Vicular layer, method for producing void layer, laminate, optical member, and optical device

Abstract

The present disclosure provides a void layer having a low refractive index and excellent mechanical strength. A void layer (11) according to the present disclosure is a void layer in which pulverized materials of a gel-like silicon compound are chemically bonded, the gel-like silicon compound is a compound in which silane compounds are condensed or partially condensed, the silane compounds include a 1-trifunctional silane compound and a tetrafunctional silane compound, and the refractive index of the void layer (11) is 1.30 or less.

Description

TECHNICAL FIELD

[0001] The present disclosure relates to a void layer, a method for manufacturing a void layer, a laminate, an optical member, and an optical device. BACKGROUND

[0002] For optical devices, a scheme using a low refractive index layer as a total reflection layer has been proposed, for example. In Patent Literature 1, for example, a laminate in which a layer having a lower refractive index than a light guide plate is interposed between the light guide plate and a reflection plate is disclosed. As the low refractive index layer, for example, in order to make the refractive index as low as possible close to that of air, a void layer having voids can be used.

[0003] PRIOR ART DOCUMENTS

[0004] PATENT LITERATURE

[0005] Patent Literature 1: Japanese Patent Application Laid-Open No. 10-62626 SUMMARY

[0006] PROBLEMS TO BE SOLVED BY THE INVENTION

[0007] As described above, the void layer is a layer having voids. In general, as for the refractive index of the void layer, there is a tendency that the more the void ratio of the void layer is increased, the lower the refractive index becomes. On the other hand, in the case where the void ratio of the void layer is increased, there is a tendency that the mechanical strength of the void layer becomes low. That is, the refractive index of the void layer and the mechanical strength of the void layer are in a trade-off relationship. Therefore, it is desirable to realize a void layer which is low in refractive index and high in mechanical strength.

[0008] Therefore, an object of the present disclosure is to provide a void layer which is low in refractive index and excellent in mechanical strength, a method for manufacturing a void layer, a laminate, an optical member, and an optical device.

[0009] METHOD FOR SOLVING THE PROBLEM

[0010] In order to achieve the above object, the void layer of the present disclosure is a void layer in which a pulverized product of a gel-like silicon compound is chemically bonded,

[0011] The above gel-like silicon compound is a compound in which a silane compound undergoes condensation or partial condensation,

[0012] As the above silane compound, a 1-3 functional silane compound and a 4 functional silane compound are included,

[0013] The above void layer has a refractive index of 1.30 or less.

[0014] The void layer of the present disclosure is a void layer in which a pulverized product of a gel-like silicon compound is chemically bonded in the presence of an additive,

[0015] The above gel-like silicon compound is a compound synthesized by condensation or partial condensation of a silane compound,

[0016] As the above additive, at least one of a cross-linking reaction promoter and a precursor thereof, and a cross-linking auxiliary agent are included,

[0017] The total content ratio of the above cross-linking reaction promoter and the precursor thereof is 1.5 mol% or more, and the total content ratio of the above cross-linking auxiliary agent is 2.0 mol% or more, with respect to the total amount of the above silane compounds,

[0018] The above void layer has a refractive index of 1.30 or less.

[0019] The manufacturing method of the void layer of the present disclosure includes a gel-like silica synthesis step, a gel pulverization step, and a bonding step,

[0020] The above gel-like silica synthesis step includes a step of synthesizing a gel-like silicon compound by condensation or partial condensation of a silane compound,

[0021] The above silane compound includes a 1-3 functional silane compound and a 4 functional silane compound,

[0022] The above gel pulverization step includes a step of pulverizing the above gel-like silicon compound to obtain a pulverized product,

[0023] The above bonding step includes a step of chemically bonding the above pulverized product.

[0024] The manufacturing method of the void layer of the present disclosure includes a gel-like silica synthesis step, a gel pulverization step, and a bonding step,

[0025] The above gel-like silica synthesis step includes a step of synthesizing a gel-like silicon compound by condensation or partial condensation of a silane compound,

[0026] The above gel pulverization step includes a step of pulverizing the above gel-like silicon compound to obtain a pulverized product,

[0027] The above bonding step includes a step of chemically bonding the above pulverized product in the presence of an additive,

[0028] As the above additive, at least one of a cross-linking reaction promoter and a precursor thereof, and a cross-linking auxiliary agent are included.

[0029] The laminate of the present disclosure includes the void layer of the present disclosure and an adhesive bonding layer,

[0030] The above adhesive bonding layer is directly laminated to one face or both faces of the above void layer.

[0031] The optical member of the present disclosure includes the void layer of the present disclosure or the laminate of the present disclosure.

[0032] The optical device of the present disclosure includes the optical member of the present disclosure.

[0033] Effects of the Invention

[0034] According to the present disclosure, it is possible to provide a void layer having low refractive index and excellent mechanical strength, a method for manufacturing a void layer, a laminate, an optical member, and an optical device. BRIEF DESCRIPTION OF DRAWINGS

[0035] Figure 1 (a) and (b) are cross-sectional views illustrating the constitution of the laminate of the present disclosure.

[0036] Figure 2 (a) and (b) are cross-sectional views illustrating another example of the constitution of the laminate of the present disclosure.

[0037] Figure 3 (a) and (b) are cross-sectional views illustrating still another example of the constitution of the laminate of the present disclosure.

[0038] Figure 4 is a graph showing the relationship between the peeling strength and the refractive index.

[0039] SYMBOL DESCRIPTION

[0040] 10, 10a, 10b, 10c, 10d, 10e Laminate

[0041] 11 Void layer

[0042] 12 Adhesive bonding layer

[0043] 13 Intermediate layer

[0044] 14 Substrate DETAILED DESCRIPTION

[0045] Next, the present disclosure will be described more specifically by way of example. However, the present disclosure is not limited in any way by the following description.

[0046] In the present disclosure, the "adhesive-bonding layer" refers to a layer formed of at least one of an adhesive and a bonding agent. In the present disclosure, the "adhesive-bonding layer" can be an "adhesive layer" formed of an adhesive, or can be a "bonding agent layer" formed of a bonding agent, or can be a layer containing both an adhesive and a bonding agent, unless otherwise specified. In addition, in the present disclosure, an adhesive and a bonding agent are sometimes collectively referred to as an "adhesive-bonding agent". In general, an agent having a relatively weak adhesive force or bonding force (for example, an agent capable of allowing re-stripping of a bonded object) is sometimes referred to as an "adhesive", and an agent having a relatively strong adhesive force or bonding force (for example, an agent incapable of allowing re-stripping of a bonded object, or an agent for which re-stripping of a bonded object is extremely difficult) is sometimes referred to as a "bonding agent" to distinguish between the two. In the present disclosure, an adhesive and a bonding agent are not clearly distinguished. In addition, in the present disclosure, an "adhesive force" and a "bonding force" are not clearly distinguished.

[0047] In the present disclosure, "on" or "on a surface" can be in a state of direct contact with the upper or the surface, or can be in a state of being interposed with other layers or the like.

[0048] In the present disclosure, the "interlayer" refers to any portion contained between one layer and other layers, including the one layer and the other layers. That is, for example, in the case of referring to the interlayer of one layer and other layers, it can be any portion of the one layer, or any portion of the other layers, or any portion of another layer contained between the one layer and the other layers. In addition, it can be a boundary portion of any two layers among the one layer, the other layers, and the another layer.

[0049] [1. Void layer, laminate]

[0050] As described above, the void layer of the present disclosure is a void layer in which pulverized products of a gel-like silicon compound are chemically bonded, the gel-like silicon compound being a compound in which a silane compound has undergone condensation or partial condensation, and the void layer has a refractive index of 1.30 or less. In addition, as another aspect, the void layer of the present disclosure is a void layer in which pulverized products of a gel-like silicon compound are chemically bonded in the presence of an additive, the gel-like silicon compound being a compound in which a silane compound has undergone condensation or partial condensation, and the additive containing at least one of a cross-linking reaction promoter and a precursor thereof, and a cross-linking auxiliary agent, the total content ratio of the cross-linking reaction promoter and the precursor thereof being 1.5 mol% or more, and the total content ratio of the cross-linking auxiliary agent being 2.0 mol% or more, with respect to the total amount of the silane compound, and the void layer having a refractive index of 1.30 or less. The use mode of the void layer of the present disclosure is not particularly limited, and for example, it can be used in the above-described laminate of the present disclosure or the like.

[0051] Further, as described above, the laminate of the present disclosure includes the void layer of the present disclosure and the adhesive bonding layer. The above-described adhesive bonding layer is directly laminated to one face or both faces of the above-described void layer. In the present disclosure, the above-described adhesive bonding layer is "directly laminated" to the above-described void layer, for example, can be that the above-described adhesive bonding layer is in direct contact with the above-described void layer, or can be that the above-described adhesive bonding layer is laminated to the above-described void layer with the above-described intermediate layer interposed therebetween.

[0052] Figure 1 The cross-sectional view of (a) shows an example of the configuration in the laminate of the present disclosure. As shown in the figure, the laminate 10 has the adhesive bonding layer 12 directly laminated to one face of the void layer 11. Here, the void layer 11 is a void layer in which the pulverized product of the gel-like silicon compound is chemically bonded. Further, the above-described gel-like silicon compound is a compound in which a silane compound has undergone condensation or partial condensation. As the above-described silane compound, a 1-3 functional silane compound and a 4 functional silane compound are included, and the proportion of the above-described 4 functional silane compound is 1 to 25 mol% with respect to the amount of the above-described 1-3 functional silane compound. The void layer 11 has a refractive index of 1.30 or less.

[0053] Further, Figure 1 The cross-sectional view of (b) shows another example of the configuration in the laminate of the present disclosure. As shown in the figure, the laminate 10a has the adhesive bonding layer 12 directly laminated to both faces of the void layer 11.

