic solvents. Examples of the organic solvent include alcohols, ethers, ketones, esters, and hydrocarbons. In addition to these, acetonitrile, acetamide, N,N-dimethylformamide, N,N-dimethylacetamide, and N-methylpyrrolidone can also be used.

[0105] In a preferred embodiment, the hydrolysis reaction may be carried out in a liquid medium containing water and alcohols. By using such a liquid medium, a barrier material with excellent transparency can be easily obtained.

[0106] The alcohol is preferably one that can be vaporized by heating when forming the barrier material. For example, the alcohol is preferably an alcohol having 6 or less carbon atoms, more preferably an alcohol having 1 to 4 carbon atoms.

[0107] The composition of the present embodiment contains a curing catalyst. The curing catalyst may be any catalyst that can promote the further polymerization reaction of the hydrolysis polycondensate of the silane compound and can cure the composition by heating or the like.

[0108] Examples of curing catalysts include acid catalysts such as hydrochloric acid, nitric acid, sulfuric acid, acetic acid, and phosphoric acid, metal catalysts containing metal elements such as tin, titanium, aluminum, zinc, iron, cobalt, manganese, and zirconium, and base catalysts such as aliphatic amines, ammonium hydroxide, tetraethylammonium hydroxide, sodium carbonate, and sodium hydroxide. One type of curing catalyst may be used alone, or two or more types may be used in combination.

[0109] Examples of the metal catalyst include metal alkoxides and metal complexes. The metal catalyst may be any catalyst capable of promoting the dehydration condensation reaction of a silane compound having a silanol group (for example, the further dehydration condensation reaction of the hydrolysis polycondensate of the silane compound), and known metal catalysts can be used without particular limitation. One type of metal catalyst may be used alone, or two or more types may be used in combination.

[0110] The metal catalyst is preferably a metal catalyst selected from the group consisting of aluminum catalysts (metal catalysts containing aluminum), nickel catalysts (metal catalysts containing nickel), titanium catalysts (metal catalysts containing titanium), and zirconium catalysts (metal catalysts containing zirconium), and more preferably a metal catalyst selected from the group consisting of aluminum catalysts, nickel catalysts, and zirconium catalysts.

[0111] Examples of the aluminum catalyst, nickel catalyst, titanium catalyst, and zirconium catalyst include metal alkoxides and metal complexes. The metal catalyst may be any catalyst capable of promoting the dehydration condensation reaction of a silane compound having a silanol group (for example, the further dehydration condensation reaction of the hydrolysis polycondensate of the silane compound), and may be, for example, a known catalyst capable of promoting the dehydration condensation reaction. Examples of the aluminum catalyst include aluminum alkylacetoacetate diisopropylate, aluminum monoacetylacetonate bis(ethylacetoacetate), and aluminum tris(acetylacetonate).

[0112] The amount of the curing catalyst may be, for example, 0.001 parts by mass or more, preferably 0.005 parts by mass or more, more preferably 0.01 parts by mass or more, and even more preferably 0.02 parts by mass or more, relative to 100 parts by mass of the silane compound. This further shortens the curing time. The amount of the curing catalyst may be, for example, 1 part by mass or less, preferably 0.9 parts by mass or less, more preferably 0.6 parts by mass or less, and even more preferably 0.5 parts by mass or less, relative to 100 parts by mass of the silane compound. This tends to further improve the long-term reliability of the barrier material.

[0113] Polyether-modified polydimethylsiloxane can be said to be a compound in which some of the methyl groups of polydimethylsiloxane have been substituted with groups containing a polyether structure.

[0114] The polyether structure is preferably a polyoxyalkylene structure, and the polyoxyalkylene structure is preferably a polyoxyethylene structure, a polyoxypropylene structure, or a structure obtained by combining these.

[0115] Examples of polyether-modified polydimethylsiloxanes include compounds having a structural unit represented by the following formula (1-1) (hereinafter also referred to as structural unit (1-1)) and a structural unit represented by the following formula (1-2) (hereinafter also referred to as structural unit (1-2)).

[0116] [ka]

[0117] In the formula, R 1 and R 2 represents an alkanediyl group, and R 3 represents an alkyl group, and n represents an integer of 2 or more.

[0118] R 1 The alkanediyl group in the formula (I) is preferably an alkanediyl group having 2 to 15 carbon atoms, more preferably an alkanediyl group having 2 to 10 carbon atoms, and even more preferably an alkanediyl group having 2 to 8 carbon atoms.