[0054] Further, as described above, the laminate of the present disclosure can have an intermediate layer between the above-described void layer and the above-described adhesive bonding layer, and the above-described intermediate layer is a layer formed by the above-described void layer and the above-described adhesive bonding layer being integrated. Figure 2 Examples of such a laminate of the present disclosure are shown. As shown in the figures, Figure 2 The laminate 10b of (a) has the adhesive bonding layer 12 directly laminated to one face of the void layer 11. The laminate 10b is the same as the laminate 10 of (a) except that there is an intermediate layer 13 between the void layer 11 and the adhesive bonding layer 12. Figure 1 The laminate 10 of (a). The intermediate layer 13 is a layer formed by the void layer 11 and the adhesive bonding layer 12 being integrated. As shown in the figure, Figure 2 The laminate 10c of (b) has the adhesive bonding layer 12 directly laminated to both faces of the void layer 11. The laminate 10c is the same as the laminate 10a of (b) except that there is an intermediate layer 13 between the void layer 11 and each of the adhesive bonding layers 12. Figure 1 The laminate 10a of (b). The intermediate layer 13 is a layer formed by the void layer 11 and the adhesive bonding layer 12 being integrated. Figure 2 The laminate of (a) is also a layer formed by the void layer 11 and the adhesive bonding layer 12 being integrated.

[0055] Furthermore, the laminate disclosed herein may or may not include other constituent elements besides the aforementioned void layer, adhesive layer, and intermediate layer. The aforementioned other constituent elements are not particularly limited, and may, for example, be a substrate. The aforementioned substrate is also not particularly limited; for example, as described later, it may be a film (e.g., a resin film), a glass plate, etc. Figure 3 An example of such a stacked body of the present disclosure is shown. As shown in the figure, Figure 3 In addition to having a substrate 14 directly contacting the surface of the void layer 11 opposite to the adhesive layer 12 and the surface of the adhesive layer 12 opposite to the void layer 11 respectively, the laminate 10d in (a) is also provided with... Figure 2 (a) is identical to layer 10b. As shown in the figure. Figure 3 (b) The laminate 10e, except that the substrate 14 is provided in direct contact with the adhesive layers 12 on both sides opposite to the void layer 11, is in contact with... Figure 3 (b) is the same as the laminate 10c. Figure 3 (a) and Figure 3 In (b), substrates 14 are provided on both sides of the laminate. However, this disclosure is not limited to this; for example, substrates 14 may be provided on only one side. Additionally, in Figure 3 (a) and Figure 3 In (b), a substrate 14 is provided in direct contact with the void layer 11 or the adhesive layer 12. However, this disclosure is not limited to this; for example, other constituent elements may exist between the substrate 14 and the void layer 11 or the adhesive layer 12. These other constituent elements are not particularly limited; for example, they may be optical functional layers. These optical functional layers are also not particularly limited; they may be, for example, optical functional layers used in conventional optical films, or, for example, microlens films, prism films, diffusion films, polarizing films, phase refraction films, high refractive index layers, etc.

[0056] As described above, the porous layer of this disclosure is a porous layer formed by chemically bonding fragments of a gel-like silicon compound. By using the fragments of the aforementioned gel-like silicon compound, the three-dimensional structure of the gel-like silicon compound is disrupted, forming a new three-dimensional structure different from that of the aforementioned gel-like silicon compound. In this way, the aforementioned porous layer becomes a layer with a new pore structure (new porous structure) that cannot be obtained by a layer formed from the aforementioned gel-like silicon compound, thereby forming a nanoscale porous layer with high porosity. Furthermore, when the aforementioned porous layer is, for example, a gel-like silicon compound, the fragments are chemically bonded together while adjusting the number of siloxane bond functional groups in the aforementioned gel-like silicon compound. Here, "gel-like silicon compound" refers to a porous polymer containing siloxane bonds, such as a porous body containing silsesquioxanes as structural units. Furthermore, since chemical bonding (e.g., cross-linking) occurs during the bonding process after a new three-dimensional structure is formed as a precursor to the aforementioned porous layer, the porous layer, for example, in the case of a functional porous body, has a structure with voids but can maintain sufficient strength and flexibility. Therefore, according to this disclosure, a porous layer can be easily and conveniently applied to various objects.

[0057] In the porous layer of this disclosure, the manner in which the aforementioned fragments are chemically bonded (through chemical bonds) is not particularly limited. Specific examples of such chemical bonds include covalent bonds, ionic bonds, and metallic bonds. For example, the fragments can be cross-linked with each other through covalent bonds (cross-linking bonds). Furthermore, the chemical bonds (e.g., the aforementioned cross-linking bonds) of the fragments can be formed by the fragments directly bonding with each other, or indirectly bonding them through other substances such as cross-linking aids, linkers, or spacers. It should be noted that the method for chemically bonding the fragments is as described later in the section on the manufacturing method of the porous layer.

[0058] The aforementioned crosslinking bonds are, for example, siloxane bonds. Examples of siloxane bonds include, for example, T2, T3, and T4 bonds, as shown below. In the case of the aforementioned gel-like silicon compound having siloxane bonds, for example, it can have any one type of bond, any two types of bonds, or all three types of bonds. Among the aforementioned siloxane bonds, a higher ratio of T2 and T3 results in greater flexibility and a better expectation of the original gel properties, but the film strength becomes weaker. On the other hand, a higher ratio of T4 in the aforementioned siloxane bonds tends to result in stronger film, but the pore size becomes smaller, and the flexibility becomes brittle. Therefore, it is preferable, for example, to change the ratio of T2, T3, and T4 according to the application.

[0059] [Chemical Formula 1]

[0060]

[0061] When the void layer of this disclosure has the above-mentioned siloxane bonds, for example, when T2 is relatively represented as "1", the ratio of T2, T3 and T4 is T2:T3:T4 = 1:[1~100]:[0~50], 1:[1~80]:[1~40], 1:[5~60]:[1~30].

[0062] In the void layer of this disclosure, as described above, the gel-like silicon compound is a compound formed by the condensation or partial condensation of silane compounds. Examples of such condensation include dehydration condensation. Furthermore, the state of partial condensation refers to, for example, a state in which some of the condensing functional groups (e.g., alkoxy groups) contained in the silane compound have undergone condensation, while other functional groups have not condensed and remain as condensing functional groups. In other words, it can also be described as a state in which, for example, some of the silane compounds form siloxane bonds, while other silane compounds do not form bonds. The proportion of the unbonded silane compounds is, for example, less than 50%, less than 30%, or less than 15%.

[0063] As described above, the void layer of this disclosure comprises 1- to 3-functional silane compounds and 4-functional silane compounds as the aforementioned silane compounds. For example, the aforementioned silane compounds may be silane compounds comprising at least one of the 1- to 3-functional silane compounds, and further comprising a 4-functional silane compound. Examples of 1- to 3-functional silane compounds include, for example, 1- to 3-functional alkoxysilanes. Examples of 4-functional silane compounds include, for example, 4-functional alkoxysilanes. Examples of 1-functional silane compounds include, for example, trimethylmethoxysilane (TMMS), trimethylethoxysilane (TMES), trimethylpropoxysilane (TMPS), etc. Examples of 2-functional silane compounds include, for example, dimethyldimethoxysilane (DDMS), dimethyldiethoxysilane (DDES), dimethyldipropoxysilane (DDPS), etc. Examples of the aforementioned trifunctional silane compounds include methyltrimethoxysilane (MTMS), methyltriethoxysilane (MTES), methyltripropoxysilane (MTPS), 3-acryloyloxypropyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, 4-vinylbutyltrimethoxysilane, 4-vinylbutyltriethoxysilane, 8-vinyloctyltrimethoxysilane, 8-vinyloctyltriethoxysilane, 10-methacryloyloxydecyltrimethoxysilane, 10-acryloyloxydecyltrimethoxysilane, 10-methacryloyloxydecyltriethoxysilane, 10-acryloyloxydecyltriethoxysilane, etc. Examples of the aforementioned tetrafunctional silane compounds include tetramethoxysilane (TMOS), tetraethoxysilane (TEOS), tetrapropoxysilane (TPOS), etc.

[0064] In the porous layer of this disclosure, the content of the tetrafunctional silane compound is, for example, 1 to 25 mol% relative to the mass of the 1- to 3-functional silane compounds. The lower limit of this content is, for example, 2 mol% or more, 3 mol% or more, or 3.5 mol% or more, and the upper limit is, for example, 20 mol% or less, 15 mol% or less, or 10 mol% or less, with a range of, for example, 2 to 20 mol%, 3 to 15 mol%, 3.5 to 15 mol%, or 3.5 to 10 mol%. It should be noted that, from the viewpoint of ease of pulverization in the gel pulverization process, the above-mentioned content is preferably not too high. Furthermore, from the viewpoint of improving the strength of the low-refractive-index layer, the above-mentioned content is preferably not too low.

[0065] The void layer disclosed herein is a void layer formed by the chemical bonding of, for example, the aforementioned pulverized gel-like silicon compound under the coexistence of additives. The additives may include, for example, at least one of a crosslinking reaction promoter and its precursor. The crosslinking reaction promoter may be, for example, an acidic or basic substance. The crosslinking reaction promoter may also be referred to as a catalyst, for example, promoting the chemical bonding (crosslinking bonds) between the pulverized gel-like silicon compound particles. Furthermore, the precursor of the crosslinking reaction promoter may also be referred to as a substance that generates the crosslinking reaction promoter by light or heat (crosslinking promoter generator).