[0119] R 2 The alkanediyl group in is preferably an alkanediyl group having 2 to 6 carbon atoms, more preferably an alkanediyl group having 2 to 4 carbon atoms, and even more preferably an alkanediyl group having 2 or 3 carbon atoms. 2 may be the same or different from each other.

[0120] R 3 The alkyl group in the formula (I) is preferably an alkyl group having 10 or less carbon atoms, more preferably an alkyl group having 8 or less carbon atoms, and even more preferably an alkyl group having 1 or more carbon atoms.

[0121] Although n is not particularly limited as long as it is 2 or more, it is preferably 5 or more, more preferably 8 or more, and even more preferably 10 or more. Furthermore, n may be, for example, 35 or less, preferably 30 or less, and even more preferably 25 or less.

[0122] The ratio of the structural unit (1-1) to the structural unit (1-2) is not particularly limited, and may be appropriately changed so as to satisfy, for example, at least one (preferably two or more, more preferably all three) of the above formulas (1) to (3).

[0123] In the polyether-modified polydimethylsiloxane, the ratio (C2 / C1) of the content C2 of the structural unit (1-2) to the content C1 of the structural unit (1-1) may be, for example, 0.01 or more, 0.02 or more, or 0.03 or more. The ratio (C2 / C1) may be, for example, 0.3 or less, 0.25 or less, or 0.2 or less.

[0124] The terminals of the polyether-modified polydimethylsiloxane (that is, the terminals of the polydimethylsiloxane) are not particularly limited, but are preferably trialkylsilyl groups, and more preferably trimethylsilyl groups.

[0125] The weight average molecular weight of the polyether-modified polydimethylsiloxane may be, for example, 100 or more, preferably 200 or more, and more preferably 500 or more. The weight average molecular weight of the polyether-modified polydimethylsiloxane may be, for example, 100,000 or less, preferably 50,000 or less, and more preferably 10,000 or less.

[0126] The amount of polyether-modified polydimethylsiloxane may be, for example, 0.001 parts by mass or more, preferably 0.005 parts by mass or more, more preferably 0.01 parts by mass or more, and even more preferably 0.02 parts by mass or more, relative to 100 parts by mass of the silane compound. This tends to further improve the uniformity of the surface. Furthermore, the amount of polyether-modified polydimethylsiloxane may be, for example, 2.0 parts by mass or less, preferably 1.0 parts by mass or less, more preferably 0.7 parts by mass or less, and even more preferably 0.5 parts by mass or less, relative to 100 parts by mass of the silane compound. This reduces the production cost of the polyether-modified polydimethylsiloxane, thereby enabling the cost of the barrier material to be reduced.

[0127] The composition of this embodiment may further contain a liquid medium. The liquid medium to be contained in the composition of this embodiment may be the liquid medium used in the hydrolysis reaction. That is, the liquid medium used in the hydrolysis reaction may be contained in the composition of this embodiment together with the hydrolysis polycondensate. Examples of the liquid medium include the same as those mentioned above.

[0128] The content of the liquid medium in the composition is not particularly limited, and may be, for example, a content that provides a viscosity of the composition suitable for application. The viscosity of the composition is not particularly limited, and may be adjusted as appropriate depending on the thickness of the barrier material to be produced, the application method, the shape of the target object, etc.

[0129] The viscosity of the composition at 25° C. may be, for example, 1 to 6000 mPa·s, and preferably 5 to 3000 mPa·s. Such a composition makes it easier to apply to an object and form a barrier material on the object.

[0130] The composition of this embodiment may further contain other components in addition to those described above. Examples of such other components include resins having hydroxyl groups in their molecular structure, metal oxide particles, and metal oxide fibers. Examples of resins having hydroxyl groups in their molecular structure include polyvinyl alcohol. Examples of metal oxide particles include silica particles and alumina particles, and these particles are preferably nano-sized (e.g., particle diameters of 1 nm or more and less than 1000 nm) (i.e., nanosilica particles and nanoalumina particles are preferred). Examples of metal oxide fibers include alumina fibers, and these metal oxide fibers preferably have a nano-sized fiber diameter (e.g., fiber diameters of 1 nm or more and less than 1000 nm) (i.e., alumina nanofibers are preferred).

[0131] The amount of the other components is not particularly limited as long as the effects described above are obtained, and may be, for example, 50 parts by mass or less, and preferably 40 parts by mass or less, per 100 parts by mass of the silane compound. The amount of the other components may be, for example, 10 parts by mass or more, or 20 parts by mass or more, per 100 parts by mass of the silane compound.

[0132] The composition according to this embodiment can be produced by the following method. <Method of producing the composition> This production method comprises a first step of heating the above-mentioned silane compound in the presence of an acid catalyst to obtain a hydrolysis polycondensate of the silane compound, and a second step of mixing the hydrolysis polycondensate of the silane compound, a curing catalyst, and a polyether-modified polydimethylsiloxane.

[0133] The first step is to hydrolyze the silane compound by heating in the presence of an acid catalyst. Suitable conditions for the hydrolysis reaction are as described above.

[0134] The second step is a step of obtaining a composition by mixing the hydrolysis polycondensate obtained in the first step, a curing catalyst, a polyether-modified polydimethylsiloxane, and, if necessary, further other components. The mixing method in the second step is not particularly limited, and any known method may be used.

[0135] <Barrier material> The barrier material of this embodiment may be a cured product of the above-mentioned barrier material-forming composition. This barrier material may also be formed by heating the above-mentioned barrier material-forming composition. The heating further polymerizes the hydrolysis polycondensate of the silane compound in the composition, forming a polysiloxane compound.

[0136] The barrier material has a low water vapor permeability and is excellent in moisture resistance. The water vapor permeability (40°C, 95% RH) of the barrier material per 25 μm thickness is, for example, 5000 g / m 2 -day or less, 4000g / m 2·day or less, and 3000g / m 2 It is even more preferable that it is 10 days or less.

[0137] The water vapor permeability (40°C, 95% RH) of the barrier material per 25 μm thickness is, for example, 100 g / m 2 -day or more, 500g / m 2 Such a barrier material has moisture-wicking properties, and can sufficiently prevent damage caused by expansion of moisture that penetrates inside, even when used in a high-temperature environment.

[0138] The water vapor permeability of the barrier material is a value measured by the moisture sensor method (Lyssy method) in accordance with JIS K7129.

[0139] The barrier material may be transparent. Such a barrier material is suitable for applications requiring transparency, such as a covering material for covering an image sensor in an image sensor package. Here, transparency means that the visible light transmittance (light transmittance at 550 nm) per mm of thickness is 80% or more.

[0140] The barrier material preferably has a visible light transmittance (550 nm light transmittance) per mm of thickness of 80% or more, more preferably 85% or more, and even more preferably 90% or more. The visible light transmittance of the barrier material is measured using a spectrophotometer.

[0141] The barrier material has excellent insulating properties and can be suitably used in applications where insulating properties are required, such as a moisture-proof barrier material for electronic components.

[0142] The volume resistivity of the barrier material is, for example, 1×10 10 Ωcm or more, and from the viewpoint of ensuring sufficient insulation as a moisture-proof barrier material for electronic components, it is 1×10 12 Ωcm or more is preferable, 1×10 14 The volume resistivity of the barrier material is preferably 1×1019 Ωcm or less, and may be 1×10 18 In this specification, the volume resistivity of the barrier material is a value measured in accordance with JIS K 6911.

[0143] The dielectric breakdown strength of the barrier material may be, for example, 10 kV / mm or more, and from the viewpoint of ensuring sufficient insulation properties as a moisture-proof barrier material for electronic components, it is preferably 50 kV / mm or more, more preferably 100 kV / mm or more. Furthermore, the dielectric breakdown strength of the barrier material may be, for example, 1000 kV / mm or less, or may be 500 kV / mm or less. In this specification, the dielectric breakdown strength of the barrier material refers to a value measured in accordance with JIS C 2110.

[0144] The barrier material has excellent heat resistance and can be suitably used in applications requiring heat resistance, such as a moisture-proof barrier material for electronic components that undergo high-temperature processes (e.g., a reflow process) during mounting. The barrier material can be suitably used, for example, as a moisture-proof barrier material that is placed on a component before heating in a reflow furnace and then subjected to the reflow furnace together with the component. Because the barrier material has excellent heat resistance, it can still exhibit sufficient moisture-proof properties even after heating in a reflow furnace.

[0145] 5% weight loss temperature (T d5 ) may be, for example, 260°C or higher, preferably 280°C or higher, and more preferably 300°C or higher. The 5% weight loss temperature of the barrier material may be, for example, 500°C or lower, or 450°C or lower. In this specification, the 5% weight loss temperature of the barrier material is a value measured using a thermogravimetric differential thermal analyzer.