[0066] As a chemical reaction that chemically bonds the aforementioned gel-like silicon compounds together, the dehydration condensation reaction of the residual silanol groups contained in the silica sol molecules is preferred. By using the aforementioned crosslinking reaction promoter to promote the reaction between the hydroxyl groups of the silanol groups, continuous film formation that solidifies the porous structure in a short time can be achieved. Examples of such crosslinking reaction promoters include photoactive catalysts and thermally active catalysts. According to the aforementioned photoactive catalyst, for example, in the bonding process described later, the aforementioned gel-like silicon compounds can be chemically bonded together (e.g., crosslinked bonds) without heating. Thus, for example, in the aforementioned bonding process, shrinkage of the pulverized material to be bonded is less likely to occur, thereby maintaining a higher porosity. For example, a substance that generates a catalyst by light (photocatalyst generator) can be used in addition to or in place of the aforementioned photoactive catalyst, and a substance that generates a catalyst by heat (thermal catalyst generator) can be used in addition to or in place of the aforementioned thermally active catalyst. As the aforementioned photocatalyst generator, there are no particular limitations, and examples include: photoalkali-generating agents (substances that generate alkaline catalysts through light irradiation), photoacid-generating agents (substances that generate acidic catalysts through light irradiation), etc., with photoalkali-generating agents being preferred. Examples of such photoalkali-generating agents include: 9-anthrylmethyl N,N-diethylcarbamate (trade name WPBG-018), (E)-1-[3-(2-hydroxyphenyl)-2-propenoyl]piperidine (trade name WPBG-027), and 1-(anthraquinone-2-yl)ethylimidazolium carboxylate. imidazolecarboxylate (trade name WPBG-140), 4-methacryloyloxypiperidine-1-carboxylic acid 2-nitrophenyl methyl ester (trade name WPBG-165), 1,2-diisopropyl-3-[bis(dimethylamino)methylene]guanidine 2-(3-benzoylphenyl)propionic acid (trade name WPBG-266), 1,2-dicyclohexyl-4,4,5,5-tetramethylbiguanidine n-butyltriphenylborate (trade name WPBG-300), and 2-(9-oxo) 1,5,7-triazabicyclo[4.4.0]dec-5-ene (Tokyo Chemical Industry Co., Ltd.), compounds containing 4-piperidinemethanol (trade name HDPD-PB100: manufactured by Heraeus Co., Ltd.), etc. It should be noted that the above-mentioned trade names containing "WPBG" are all trade names of Wako Pure Chemical Industries Co., Ltd. Examples of photoacid-generating agents include: aromatic sulfonium salts (trade name SP-170: ADEKA Co., Ltd.), triarylsulfonium salts (trade name CPI101A: San-Apro Ltd.), aromatic iodine... Salt (trade name Irgacure 250: Ciba Japan Co., Ltd.), etc. Furthermore, the crosslinking reaction promoter that chemically bonds the pulverized gel-like silicon compound to each other is not limited to the aforementioned photoactive catalyst and photocatalyst generator; for example, it can be a thermally active catalyst or a thermal catalyst generator such as urea. Examples of crosslinking reaction promoters that chemically bond the pulverized gel-like silicon compound to each other include alkaline catalysts such as potassium hydroxide, sodium hydroxide, and ammonium hydroxide, and acid catalysts such as hydrochloric acid, acetic acid, and oxalic acid. Among these, an alkaline catalyst is preferred. For the aforementioned crosslinking reaction promoter and its precursor, for example, at least one of the aforementioned crosslinking reaction promoter and its precursor can be added to a sol-particle liquid (e.g., a suspension) containing the aforementioned pulverized material (gel-like silicon compound) just before application, or a mixture of at least one of the aforementioned crosslinking reaction promoter and its precursor mixed in a solvent can be prepared for use. The aforementioned mixture may be, for example, a coating solution obtained by directly adding to and dissolving the aforementioned sol-particle liquid, a solution obtained by dissolving at least one of the aforementioned crosslinking reaction promoters and their precursors in a solvent, or a dispersion obtained by dispersing at least one of the aforementioned crosslinking reaction promoters and their precursors in a solvent. The solvent is not particularly limited, and examples include water and buffer solutions. The amount of the aforementioned crosslinking reaction promoters and their precursors added is not particularly limited, and may be, for example, 0.01 to 20% by weight, 0.05 to 10% by weight, or 0.1 to 5% by weight relative to the weight of the aforementioned gel-like silicon compound.

[0067] Relative to the total amount of the above-mentioned 1-3 functional silane compounds and the above-mentioned 4 functional silane compounds, the lower limit of the total content ratio of the above-mentioned crosslinking reaction promoter and its precursor is, for example, 1 mol% or more, 1.5 mol% or more, 2 mol% or more, or 2.5 mol% or more, and the upper limit is, for example, 5 mol% or less, 4 mol% or less, 3.5 mol% or less, or 3 mol% or less.

[0068] It should be noted that, in the void layer of this disclosure, when the silane compound is not included, the lower limit of the total content of the crosslinking reaction promoter and its precursor relative to the total amount of the silane compound is, for example, 1.5 mol% or more, 2 mol% or more, or 2.5 mol% or more, and the upper limit is, for example, 5 mol% or less, 4 mol% or less, 3.5 mol% or less, or 3 mol% or less.

[0069] Additionally, the aforementioned additive may include, for example, a crosslinking aid. This crosslinking aid can also be described as a medium, for example, used to indirectly bond the pulverized gel-like silicon compound with each other through chemical bonding. By allowing the crosslinking aid to enter between the pulverized particles and to interact or bond with them, even particles that are slightly separated can bond together, thereby efficiently improving strength.

[0070] As the aforementioned crosslinking aid, a multi-crosslinked silane monomer is preferred. Specifically, the aforementioned multi-crosslinked silane monomer may have, for example, two or more but three or fewer alkoxysilyl groups, the chain length between the alkoxysilyl groups may be one or more but less than 10 carbon atoms, and may also contain elements other than carbon. Examples of crosslinking aids include: bis(trimethoxysilyl)ethane, bis(triethoxysilyl)ethane, bis(trimethoxysilyl)methane, bis(triethoxysilyl)methane, bis(triethoxysilyl)propane, bis(trimethoxysilyl)propane, bis(triethoxysilyl)butane, bis(trimethoxysilyl)butane, bis(triethoxysilyl)pentane, bis(trimethoxysilyl)pentane, bis(triethoxysilyl)hexane, bis(trimethoxysilyl)hexane, bis(trimethoxysilyl)-N-butyl-N-propylethane-1,2-diamine, tris(3-trimethoxysilylpropyl)isocyanurate, tris(3-triethoxysilylpropyl)isocyanurate, etc. The amount of the crosslinking aid is not particularly limited, but is, for example, 0.01 to 20% by weight, 0.05 to 15% by weight, or 0.1 to 10% by weight relative to the weight of the gel-like silicon compound.

[0071] Relative to the total amount of the above-mentioned 1-3 functional silane compounds and the above-mentioned 4 functional silane compounds, the lower limit of the total content ratio of the above-mentioned crosslinking aid is, for example, 1 mol% or more, 2 mol% or more, 2.5 mol% or more, or 3 mol% or more, and the upper limit is, for example, 6 mol% or less, 5.5 mol% or less, 5 mol% or less, 4.5 mol% or less, or 3.5 mol% or less.

[0072] It should be noted that, in the void layer of this disclosure, when the silane compound is not included in the above-mentioned tetrafunctional silane compound, the lower limit of the total content of the crosslinking aid relative to the total amount of the silane compound is, for example, 2 mol% or more or 2.5 mol% or more, and the upper limit is, for example, 6 mol% or less, 5 mol% or less, 4 mol% or less, 3.5 mol% or less or 3 mol% or less.

[0073] The porosity layer disclosed herein, for example, has a porous structure. The porosity size of the pores in the aforementioned porosity layer refers to the diameter of the major axis, which is the diameter of the minor axis of the pore (hole). The porosity size is, for example, 5 nm to 200 nm. The aforementioned porosity size is, for example, 5 nm or more, 10 nm or more, or 20 nm or more, with upper limits such as 200 nm or less, 150 nm or less, 100 nm or less, 50 nm or less, 40 nm or less, or 30 nm or less, and a range such as 5 nm to 200 nm or 10 nm to 100 nm. Regarding the aforementioned porosity size, since the preferred porosity size needs to be determined according to the intended use of the porosity structure, it is, for example, necessary to adjust to the desired porosity size according to the purpose. The aforementioned porosity size can be evaluated, for example, by the following methods.

[0074] (SEM observation of the cross-section of the void layer)

[0075] In this disclosure, the morphology of the void layer can be observed and analyzed using SEM (scanning electron microscope). Specifically, for example, the void layer can be processed by FIB under cooling (accelerating voltage: 30 kV), and the resulting cross-sectional sample can be imaged at 100,000x magnification using an FIB-SEM (manufactured by FEI: trade name Helios NanoLab600, accelerating voltage: 1 kV).

[0076] (Evaluation of gap size)

[0077] In this disclosure, the aforementioned pore size can be quantified using the BET test method. Specifically, 0.1 g of the sample (the aforementioned pore layer) is placed into the capillary of a pore distribution / specific surface area measuring device (BELLSORP MINI / MicrotracBEL, a trade name) and subjected to reduced pressure drying at room temperature for 24 hours to degas the gas within the pore structure. Then, by adsorbing nitrogen onto the sample, BET curves, BJH curves, and adsorption isotherms are plotted to determine the pore distribution. Thus, the pore size can be evaluated.

[0078] The void layer disclosed herein can, for example, have a porous structure (multi-pore structure) as described above, or for example, it can be an open-pore structure with a continuous pore structure. An open-pore structure refers to a structure in which the pore structures are three-dimensionally connected, or in other words, a state where the internal voids of the pore structure are continuous. When a porous body has an open-pore structure, the porosity within the bulk can be increased; however, when using closed-pore particles such as hollow silica, an open-pore structure cannot be formed. In contrast, in the void layer, since the sol particles (the pulverized material forming the porous gel of the sol) have a three-dimensional dendritic structure, these dendritic particles settle / accumulate in the coating film (a coating film containing the sol of the pulverized porous gel), thereby easily forming an open-pore structure. Furthermore, in the void layer, it is more preferable to form an integral structure with a plurality of fine pores distributed within the open-pore structure. The aforementioned overall structure refers to a hierarchical structure, for example, existing in the form of a structure with micropores at the nanoscale and an open structure composed of a collection of the same nanopores. When forming the aforementioned overall structure, for example, the micropores can impart membrane strength, and the large open pores can impart high porosity, thereby simultaneously achieving membrane strength and high porosity. To form the aforementioned overall structure, for example, it is first important to control the pore distribution of the generated void structure in the porous gel during the pre-pulverization stage. Furthermore, for example, when pulverizing the porous gel, the overall structure can be formed by controlling the particle size distribution of the pulverized material to a desired size.