[0146] The shape of the barrier material is not particularly limited. The barrier material may be formed, for example, into a film, and such a barrier material can be used as a moisture-proof barrier film. The barrier material may be formed so as to fill gaps between members, in which case it can prevent moisture from entering through the gaps. The barrier material may be formed so as to cover members, in which case it can prevent the members from coming into contact with moisture.

[0147] <Barrier material manufacturing method> The method for producing a barrier material according to this embodiment includes a heating step of heating the composition to form a barrier material, in which the hydrolysis polycondensate of the silane compound in the composition is further polymerized by heating to form a polysiloxane compound.

[0148] In the heating step, the liquid medium in the composition may be removed by heating, i.e., the heating step may be a step of forming a barrier material containing a polysiloxane compound by drying the composition by heating.

[0149] The heating temperature in the heating step is not particularly limited, as long as it is a temperature at which the silane oligomer can be polymerized. Furthermore, when the composition contains a liquid medium, the heating temperature is preferably a temperature at which the liquid medium volatilizes. The heating temperature may be, for example, 70°C or higher, preferably 100°C or higher. The heating temperature may be, for example, 200°C or lower, preferably 180°C or lower.

[0150] The present manufacturing method may further include a coating step of coating the composition. In this case, the heating step can be said to be a step of heating the coated composition.

[0151] The method for applying the composition is not particularly limited, and may be changed as appropriate depending on the shape of the object to be coated, the thickness of the barrier material, etc.

[0152] In this manufacturing method, the composition may be applied to an object to which moisture resistance is to be imparted, thereby forming a barrier material on the object. Alternatively, in this manufacturing method, a barrier material having a predetermined shape may be manufactured, and then the manufactured barrier material may be applied to the object.

[0153] <Barrier material applications> The use of the barrier material according to this embodiment is not particularly limited, and the barrier material can be suitably used in various applications requiring moisture resistance. For example, the barrier material can be suitably used as a moisture-proof barrier material for electronic components.

[0154] The barrier material according to this embodiment has excellent moisture-proof properties even in high-temperature environments (e.g., 100°C or higher). Therefore, the barrier material according to this embodiment can be suitably used in applications such as a moisture-proof barrier material for electronic components used in high-temperature environments and a moisture-proof barrier material for electronic components that undergo high-temperature processes during mounting. Specifically, the barrier material according to this embodiment can be suitably used as a moisture-proof barrier material for power semiconductors, image sensors, displays, etc.

[0155] A preferred embodiment of the use of the barrier material will be described in detail below, but the use of the barrier material is not limited to the following.

[0156] <Application example 1> One embodiment of the present invention relates to a product having a moisture-proof treated member. Such a product includes a member and a barrier material formed on the member. The barrier material may be formed on one member or on multiple members. For example, the barrier material may be formed to cover one or multiple members, or may be formed to cover a joint between two members.

[0157] Such a product is produced by a manufacturing method comprising a first step of applying the above-mentioned barrier material-forming composition onto a member and a second step of heating the applied composition to form a barrier material on the member. This manufacturing method may further comprise a step of exposing the moisture-proof treated member to high temperatures (e.g., reflow soldering, thermal curing of chip bonds, drying of materials by heating, etc.).

[0158] Specific examples of such applications include the following electronic components:

[0159] (Electronic parts A-1) An electronic component according to one embodiment includes a substrate, a cover glass, an image sensor disposed between the substrate and the cover glass, a support member that supports the cover glass and the image sensor on the substrate, and the above-mentioned barrier material provided on the joint between the cover glass and the support member.

[0160] Such electronic components can be manufactured, for example, by a manufacturing method including a coating step of applying a barrier material-forming composition to the joint between the support member and the cover glass, and a barrier material-forming step of heating the applied composition to form a barrier material on the joint.

[0161] (Electronic Parts A-2) According to one embodiment, an electronic component includes a substrate, an image sensor disposed on the substrate, and the barrier material provided on the image sensor.

[0162] The barrier material can be excellent in moisture resistance and transparency. Therefore, the barrier material can be suitably used as an encapsulant for encapsulating an image sensor. Such an electronic component can be used to construct an image sensor package without using a cover glass, which is expected to reduce the component size and improve handling.