[0079] In the void layer of this disclosure, there is no particular limitation on the haze characterizing transparency, the lower limit of which is, for example, more than 0.1%, more than 0.2% or more than 0.3%, and the upper limit of which is, for example, less than 10%, less than 5%, or less than 3%, and the range is, for example, 0.1 to 10%, 0.2 to 5%, or 0.3 to 3%.

[0080] The aforementioned haze can be measured using, for example, the method described below.

[0081] (Evaluation of haze)

[0082] The void layer (the void layer of this disclosure) was cut into 50mm × 50mm pieces and placed in a haze meter (manufactured by Murakami Color Technology Research Institute Co., Ltd.: HM-150) to measure the haze. The haze value was calculated using the following formula.

[0083] Haze (%) = [Diffusion transmittance (%) / Total light transmittance (%)] × 100 (%)

[0084] Regarding refractive index, it is generally defined as the ratio of the speed of light propagation at the wavefront in a vacuum to the speed of light propagation within a medium. It should be noted that, unless otherwise specified, the refractive index described above refers to the refractive index measured at a wavelength of 550 nm in this disclosure. Furthermore, the method for measuring the refractive index is not particularly limited; for example, it can be measured using the methods described below.

[0085] As described above, the refractive index of the void layer in this disclosure is 1.30 or less. The upper limit of the refractive index of the void layer is, for example, 1.30 or less, less than 1.30, 1.26 or less, 1.25 or less, less than 1.25, 1.24 or less, 1.23 or less, or 1.22 or less; the lower limit is, for example, 1.05 or more, 1.10 or more, 1.15 or more, 1.16 or more, 1.17 or more, 1.18 or more, or 1.19 or more; and the range is, for example, 1.05 or more and 1.30 or less, 1.05 or more and less than 1.30, 1.10 or more and 1.25 or less, 1.15 or more and less than 1.25, or 1.19 or more and less than 1.25. The method for determining the refractive index of the void layer is not particularly limited; for example, it can be determined by the following method.

[0086] The lower limit of the porosity of the aforementioned void layer is, for example, 30% or more or 50% or more, and the upper limit is, for example, 90% or less, 75% or less or 60% or less, and the range is, for example, 30 to 90% or 50 to 75% or 50 to 60% of volume.

[0087] (Evaluation of the refractive index of the void layer)

[0088] After forming a void layer (the void layer of this disclosure) on an acrylic film, it is cut into 50mm × 50mm pieces and adhered to the surface of a glass plate (thickness: 3mm) using an adhesive layer. The central portion of the back side of the glass plate (approximately 20mm in diameter) is coated with black ink to prepare a sample that does not reflect light from the back side of the glass plate. The sample is then placed on an ellipsometer (manufactured by JAWoollam Japan: VASE) to measure the refractive index at a wavelength of 550nm and an incident angle of 50–80 degrees. The average value is taken as the refractive index.

[0089] For the porosity of the aforementioned porosity layer after a heat-humidification durability test at 85°C and 85%RH for 500 hours, the lower limit is, for example, 10% or more by volume, 20% or more by volume, 30% or more by volume, 40% or more by volume, 50% or more by volume, 60% or more by volume, 70% or more by volume, 80% or more by volume, 85% or more by volume, or more than 85% by volume. The method for determining the refractive index of the aforementioned porosity layer is not particularly limited; for example, it can be determined by the following methods.

[0090] (Evaluation of the porosity retention rate of the porous layer)

[0091] The fabricated laminate was placed in an oven at 85°C and 85%RH for 500 hours for a heat and humidification durability test. SEM can be used to confirm the degree of pore filling in the void areas of the void layer after the heat and humidification durability test, and the porosity retention rate can be calculated.

[0092] The thickness of the void layer disclosed herein is not particularly limited, but its lower limit is, for example, 0.05 μm or more or 0.1 μm or more, and its upper limit is, for example, 1000 μm or less, 100 μm or less, 10 μm or less, 5 μm or less or 2 μm or less, and its range is, for example, 0.05 to 1000 μm or 0.1 to 100 μm.

[0093] The morphology of the void layer disclosed herein is not particularly limited; for example, it can be a membrane shape or a block shape.

[0094] The method for manufacturing the void layer disclosed herein is not particularly limited. For example, it can be manufactured by the method for manufacturing void layers described later or by the methods described in International Publication No. 2019 / 065999 and International Publication No. 2019 / 065803. The description in that publication is incorporated herein by reference.

[0095] In this disclosure, the adhesive layer described above is not particularly limited. The adhesive or bonding agent forming the adhesive layer is not particularly limited; for example, common adhesives or bonding agents can be used. Examples of such adhesives or bonding agents include polymer adhesives made from acrylics, vinyl alcohols, silicones, polyesters, polyurethanes, polyethers, and rubber-based adhesives. Additionally, adhesives composed of water-soluble crosslinking agents of vinyl alcohol polymers such as glutaraldehyde, melamine, and oxalic acid can also be used. Only one of these adhesives or bonding agents may be used, or multiple adhesives may be used in combination (e.g., mixing, lamination, etc.). The thickness of the adhesive layer is not particularly limited, and may be, for example, 0.1–100 μm, 5–50 μm, 10–30 μm, or 12–25 μm.

[0096] In the adhesive layer of the laminate disclosed herein, the nanoindentation hardness is, for example, 0.5 MPa or more. The lower limit of the nanoindentation hardness can be, for example, 0.55 MPa or more, 0.6 MPa or more, or 0.65 MPa or more, and the upper limit can be, for example, 2.0 MPa or less, 1.5 MPa or less, 1.3 MPa or less, or 1.1 MPa or less. The method for measuring the nanoindentation hardness is not particularly limited; for example, it can be measured by the following method.

[0097] (Evaluation of nanoindentation hardness)

[0098] The sample to be measured was cut into approximately 1 cm square pieces and fixed to a given support. The nanoindentation hardness of the adhesive layer in the laminate of this disclosure was measured under the following conditions. The nanoindentation hardness can be measured using the nanoindentation method.

[0099] • Analytical apparatus: Manufactured by Hysitron Inc., Triboindenter

[0100] • Indenter used: Conical (spherical: 20μm diameter)

[0101] • Measurement method: Single indentation measurement

[0102] • Measurement temperature: room temperature

[0103] • Indentation depth: 2000nm

[0104] The nanoindentation hardness is calculated using the following formula based on the maximum load (Pmax) and the contact projected area (A) obtained from the measurement.

[0105] Nanoindentation hardness = Pmax / A

[0106] It should be noted that the above-mentioned nanoindentation hardness can be the nanoindentation hardness of any surface of the adhesive layer or any surface in the cross-section of the adhesive layer.

[0107] In the laminate of this disclosure, the peel strength between the void layer and the adhesive layer, measured using a tensile testing machine at a tensile speed of 0.3 m / min, is, for example, 3 N / 25 mm or more. The lower limit of the peel strength can be, for example, 3.5 N / 25 mm or more, 4.0 N / 25 mm or more, or 5.0 N / 25 mm or more. The higher the peel strength, the higher the interlayer mechanical strength of the laminate of this disclosure; therefore, the upper limit of the peel strength is not particularly limited, and can be, for example, 20 N / 25 mm or less, 15 N / 25 mm or less, or 10 N / 25 mm or less. The peel strength is, for example, the peel strength measured due to the cohesive failure of the void layer. The method for measuring the peel strength is not particularly limited; for example, it can be measured by the following methods.

[0108] (Evaluation of interlayer peel strength)

[0109] A material having a void layer (the void layer of this disclosure) and an adhesive layer (the adhesive layer in the laminate of this disclosure) formed on a resin film substrate is prepared. An acrylic adhesive layer (20 μm thick) is bonded to the resin film substrate on the side opposite to the void layer. The bonded sample is cut into 50 mm × 25 mm pieces to make adhesive tape sheets. Next, the adhesive layer (10 μm thick) on the void layer side is bonded to a strip of PET film (T100: manufactured by Mitsubishi Resin Film Co., Ltd.) cut into 25 mm × 100 mm shapes, and the acrylic adhesive layer on the resin film substrate side is laminated with glass to fix it. The sample prepared in this way is clamped in a tensile testing machine (manufactured by Shimadzu Corporation, trade name: Autograph AG-Xplus) with a chuck distance of 100 mm, and a 180° peel test is performed at a tensile speed of 0.3 m / min. Perform N=3 50mm peel tests and set the average test force as the peel strength between the aforementioned layers.

[0110] The refractive index of the void layer of this disclosure, measured in the form of a laminate, is, for example, 1.30 or less. The upper limit of the refractive index of the void layer, measured in the form of a laminate, is, for example, 1.30 or less, less than 1.30, 1.26 or less, 1.25 or less, less than 1.25, 1.24 or less, 1.23 or less, or 1.22 or less; the lower limit is, for example, 1.05 or more, 1.10 or more, 1.15 or more, 1.16 or more, 1.17 or more, 1.18 or more, or 1.19 or more; and the range is, for example, 1.05 or more and 1.30 or less, 1.05 or more and less than 1.30, 1.10 or more and 1.25 or less, 1.15 or more and less than 1.25, or 1.19 or more and less than 1.25. The method for measuring the refractive index of the void layer of this disclosure, measured in the form of a laminate, is not particularly limited; for example, it can be measured by the following method.

[0111] (Evaluation of the refractive index of the void layer as determined in the state of a laminate)

[0112] The prism of the prism coupler (manufactured by Metricon) is tightly fitted to the substrate side of a laminate (glass / adhesive layer / void layer / acrylic substrate) with an adhesive layer on the void layer, and the critical angle for total internal reflection is measured using a laser. The refractive index can be calculated from the measured critical angle value.

[0113] The laminate disclosed herein may be, for example, a laminate that satisfies the following condition (1) when the refractive index is set to X and the peel strength is set to Y. Figure 4 A graph showing the relationship between peel strength and refractive index under condition (1) is shown. It should be noted that... Figure 4 In the figure, the horizontal axis represents the refractive index, and the vertical axis represents the peel strength (N / 25mm).

[0114] Condition (1): Y ≥ 80X - 93.8

[0115] In addition, the laminate of this disclosure may be, for example, a laminate that satisfies the following condition (2) when the refractive index is set to X and the peel strength is set to Y. Figure 4 A graph showing the relationship between peel strength and refractive index under condition (1) is shown.

[0116] Condition (2): Y ≥ 100X - 117

[0117] When conditions (1) or (2) above are met, for example, a laminate with low refractive index and high peel strength (i.e., excellent mechanical strength) can be obtained. There are no particular limitations in order to meet conditions (1) and (2) above; for example, the types and proportions of the above-mentioned four-functional silane compounds and additives can be appropriately adjusted.

[0118] In this disclosure, the intermediate layer is not particularly limited, and may be, for example, a layer formed by integrating a portion of the void layer with a portion of the adhesive layer as described above. The thickness of the intermediate layer is not particularly limited, and may be, for example, 1~1500nm, 5~1000nm, 10~800nm, or 20~500nm.

[0119] The morphology of the laminates disclosed herein is not particularly limited, but is generally membrane-shaped.

[0120] The laminate of this disclosure is, for example, a roll. Alternatively, the laminate of this disclosure may further include a resin film as described above, and the aforementioned void layer may be formed on the elongated resin film. In this case, another elongated film may be laminated onto the laminate of this disclosure, or another elongated resin film (e.g., interlayer paper, release film, surface protective film, etc.) may be laminated onto the laminate of this disclosure containing the aforementioned resin film and the aforementioned void layer before being rolled into a roll.

[0121] The method for manufacturing the laminate disclosed herein is not particularly limited. For example, it can be manufactured using the manufacturing method of the present disclosure as shown below. Furthermore, regarding the method for manufacturing the optical laminate of the present disclosure that does not contain a resin film, unless otherwise specified, it can be performed in the same manner as the method for manufacturing the laminate of the present disclosure, except that a resin film is not used.

[0122] [2. Manufacturing methods for void layers and laminates]

[0123] The method for manufacturing the void layer and the laminate of this disclosure is not particularly limited; for example, it can be carried out by the manufacturing method described below. However, the following description is merely illustrative and does not constitute any limitation on this disclosure.

[0124] The method for manufacturing a laminate containing a void layer disclosed herein includes, for example, a void layer forming step for forming the void layer, and an adhesive layer forming step for forming the adhesive layer on the void layer. The method for manufacturing the laminate may further include an intermediate layer forming step for reacting the void layer with the adhesive layer to form the intermediate layer.

[0125] As described above, the void layer formation process (the void layer manufacturing method of this disclosure) includes a gel-like silica synthesis process, a gel pulverization process, and a bonding process. The void layer formation process (the void layer manufacturing method of this disclosure) may or may not include other processes besides the aforementioned gel-like silica synthesis process, gel pulverization process, and bonding process. These other processes are not particularly limited and may include, for example, the coating process and drying process described later.

[0126] The aforementioned gelled silica synthesis process includes a step of synthesizing a gelled silica compound by condensing or partially condensing the aforementioned silane compound. The aforementioned gelled silica synthesis process may include, for example, a step of gelling a blocky porous body in a solvent to form a gel. In this case, for example, in the initial pulverization stage of the plurality of stages described later (e.g., the first pulverization stage described later), the gel that has been gelled by the aforementioned gelled silica synthesis process is used.

[0127] The method for manufacturing the aforementioned void layer includes, for example, a maturation step in which the gel, after gelation, is matured in a solvent. In this case, for example, the gel after the maturation step is used in the initial crushing stage (e.g., the first crushing stage) of the aforementioned multiple crushing stages.

[0128] The aforementioned gel pulverization process includes the step of pulverizing the aforementioned gel-like silicon compound to obtain pulverized material. The aforementioned gel pulverization process can be a single stage, but is preferably divided into multiple pulverization stages. The number of pulverization stages is not particularly limited; for example, it can be two stages or more than three stages.

[0129] The volume average particle size of the gel after the first pulverization stage can be, for example, 0.5~100 μm, 1~100 μm, 1~50 μm, 2~20 μm, or 3~10 μm. The volume average particle size of the gel after the second pulverization stage can be, for example, 10~1000 nm, 100~500 nm, or 200~300 nm. The volume average particle size represents the particle size deviation of the pulverized material in the liquid containing the gel (gel-containing liquid). The volume average particle size can be measured by particle size distribution evaluation devices such as dynamic light scattering and laser diffraction, and electron microscopes such as scanning electron microscope (SEM) and transmission electron microscope (TEM).

[0130] In the method for manufacturing the void layer disclosed herein, for example, a solvent replacement step is performed after the aforementioned gel-like silica synthesis step, in which the aforementioned solvent is replaced with another solvent. In this case, for example, in the initial pulverization stage of the aforementioned plurality of pulverization stages (e.g., the aforementioned first pulverization stage), the aforementioned gel in the other solvent is used.

[0131] In at least one of the pulverization stages of the plurality of stages in the manufacturing method of the porous layer disclosed herein (e.g., at least one of the first pulverization stage and the second pulverization stage), the pulverization of the porous body is controlled, for example, while measuring the shear viscosity of the liquid.

[0132] At least one of the crushing stages (e.g., at least one of the first crushing stage and the second crushing stage) in the above-mentioned multiple stages of the method for manufacturing the void layer of this disclosure is carried out by, for example, high-pressure medialess crushing.

[0133] It should be noted that, in the following, in the method for manufacturing the void layer disclosed herein, the gel-containing pulverized liquid obtained by the process including the above-described gel pulverization process is sometimes simply referred to as "gel-containing pulverized liquid".

[0134] According to the above-described gel-containing pulverized liquid, for example, the porous layer, which serves as a functional porous body, can be formed by forming a coating film thereon and chemically bonding the pulverized particles in the coating film through a bonding process. According to the above-described gel-containing pulverized liquid, for example, the porous layer can be applied to various objects. Therefore, the above-described gel-containing pulverized liquid and its manufacturing method are useful, for example, in the manufacture of the aforementioned porous layer.

[0135] The aforementioned liquid containing gel fragments has, for example, excellent uniformity, so that when the aforementioned void layer is used for applications such as optical components, it can have a good appearance.

[0136] The aforementioned gel-containing pulverized liquid may be, for example, a gel-containing pulverized liquid used to obtain a layer (porosity layer) with high porosity by applying (coating) the aforementioned gel-containing pulverized liquid onto a substrate (coating process) and further drying it (drying process).

[0137] In the above coating process, the coating method for the liquid containing gel fragments is not particularly limited, and conventional coating methods can be used. Examples of such coating methods include: slot die coating, reverse gravure coating, micro-gravure coating, dip coating, spin coating, brush coating, roller coating, flexographic printing, wire rod coating, spray coating, extrusion coating, curtain coating, and reverse coating. From the viewpoints of productivity and coating smoothness, extrusion coating, curtain coating, roller coating, and micro-gravure coating are preferred. The amount of the liquid containing gel fragments applied is not particularly limited; for example, it can be appropriately set in a way that achieves an appropriate thickness for the void layer. The thickness of the void layer is not particularly limited, for example, as described above.

[0138] In the aforementioned drying process, the liquid containing gel-powdered material is dried (i.e., the dispersion medium contained in the liquid containing gel-powdered material is removed) to form the dried coating film (precursor layer of the void layer). The drying temperature in the aforementioned drying process is, for example, 50~250°C, 60~150°C, or 70~130°C, and the drying time is, for example, 0.1~30 minutes, 0.2~10 minutes, or 0.3~3 minutes. Regarding the drying temperature and time, for example, those that exhibit continuous productivity and high cavitation rate are preferred, with lower temperatures and shorter times being preferable. If the conditions are too harsh, for example, when the substrate is a resin film, temperatures close to the glass transition temperature of the substrate may cause the substrate to stretch in the drying oven, potentially leading to defects such as cracks in the void structure formed immediately after coating. On the other hand, if the conditions are too lenient, for example, since residual solvent is present when the roll-to-roll is removed from the drying oven, there is a possibility of scratches or other appearance defects when rubbed against the rollers in subsequent processes.

[0139] The drying method described above can be, for example, natural drying, heated drying, or vacuum drying. There are no particular limitations on the drying method; for example, a conventional heating mechanism can be used. Examples of such heating mechanisms include hot air blowers, heated rollers, and far-infrared heaters. Among these, heated drying is preferred when continuous industrial production is required.

[0140] The aforementioned bonding process includes a step of chemically bonding the aforementioned pulverized materials. This bonding process can be performed, for example, by irradiating or heating the coating film containing a catalyst or catalyst generator previously added to the liquid containing the gel-containing pulverized materials; or by spraying the coating film with the catalyst followed by irradiation or heating; or by spraying the catalyst or catalyst generator while simultaneously irradiating or heating. The catalyst can be, for example, the aforementioned crosslinking reaction promoter, or a strength enhancer that increases the strength of the aforementioned porous layer; the crosslinking promoter can also function as the aforementioned strength enhancer.

[0141] The cumulative light intensity of the illumination mentioned above is not specifically limited, but can be converted to 360nm, for example, 200~800mJ / cm². 2 250~600mJ / cm 2 or 300~400mJ / cm 2 From the perspective of preventing insufficient irradiation and the failure of catalyst decomposition due to light absorption, which would lead to inadequate effectiveness, 200 mJ / cm 2 The above-mentioned cumulative light intensity is preferable. Furthermore, from the viewpoint of preventing damage to the substrate beneath the void layer and the formation of thermal wrinkles, 800 mJ / cm² is recommended. 2 The following cumulative light levels are recommended.

[0142] The heating temperature and heating time in the above heating process are not particularly limited, and the conditions for the above heating treatment are not particularly limited. For example, the heating temperature is 50~250℃, 60~150℃, or 70~130℃, and the heating time is 0.1~30 minutes, 0.2~10 minutes, or 0.3~3 minutes. Alternatively, the process of drying the coated liquid containing gel fragments as described above can also be a process of performing a chemical reaction in the presence of the catalyst. That is, in the process of drying the coated liquid containing gel fragments (e.g., a suspension), the fragments can be chemically bonded together through a chemical reaction in the presence of the catalyst. In this case, the fragments (microporous particles) can be more firmly bonded together by further heating the coating film after the drying process. Furthermore, it is conceivable that the chemical reaction in the presence of the catalyst may sometimes occur in the process of preparing the liquid containing microporous particles (e.g., a suspension) and the process of coating the liquid containing microporous particles. However, this conjecture does not limit this disclosure in any way.