[0163] In this application, the visible light transmittance (550 nm) of the barrier material per mm of thickness is preferably 95% or more, more preferably 97% or more, and even more preferably 99% or more.

[0164] Such electronic components can be manufactured, for example, by a manufacturing method including a coating step of coating a barrier material-forming composition on an image sensor, and a barrier material-forming step of heating the coated composition to form a barrier material on the image sensor.

[0165] <Application example 2> One embodiment of the present invention relates to a product having a first member and a second member joined to the first member, the joint between the first member and the second member being moisture-proofed. Such a product includes the first member, the second member, and a barrier material provided between the first member and the second member, and the first member and the second member are joined via the barrier material.

[0166] Such a product can be produced by a manufacturing method comprising: a first step of disposing a barrier material-forming composition between a first member and a second member; and a second step of heating the composition to form a barrier material and bonding the first member and the second member together via the barrier material. This manufacturing method may further comprise a step of exposing the first member and the second member bonded together via the barrier material to high temperatures (e.g., reflow soldering, thermal curing of chip bonds, drying of materials by heating, etc.).

[0167] Specific examples of such applications include the following electronic components:

[0168] (Electronic parts B-1) An electronic component according to one embodiment includes a substrate, a cover glass, an image sensor disposed between the substrate and the cover glass, a support member that supports the cover glass and the image sensor on the substrate, and a barrier material that bonds the cover glass and the support member.

[0169] Such electronic components can be manufactured, for example, by a manufacturing method including the steps of placing a barrier material-forming composition between a support member and a cover glass, heating the composition to form a barrier material, and bonding the support member and the cover glass via the barrier material.

[0170] <Application example 3> One aspect of the invention relates to a product comprising a moisture barrier member. Such a product may be, for example, an assembly of multiple components including the moisture barrier member, and may be made of a barrier material.

[0171] Such a product can be produced by a manufacturing method comprising a first step of heating the barrier material-forming composition to produce a moisture-proof member made of a barrier material, and a second step of assembling a plurality of members including the moisture-proof member. This manufacturing method may further comprise a step of exposing the assembly obtained in the second step to high temperatures (e.g., reflow soldering, thermal curing of chip bonds, drying of materials by heating, etc.).

[0172] Specific examples of such applications include the following electronic components:

[0173] (Electronic parts C-1) According to one embodiment, an electronic component includes a substrate, at least one component selected from the group consisting of a MEMS sensor, a wireless module, and a camera module, and a moisture-proof member having a barrier material.

[0174] The barrier material has excellent moisture resistance, and therefore the electronic component has excellent moisture resistance, and degradation of sensing characteristics due to moisture absorption is sufficiently prevented.

[0175] Such electronic components can be manufactured by a manufacturing method including the steps of: preparing a moisture-proof member having a barrier material by heating a barrier material-forming composition; and assembling a plurality of components including the moisture-proof member. Here, the barrier material may be formed independently of the substrate and the component, or may be formed integrally with the component by heating the barrier material-forming composition applied to the component.

[0176] Although the preferred embodiments of the present invention have been described above, the present invention is not limited to the above embodiments. [Example]

[0177] (solution 13 C-NMR measurement conditions) Device name: JEOL RESONANCE ECX400II Observed nucleus: 13C Observation frequency: 10.052MHz Measurement temperature: room temperature (23℃) Measurement solvent: CDCl3 Pulse width: 11.4 μsec (45°) Pulse repetition time: 2.0 seconds Accumulation count: 700 times Sample concentration (sample / measurement solvent): 100 mg / 1.0 ml

[0178] (solution 1 H-NMR measurement conditions) Device name: JEOL RESONANCE ECX400II Observed nucleus: 1H Observation frequency: 399.78MHz Measurement temperature: room temperature (23℃) Measurement solvent: CDCl3 Pulse width: 6.64 μsec (90°) Pulse repetition time: 5.0 seconds Number of times: 8 Sample concentration (sample / measurement solvent): 10 mg / 1.0 ml

[0179] Example 1 <Preparation of polyether-modified polydimethylsiloxane> As a polyether-modified polydimethylsiloxane, N2 / N1 is 2.6, S C2 / S C1 is 2.6, S H2 / S H1 A polyether-modified polydimethylsiloxane having a viscosity of 1.2 (hereinafter also referred to as polyether-modified polydimethylsiloxane (S-1)) was prepared.