[0143] The aforementioned adhesive layer forming process may include, for example, an adhesive coating process of applying the adhesive coating liquid to a substrate; and a heating and drying process of heating and drying the substrate coated with the adhesive coating liquid. For example, the adhesive layer can be formed on the void layer by attaching the adhesive layer side of an adhesive tape or similar material, on which the adhesive layer is laminated, to the void layer. In this case, the adhesive tape or similar material can remain in an adhered state or can be peeled off from the adhesive layer. In particular, by peeling off the material, a substrate-free (substrate-free) laminate can be formed, thereby significantly reducing the thickness and suppressing the increase in thickness of the device, etc. In this disclosure, the adhesive layer may be manufactured, for example, using the adhesive coating liquid as described above.

[0144] The above-described adhesive layer forming process can be performed, for example, as described below. First, the adhesive coating liquid is manufactured by a mixing process in which all components of the adhesive coating liquid are mixed. The adhesive coating liquid may, for example, contain a (meth)acrylic polymer, and may further contain or not contain a crosslinking agent (e.g., isocyanate crosslinking agent, epoxy crosslinking agent). The adhesive coating liquid may, for example, contain: the above-described (meth)acrylic polymer, a monomer having one or two reactive double bonds in one molecule, a crosslinking agent, and an organic peroxide. In this case, if the adhesive coating liquid contains other components, these other components may also be mixed together. For example, the polymerization solvent used in manufacturing the (meth)acrylic polymer may not be removed, and the adhesive coating liquid may be directly mixed as a component. Furthermore, the method for manufacturing the adhesive coating liquid may include steps other than the above-described mixing process, or it may not include other steps, and all components of the adhesive coating liquid may be mixed solely through the above-described mixing process.

[0145] Next, the adhesive coating liquid is applied to the substrate (adhesive coating liquid application step). The substrate is not particularly limited; for example, it can be a film or similar substrate. Preferred substrates include, but are not limited to, thermoplastic resin substrates, glass substrates, inorganic substrates such as silicon, plastics molded from thermosetting resins, semiconductor components, and carbon fiber materials such as carbon nanotubes. Examples of substrate forms include films and sheets. Examples of thermoplastic resins include, for example, polyethylene terephthalate (PET), acrylic acid, cellulose acetate propionate (CAP), cyclic olefin polymers (COP), cellulose triacetate (TAC), polyethylene naphthalate (PEN), polyethylene (PE), and polypropylene (PP). Furthermore, the coating thickness of the adhesive coating liquid in the adhesive coating liquid application step is not particularly limited; it can be adjusted appropriately to achieve a given thickness of the dried adhesive layer. There is no particular limitation on the thickness of the adhesive layer after drying, for example, as described later.

[0146] Next, the substrate coated with the aforementioned adhesive liquid is subjected to heat drying (heat drying step). In this heat drying step, the heating temperature is not particularly limited, and can be, for example, 50°C or higher, 80°C or higher, 100°C or higher, or 155°C or higher, or, for example, 200°C or lower, 180°C or lower, or 160°C or lower. The heating drying time is not particularly limited, and can be, for example, 0.5 minutes or more, 1 minute or more, or 3 minutes or more, or, for example, 60 minutes or less, 30 minutes or less, 20 minutes or less, or 10 minutes or less. In this heat drying step, for example, a crosslinking reaction and graft polymerization occur between the aforementioned (meth)acrylic polymer and the crosslinking agent. As a result, for example, as described above, the amount of semi-polymer present in the adhesive liquid is reduced, and the adhesive layer is less likely to penetrate into the recesses of the first optical film. Thus, the adhesive layer used in the laminate of this disclosure can be manufactured.

[0147] Next, as described above, the adhesive layer is bonded to the void layer (bonding process). This method is not particularly limited; for example, as described above, the adhesive layer can be formed on the void layer by bonding the adhesive layer side of an adhesive tape or similar material, on which the adhesive layer of the present disclosure is laminated on a substrate, to the void layer. In this way, the laminate of the present disclosure can be manufactured.

[0148] The thickness of the adhesive layer is not particularly limited, for example, it is 0.1~100μm, 5~50μm, 10~30μm or 12~25μm.

[0149] In the method for manufacturing the laminate disclosed herein, for example, a heating step may be performed after the bonding step to heat the adhesive layer and the void layer. Hereinafter, this heating step is sometimes referred to as an "aging step." In the heating step (aging step), the heating temperature is not particularly limited, and may be, for example, 40°C or higher, 45°C or higher, or 50°C or higher, or, for example, 80°C or lower, 70°C or lower, 60°C or lower, or 55°C or lower. The heating time is not particularly limited, and may be, for example, 1 minute or more, 10 minutes or more, 60 minutes or more, or 1800 minutes or more, or, for example, 3000 minutes or lower, 2800 minutes or lower, 2500 minutes or lower, or 2000 minutes or lower. In this aging step, for example, the void layer and the adhesive layer may fuse together to form an intermediate layer. This intermediate layer, for example, acts as a barrier, suppressing the reduction in porosity caused by the adhesive filling the voids in the void layer. It should be noted that the above-mentioned void layer and the above-mentioned adhesive layer can be integrated into one, which can be the case where the adhesive layer is embedded in the void layer and chemically bonded together, or the case where the adhesive layer is embedded in the void layer.

[0150] The aforementioned adhesive layer protects the void layer from physical damage (especially abrasions). Furthermore, the adhesive layer is preferably a layer with excellent pressure resistance, so that the void layer will not be damaged even when fabricating an adhesive sheet containing a void layer without a substrate (substrate-free), but this is not particularly limited.

[0151] The resulting laminate can be further laminated with other films (layers) as described above to form a laminated structure containing the aforementioned porous layer (porous structure). In this case, the constituent elements can be laminated with, for example, the aforementioned adhesive layer (adhesive or bonding agent) sandwiched between them.

[0152] From an effective perspective, for example, the lamination of the above-mentioned components can be carried out by using continuous processing of long strip films (so-called roll-to-roll, etc.), and when the substrate is a molded object / component, it can also be carried out by laminating substrates that have undergone batch processing.

[0153] [3. Optical components]

[0154] As described above, the optical component of this disclosure includes the void layer or the laminate of this disclosure. The optical component of this disclosure is characterized by including the void layer or the laminate of this disclosure, with no other limitations on its composition. For example, in addition to including the aforementioned void layer or the aforementioned laminate, the optical component of this disclosure may further include other layers. The optical component of this disclosure may, for example, be in a rolled form.

[0155] [4. Optical devices]

[0156] As described above, the optical device disclosed herein includes the optical components of this disclosure. The optical device of this disclosure is not particularly limited; for example, it can be an image display device or an illumination device. Examples of such image display devices include liquid crystal displays, organic EL (Electroluminescence) displays, and micro LED (Light Emitting Diode) displays. Examples of such illumination devices include, for example, organic EL lighting.

[0157] Example

[0158] The embodiments of this disclosure will now be described. However, this disclosure is not limited to the following embodiments.

[0159] It should be noted that, in the following reference examples, embodiments, and comparative examples, unless otherwise specified, the parts (relative amounts) of each substance are parts by mass (parts by weight). In the following reference examples, embodiments, and comparative examples, the adhesive (adhesive composition) described later was used as the adhesive. In the following reference examples, embodiments, and comparative examples, "adhesive layer" is equivalent to "adhesive bonding layer." That is, in the following reference examples, embodiments, and comparative examples, unless otherwise specified, "adhesive layer" and "adhesive bonding layer" have the same meaning.

[0160] In addition, in the following reference examples, embodiments and comparative examples, the nanoindentation hardness, the refractive index of the void layer (refractive index (layer)) measured in the state of a laminate, and the refractive index (refractive index (void layer)) measured only in the case of the void layer, peel strength and void retention rate were measured by the methods described in the embodiments.

[0161] It should be noted that in the adhesive layers of the following reference examples, embodiments and comparative examples, it is presumed that the polymer (acrylic polymer) is cross-linked by a cross-linking agent and forms a cross-linked structure through the heating and drying of the applied adhesive, but the cross-linked structure has not been confirmed.

[0162] [Reference Example 1: Formation of the adhesive layer (adhesive 1)]

[0163] The adhesive layer of this reference example (reference example 1) was formed according to the steps (1) to (3) below.

[0164] (1) Preparation of acrylic polymer solutions

[0165] In a four-necked flask equipped with a stirring blade, thermometer, nitrogen inlet tube, and condenser, 90.7 parts of butyl acrylate, 6 parts of N-acryloylmorpholine, 3 parts of acrylic acid, 0.3 parts of 2-hydroxybutyl acrylate, and 0.1 parts by weight of 2,2'-azobisisobutyronitrile (2,2'-azobisisobutyronitrile) as a polymerization initiator, along with 100 g of ethyl acetate, were added. Nitrogen gas was then introduced while the contents of the four-necked flask were slowly stirred to purge the solution. The liquid temperature in the four-necked flask was then maintained at approximately 55°C for 8 hours to prepare an acrylic polymer solution.

[0166] (2) Preparation of acrylic adhesive compositions

[0167] An acrylic adhesive composition (acrylic adhesive solution) was prepared by combining 100 parts of the solid component of the acrylic polymer solution obtained in (1) above with 0.2 parts of isocyanate crosslinking agent (commercial name "CORONATE L" manufactured by Nippon Polyurethanes Co., Ltd., an adduct of trimethylolpropane toluene diisocyanate), 0.3 parts of benzoyl peroxide (commercial name "NYPER BMT" manufactured by Nippon Oils Co., Ltd.), and 0.1 parts of γ-epoxypropoxypropylmethoxysilane (commercial name "KBM-403" manufactured by Shin-Etsu Chemical Co., Ltd.).

[0168] (3) Formation of adhesive layer

[0169] The acrylic adhesive composition obtained in (2) above was applied to one side of a polyethylene terephthalate (PET) film (manufactured by Mitsubishi Chemical Polyester Film Co., Ltd., thickness: 38 μm) that had been treated with silicone, so that the thickness of the dried adhesive layer reached 10 μm. The film was dried at 150°C for 3 minutes to form adhesive 1 as an adhesive layer (adhesive bonding layer).

[0170] [Reference Example 2: Formation of the adhesive layer (adhesive 2)]

[0171] The adhesive layer of this reference example (reference example 2) was formed according to the steps (1) to (3) below.

[0172] (1) Preparation of (meth)acrylic acid polymer (A1) solution

[0173] A monomer mixture containing 79.5 parts butyl acrylate, 15 parts N-acryloylmorpholine, 5 parts acrylic acid, and 0.5 parts 4-hydroxybutyl acrylate was added to a four-necked flask equipped with a stirring blade, thermometer, nitrogen inlet tube, and condenser. Further, 0.1 parts of 2,2'-azobisisobutyronitrile (2,2'-Azobisisobutyronitrile) as a polymerization initiator was added along with 70 parts ethyl acetate to 100 parts of the monomer mixture. After nitrogen purging by slowly stirring and introducing nitrogen, the liquid temperature in the flask was maintained at approximately 55°C for 2 hours to prepare a solution of a (meth)acrylic acid polymer (A1) with a weight-average molecular weight (Mw) of 3 million and an Mw / Mn ratio of 2.5.

[0174] (2) Preparation of (meth)acrylic adhesive compositions

[0175] A solution of an acrylic adhesive composition was prepared by mixing 100 parts of the solid component of the obtained (meth)acrylic polymer (A1) solution with 0.2 parts of isocyanate crosslinking agent (commercial name "CORONATE L" manufactured by Nippon Polyurethane Industry Co., Ltd., an adduct of trimethylolpropane toluene diisocyanate) and 0.2 parts of epoxy crosslinking agent 1,3-bis(N,N-diglycidylaminomethyl)cyclohexane (commercial name "TETRAD C" manufactured by Mitsubishi Gas Chemical Co., Ltd.).

[0176] (3) Formation of adhesive layer

[0177] Next, the solution of the above acrylic adhesive composition was applied to one side of a polyethylene terephthalate membrane (separator: manufactured by Mitsubishi Chemical Polyester Film Co., Ltd., MRF38) treated with an organosilicon release agent in such a way that the thickness of the dried adhesive layer reached 10 μm. The membrane was dried at 155°C for 1 minute, and adhesive 2 as an adhesive layer (adhesive bonding layer) was formed on the surface of the separator.

[0178] [Reference Example 3: Formation of the adhesive layer (adhesive 3)]

[0179] The adhesive layer of this reference example (reference example 3) was formed according to the steps (1) to (3) below.

[0180] (1) Preparation of acrylic polymer solutions

[0181] In a four-necked flask equipped with a stirring blade, thermometer, nitrogen inlet tube, and condenser, 99 parts of butyl acrylate, 1 part of 4-hydroxybutyl acrylate, and 0.1 parts of 2,2'-azobisisobutyronitrile (2,2'-azobisisobutyronitrile) as a polymerization initiator, along with 100 parts of ethyl acetate, were added. Next, nitrogen was introduced while slowly stirring the contents of the four-necked flask to perform nitrogen purging. Then, the liquid temperature in the four-necked flask was maintained at approximately 55°C for 8 hours to carry out the polymerization reaction, preparing a solution of acrylic polymer.

[0182] (2) Preparation of acrylic adhesive compositions

[0183] A solution of an acrylic adhesive composition was prepared by combining 100 parts of the solid component of the acrylic polymer solution obtained in (1) above with 0.1 parts of isocyanate crosslinking agent (trade name "Takenate D110N" manufactured by Mitsui Takeda Chemical Co., Ltd., trimethylolpropane dimethyl diisocyanate), 0.1 parts of benzoyl peroxide (trade name "NYPER BMT" manufactured by Nippon Oils & Fats Co., Ltd.), and 0.2 parts of γ-epoxypropoxypropylmethoxysilane (trade name "KBM-403" manufactured by Shin-Etsu Chemical Co., Ltd.).

[0184] (3) Formation of adhesive layer

[0185] The solution of the acrylic adhesive composition obtained in (2) above was applied to one side of a polyethylene terephthalate membrane (separator: manufactured by Mitsubishi Chemical Polyester Film Co., Ltd., trade name "MRF38") after being treated with an organosilicon stripper, and dried at 150°C for 3 minutes to form an adhesive 3 with a thickness of 20 μm as an adhesive layer (adhesive bonding layer) on the surface of the separator.

[0186] [Examples 1-8, Comparative Examples 1-3: Fabrication of laminates containing void layers]

[0187] The laminates containing void layers of Examples 1-8 and Comparative Examples 1-3 were manufactured using the following method.

[0188] (Example 1)

[0189] (1) Gel formation of silicon compounds (synthesis process of gel-like silica)

[0190] Mixture A was prepared by dissolving 1.90 g of methyltrimethoxysilane (MTMS) and 0.1 g of tetraethoxysilane (TEOS), precursors of silicon compounds, in 4.4 g of dimethyl sulfoxide (DMSO). 1.0 g of a 0.01 mol / L aqueous oxalic acid solution was added to mixture A, and the mixture was stirred at room temperature for 30 minutes, thereby hydrolyzing MTMS to generate mixture B containing trihydroxymethylsilane and tetrahydroxysilane. After adding 0.38 g of 28% by weight ammonia and 0.2 g of pure water to 5.5 g of DMSO, mixture B was further added, and the mixture was stirred at room temperature for 15 minutes, thereby gelling the trihydroxymethylsilane and tetrahydroxysilane to obtain mixture C containing a gel-like silicon compound.

[0191] (2) Aging treatment

[0192] The mixture C containing the gel-like silicon compound prepared as described above was directly incubated at 40°C for 20 hours to perform a curing treatment.

[0193] (3) Pulverization process (gel pulverization process)

[0194] Next, the gel-like silicon compound, after being cured as described above, was broken into particles of several mm to several cm in size using a scraper. Then, 40 g of isopropanol (IPA) was added to mixture C, and after gentle stirring, it was allowed to stand at room temperature for 6 hours to decant the solvent and catalyst in the gel. Solvent replacement was achieved by performing the same decanting process three times, yielding mixture D. Next, the gel-like silicon compound in mixture D was subjected to high-pressure, media-free grinding. The grinding process (high-pressure, media-free grinding) was performed using a homogenizer (SMT Corporation, trade name "UH-50"). 1.85 g of the gel-like compound and 1.15 g of IPA from mixture D were weighed into a 5 cc screw-top bottle, and then ground for 2 minutes at 50 W and 20 kHz.

[0195] Through this pulverization process, the gel-like silicon compound in the above-mentioned mixture D is pulverized, thereby forming a sol solution E of pulverized material from mixture D. The volume average particle size, representing the particle size deviation of the pulverized material contained in sol solution E, was confirmed using a dynamic light scattering nano-trajectory particle size analyzer (manufactured by Nikkiso Corporation, UPA-EX150 type), and the result was 0.50~0.70 μm. Furthermore, relative to 0.75 g of sol solution E, 0.124 g of a 1.5 wt% MEK (methyl ethyl ketone) solution (Wako Pure Chemical Industries Co., Ltd., trade name: WPBG266), a precursor of the crosslinking reaction promoter, and 0.036 g of a 5 wt% MEK solution (bis(trimethoxysilyl)hexane), a crosslinking aid, were added to obtain a coating solution for forming a low refractive index layer.

[0196] A low-refractive-index layer forming solution was applied to an acrylic substrate and dried to form a porous layer with a thickness of approximately 850 nm (porosity 59% by volume). It should be noted that a wire rod was used for coating, and the drying temperature and drying time were set to 100°C and 2 minutes, respectively. Next, the porous layer was subjected to UV irradiation (300 mJ) to bond the fragments of the aforementioned gel-like compound together (bonding process). It should be noted that the bonding of the fragments of the aforementioned gel-like compound based on the bonding process likely includes at least one of cross-linking bonding (covalent bonding) where the fragments bond directly without a cross-linking aid, and cross-linking bonding (covalent bonding) via the aforementioned cross-linking aid. Then, an adhesive 1 with a thickness of 10 μm was bonded to the porous layer and cured at 50°C for 30 hours to produce the porous layer of this embodiment. Furthermore, a laminate of this embodiment was manufactured using the manufactured porous layer.

[0197] (Example 2)

[0198] The amounts of the photoalkali-generating agent and crosslinking aid in Example 1 were changed to a ratio of 0.186 g of a 1.5% by weight MEK (methyl ethyl ketone) solution of the photoalkali-generating agent (Wako Pure Chemical Industries, Ltd., trade name: WPBG266) and 0.054 g of a 5% by weight MEK solution of the crosslinking aid (1,6-bis(trimethoxysilyl)hexane) relative to 0.75 g of sol solution E. Otherwise, the same procedures as in Example 1 were performed to manufacture the void layer of this embodiment. Furthermore, the laminate of this embodiment was manufactured using the manufactured void layer.

[0199] (Example 3)

[0200] The amount of tetraethoxysilane (TEOS) added in Example 1 was changed to 0.2g, but the same operation as in Example 1 was performed to manufacture the void layer of this embodiment. Furthermore, the laminate of this embodiment was manufactured using the manufactured void layer.

[0201] (Example 4)

[0202] The amount of tetraethoxysilane (TEOS) added in Example 1 was changed to 0.2g, and the same operation as in Example 2 was performed to manufacture the void layer of this embodiment. Furthermore, the laminate of this embodiment was manufactured using the manufactured void layer.

[0203] (Example 5)

[0204] Adhesive 2 was used instead of adhesive 1 used in Example 1, and the void layer of this embodiment was manufactured by performing the same operations as in Example 1. Furthermore, the laminate of this embodiment was manufactured using the manufactured void layer.

[0205] (Example 6)

[0206] The amount of tetraethoxysilane (TEOS) added in Example 1 was changed to 0.3g, but the same operation as in Example 1 was performed to manufacture the void layer of this embodiment. Furthermore, the manufactured void layer was used to manufacture the laminate of this embodiment.