[0180] <Preparation of Barrier Material-Forming Composition> 10 parts by mass of 2-BuOH (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.), 64.9 parts by mass of silane oligomer (manufactured by Shin-Etsu Chemical Co., Ltd., product name: X-40-9227), 14.3 parts by mass of methyltrimethoxysilane (manufactured by Shin-Etsu Chemical Co., Ltd., product name: KBM-13, hereinafter abbreviated as "MTMS"), 2.0 parts by mass of linear polysiloxane (manufactured by Momentive Performance Materials Japan, LLC, product name: YF3800, kinematic viscosity at 25°C: 80 mm 2 A mixture of 0.1 parts by mass of nitric acid and 11.3 parts by mass of water was mixed and reacted at 70°C for 1 hour while stirring with a stirrer. Next, 0.28 parts by mass of a nickel catalyst (manufactured by Momentive Performance Materials Japan, LLC, product name: CR12, solids content: 12% by mass), 0.02 parts by mass of an aluminum catalyst (aluminum alkylacetoacetate diisopropylate, manufactured by Matsumoto Fine Chemical Co., Ltd., product name: Aluminum Chelate M), and 0.5 parts by mass of polyether-modified polydimethylsiloxane (S-1) were added and mixed to obtain a barrier material-forming composition.

[0181] Example 2 As a polyether-modified polydimethylsiloxane, N2 / N1 is 3.5, S C2 / S C1 3.5, S H2 / S H1A polyether-modified polydimethylsiloxane (hereinafter also referred to as polyether-modified polydimethylsiloxane (S-2)) having a viscosity index of 1.6 was prepared. A barrier material-forming composition was obtained in the same manner as in Example 1, except that the polyether-modified polydimethylsiloxane (S-1) was replaced with the polyether-modified polydimethylsiloxane (S-2).

[0182] (Comparative Example 1) As a polyether-modified polydimethylsiloxane, N2 / N1 is 6.2, S C2 / S C1 is 6.2, S H2 / S H1 A polyether-modified polydimethylsiloxane (hereinafter also referred to as polyether-modified polydimethylsiloxane (X-1)) having a viscosity index of 2.9 was prepared. A barrier material-forming composition was obtained in the same manner as in Example 1, except that the polyether-modified polydimethylsiloxane (S-1) was changed to the polyether-modified polydimethylsiloxane (X-1).

[0183] (Comparative Example 2) As a polyether-modified polydimethylsiloxane, N2 / N1 is 4.4, S C2 / S C1 is 4.4, S H2 / S H1 A polyether-modified polydimethylsiloxane (hereinafter also referred to as polyether-modified polydimethylsiloxane (X-2)) having a viscosity index of 1.9 was prepared. A barrier material-forming composition was obtained in the same manner as in Example 1, except that the polyether-modified polydimethylsiloxane (S-1) was changed to the polyether-modified polydimethylsiloxane (X-2).

[0184] (Evaluation method) The barrier material-forming compositions obtained in the examples and comparative examples were evaluated for moisture resistance (moisture absorption rate) and visibility by the following methods. The results are shown in Table 1.

[0185] <Moisture resistance (moisture absorption rate)> One side of a 0.4 mm thick copper-clad laminate MCL-E-700G (Hitachi Chemical Co., Ltd., product name) was masked, and the copper foil on one side was removed by immersion in a copper etching solution to produce a 40 mm square base substrate. Next, a barrier material-forming composition was applied to the side of the base substrate from which the copper foil had been removed so that the thickness after drying would be 30 μm, and the composition was dried at 150°C for 1 hour using a safety oven (Espec Corporation, product name: SPHH-202). This formed a barrier material on the substrate, yielding an evaluation substrate with a barrier material. The evaluation substrate with the barrier material was dried at 150°C for 1 hour using a safety oven (manufactured by Espec Corporation, product name: SPHH-202) to obtain a measurement sample. The mass of the obtained measurement sample was measured to determine the initial mass m4. Next, a constant temperature and humidity chamber (manufactured by Kato Corporation, product name: SE-44CI-A) was used to treat the sample in an atmosphere of 85°C / 85% RH for 120 hours to obtain a sample after constant temperature and humidity treatment. The mass of the measurement sample after constant temperature and humidity treatment was measured to determine the mass after constant temperature and humidity treatment m5. The moisture absorption rate QB (%) was calculated from the initial mass m4 and the mass after constant temperature and humidity treatment m5 using the following formula. QB = 100 × (m5 - m4) / m4

[0186] <Visibility> The barrier material-forming composition was applied to a three-terminal regulator (SOT-89 NJM78L05UA, manufactured by New Japan Radio Co., Ltd.) so that the thickness after drying would be 30 μm, and then dried at 150°C for 1 hour using a safety oven (manufactured by Espec Corporation, product name: SPHH-202). Thereafter, a visual evaluation was performed to determine whether the label on the three-terminal regulator could be recognized.

[0187] [Table 1]

Claims

1. The composition includes a mixture of a hydrolysis polycondensate of a silane compound containing a silane oligomer and a silane monomer, a curing catalyst, and a polyether-modified polydimethylsiloxane, The polyether-modified polydimethylsiloxane １ In the H-NMR spectrum, a peak P corresponds to a hydrogen atom on a carbon atom bonded to a silicon atom. Ｈ１ Peak area S Ｈ１ Peak P corresponding to hydrogen atoms on carbon atoms bonded to oxygen atoms Ｈ２ Peak area S Ｈ２ The ratio (S Ｈ２ / S Ｈ１ ) is 1.0 to 1.

8.

2. The composition of claim 1 , wherein the silane oligomer has a silicon atom bonded to three oxygen atoms.

3. 3. The composition according to claim 1, wherein the ratio of the total number of silicon atoms bonded to three oxygen atoms and silicon atoms bonded to four oxygen atoms to the total number of silicon atoms in the silane oligomer is 30% or more.

4. The composition according to any one of claims 1 to 3, wherein the silane monomer comprises at least one selected from the group consisting of alkyltrialkoxysilanes, aryltrialkoxysilanes, and tetraalkoxysilanes.

5. The composition according to any one of claims 1 to 4, wherein the content of the silane monomer in the silane compound is 5 to 40 parts by mass per 100 parts by mass of the silane oligomer.

6. The composition according to any one of claims 1 to 5, wherein the silane compound further comprises a linear polysiloxane.

7. The linear polysiloxane has a kinematic viscosity of 50 mm at 25°C. ２ The composition of claim 6, wherein the .lambda. / s or more.

8. 8. The composition according to claim 6, wherein the linear polysiloxane has a diorganopolysiloxane chain.

9. The composition according to any one of claims 6 to 8, wherein the linear polysiloxane has groups selected from the group consisting of silanol groups and alkoxy groups at both ends thereof.

10. The composition according to any one of claims 6 to 9, wherein the content of the linear polysiloxane in the silane compound is 1 to 30 parts by mass per 100 parts by mass of the silane oligomer.

11. A method for producing a composition according to any one of claims 1 to 10, comprising the steps of: a step of heating the silane compound in the presence of an acid catalyst to obtain the hydrolysis polycondensate; mixing the hydrolysis polycondensate, the curing catalyst, and the polyether-modified polydimethylsiloxane; A manufacturing method comprising:

12. The method according to claim 11, wherein the acid catalyst comprises at least one selected from the group consisting of acetic acid, phosphoric acid, hydrochloric acid, and nitric acid.

13. A method for producing a barrier material, comprising the step of curing the composition according to any one of claims 1 to 10 to form a barrier material.

14. A method for manufacturing a product having a moisture-proof treated member, comprising: A first step of applying the composition according to any one of claims 1 to 10 onto a member; a second step of curing the applied composition to form a barrier material on the member; A manufacturing method comprising:

15. A method for manufacturing a product having a first member and a second member joined to the first member, wherein a joint between the first member and the second member is subjected to moisture-proofing treatment, A first step of disposing the composition according to any one of claims 1 to 10 between a first member and a second member; a second step of curing the composition to form a barrier material and bonding the first member and the second member via the barrier material; A manufacturing method comprising:

16. A method for manufacturing a product including a moisture-proof member, a first step of curing the composition according to any one of claims 1 to 10 to produce a moisture-proof member having a barrier material; a second step of assembling a plurality of members including the moisture-proof member; A manufacturing method comprising:

17. A barrier material which is a cured product of the composition according to any one of claims 1 to 10.

18. The components and The barrier material of claim 17 formed on the member; A product comprising:

19. A barrier material according to claim 17, comprising: a first member; a second member; and the barrier material according to claim 17 disposed between the first member and the second member; A product in which the first member and the second member are bonded together via the barrier material.

20. 20. An article of manufacture that is an assembly of multiple components including a moisture barrier component having the barrier material of claim 17.

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