[0207] (Example 7)

[0208] The amount of tetraethoxysilane (TEOS) added in Example 1 was changed to 0.4 g, but the same operation as in Example 1 was performed to manufacture the void layer of this embodiment. Furthermore, the laminate of this embodiment was manufactured using the manufactured void layer.

[0209] (Example 8)

[0210] The amount of tetraethoxysilane (TEOS) added in Example 1 was changed to 0.2 g, and the amounts of the photoalkalizing agent and the dual crosslinking accelerator were changed to 0.062 g of a 1.5% by weight MEK (methyl ethyl ketone) solution of the photoalkalizing agent (Wako Pure Chemical Industries, Ltd., trade name: WPBG266) and 0.018 g of a 5% by weight MEK solution of the dual crosslinking accelerator ((trimethoxysilyl)hexane) relative to 0.75 g of sol solution E. Otherwise, the same operation as in Example 1 was performed to manufacture the void layer of this embodiment. Furthermore, the laminate of this embodiment was manufactured using the manufactured void layer.

[0211] (Comparative Example 1)

[0212] In Example 9, tetraethoxysilane (TEOS) was not added, but the same procedures as in Example 9 were performed to manufacture the void layer of this comparative example. Furthermore, the manufactured void layer was used to manufacture a laminate of this comparative example.

[0213] (Comparative Example 2)

[0214] Adhesive 2 was used instead of adhesive 1 used in Comparative Example 1, and the void layer of this Comparative Example was manufactured by performing the same operation as in Comparative Example 1. Furthermore, the laminate of this embodiment was manufactured using the manufactured void layer.

[0215] (Comparative Example 3)

[0216] Adhesive 3 was used instead of adhesive 1 used in Comparative Example 1, and the same operation as in Comparative Example 1 was performed to manufacture the void layer of this comparative example. Furthermore, the manufactured void layer was used to manufacture the laminate of this comparative example.

[0217]

[0218] As shown in Table 1 above, the interlayer peel strength of the laminate containing the void layer in the embodiment is 3 N / 25 mm or more, which is good. On the other hand, the interlayer peel strength of the laminates in the comparative examples is less than 3 N / 25 mm.

[0219] in addition, Figure 4 A coordinate graph is shown, illustrating the relationship between peel strength and refractive index for examples and comparative examples where the nanoindentation hardness reached 0.5 MPa or higher when fabricating the laminate. Figure 4 In the examples, the formula "Y = 136.4x - 159.92" is a linear function representing the average of two points from Examples 1 and 2, where the amounts of the trifunctional silane compound and the tetrafunctional silane compound are 3.5 mol%, and only the amounts of the crosslinking aid and the substance that generates the crosslinking reaction promoter are varied. The formula "Y = 141.37x - 165.06" is a linear function representing the average of three points from Examples 3, 4, and 8, where the amounts of the trifunctional silane compound and the tetrafunctional silane compound are 6.9 mol%, and only the amounts of the crosslinking aid and the substance that generates the crosslinking reaction promoter are varied.

[0220] like Figure 4 As shown, in all embodiments, the peel strength between the void layer and the adhesive layer reached 3 N / 25 mm or more. Furthermore, the void layers in all embodiments achieved results satisfying condition (1) (Y≥80X-93.8) described in the embodiment. It is also known that the void layers in the embodiments, by containing a tetrafunctional silane compound as a silane compound, exhibited greater peel strength compared to void layers with the same refractive index that do not contain a tetrafunctional silane compound. That is, results satisfying condition (2) (Y≥100X-117) described in the embodiment were achieved. Additionally, by increasing the proportion of the crosslinking aid and the crosslinking reaction promoter (the precursor of the crosslinking reaction promoter), further improvements in peel strength were obtained.

[0221] This disclosure may also be described, for example, as in the following notes. However, the following notes are examples, and this disclosure is not limited to these methods.

[0222] (Postscript 1)

[0223] A porous layer, which is a porous layer formed by the chemical bonding of fragments of a gel-like silicon compound.

[0224] The aforementioned gel-like silicon compounds are compounds formed by the condensation or partial condensation of silane compounds.

[0225] The aforementioned silane compounds include 1- to 3-functional silane compounds and 4-functional silane compounds.

[0226] The refractive index of the aforementioned void layer is below 1.30.

[0227] (Postscript 2)

[0228] According to the void layer described in Appendix 1, wherein,

[0229] The content of the above-mentioned 4-functional silane compounds is 1-25 mol relative to the amount of the 1-3 functional silane compounds.

[0230] (Note 3)

[0231] According to the void layer described in Appendix 1 or 2, wherein,

[0232] The aforementioned porous layer is formed by the chemical bonding of the pulverized gel-like silicon compound under the coexistence of additives.

[0233] The aforementioned additive includes at least one of a cross-linking reaction promoter and its precursor.

[0234] The aforementioned precursor is a substance that generates the aforementioned cross-linking reaction promoter through light or heat.

[0235] (Postscript 4)

[0236] According to the void layer described in Appendix 3, wherein...

[0237] The aforementioned cross-linking reaction promoters are acidic or alkaline substances.

[0238] (Note 5)

[0239] According to the void layer described in Appendix 3 or 4, wherein,

[0240] The total content of the crosslinking reaction promoter and its precursor is 1 mol% or more, relative to the total amount of the above-mentioned 1-3 functional silane compounds and the above-mentioned 4 functional silane compounds.

[0241] (Note 6)

[0242] According to any one of Appendices 1 to 5, the void layer, wherein,

[0243] The aforementioned porous layer is formed by the chemical bonding of the pulverized gel-like silicon compound under the coexistence of additives.

[0244] The aforementioned additives include cross-linking auxiliaries.

[0245] (Note 7)

[0246] According to the void layer described in Appendix 6, wherein,

[0247] The total content of the crosslinking aid is 1 mol% or more, relative to the total amount of the 1-3 functional silane compounds and the 4 functional silane compounds mentioned above.

[0248] (Note 8)

[0249] A porous layer, which is formed by the chemical bonding of fragments of a gel-like silicon compound in the presence of additives.

[0250] The aforementioned gel-like silicon compounds are compounds formed by the condensation or partial condensation of silane compounds.

[0251] The additives described above include at least one of a crosslinking reaction promoter and its precursor, and a crosslinking auxiliary agent.

[0252] Relative to the total amount of the aforementioned silane compounds, the total content of the aforementioned crosslinking reaction promoter and its precursor is 1.5 mol% or more, and the total content of the aforementioned crosslinking auxiliaries is 2.0 mol% or more.

[0253] The refractive index of the aforementioned void layer is below 1.30.

[0254] (Note 9)

[0255] A method for manufacturing a porous layer includes a gel-like silica synthesis step, a gel pulverization step, and a bonding step.

[0256] The above-mentioned process for synthesizing gel-like silica includes a step of synthesizing gel-like silicon compounds by condensing or partially condensing silane compounds.

[0257] The aforementioned silane compounds include 1- to 3-functional silane compounds and 4-functional silane compounds.

[0258] The above-mentioned gel pulverization process includes the step of pulverizing the above-mentioned gel-like silicon compound to obtain pulverized material.

[0259] The above-mentioned bonding process includes a process of chemically bonding the above-mentioned pulverized materials.

[0260] (Postscript 10)

[0261] A method for manufacturing a porous layer includes a gel-like silica synthesis step, a gel pulverization step, and a bonding step.

[0262] The above-mentioned process for synthesizing gel-like silica includes a step of synthesizing gel-like silicon compounds by condensing or partially condensing silane compounds.

[0263] The above-mentioned gel pulverization process includes the step of pulverizing the above-mentioned gel-like silicon compound to obtain pulverized material.

[0264] The aforementioned bonding process includes a step of chemically bonding the aforementioned pulverized materials under conditions where additives are present.

[0265] The additive includes at least one of a crosslinking reaction promoter and its precursor, and a crosslinking auxiliary agent.

[0266] (Postscript 11)

[0267] A laminate comprising a void layer as described in any one of Appendices 1 to 8, and an adhesive layer,

[0268] The aforementioned adhesive layer is directly laminated on one or both sides of the aforementioned void layer.

[0269] (Postscript 12)

[0270] An optical component comprising a void layer as described in any one of Appendices 1 to 8.

[0271] (Postscript 13)

[0272] An optical component comprising the laminate described in Appendix 11.

[0273] (Postscript 14)

[0274] An optical device comprising the optical components described in Appendix 12.

[0275] (Postscript 15)

[0276] The optical device described in Appendix 14 is an image display device or an illumination device.

[0277] (Postscript 16)

[0278] An optical device comprising the optical components described in Appendix 13.

[0279] (Postscript 17)

[0280] The optical device described in Appendix 16 is an image display device or an illumination device.

[0281] Industrial applicability

[0282] As described above, according to this disclosure, a void layer with low refractive index and excellent mechanical strength, a method for manufacturing the void layer, a laminate, an optical component, and an optical device can be provided. The application of this disclosure is not particularly limited. For example, the optical device of this disclosure is not particularly limited, and examples include image display devices and lighting devices. Examples of image display devices include, for example, liquid crystal displays, organic EL displays, and micro LED displays. Examples of lighting devices include, for example, organic EL lighting. Furthermore, the application of the laminate of this disclosure is not limited to the optical components and optical devices of this disclosure, and can be used in a wide range of applications.

[0283] This application claims priority based on Japanese Application Special Purpose 2023-107487, filed on June 29, 2023, the entire contents of which are hereby cited.

Claims

1. A porous layer, which is a porous layer formed by chemically bonding fragments of a gel-like silicon compound. The gel-like silicon compound is a compound formed by the condensation or partial condensation of silane compounds. The silane compounds include 1- to 3-functional silane compounds and 4-functional silane compounds. The refractive index of the void layer is below 1.

30.

2. The void layer according to claim 1, wherein, The content of the 4-functional silane compound is 1-25 mol relative to the amount of the 1-3 functional silane compound.

3. The void layer according to claim 1, wherein, The void layer is formed by the chemical bonding of the pulverized gel-like silicon compound under the coexistence of additives. The additive includes at least one of a cross-linking reaction promoter and its precursor. The precursor is a substance that generates the crosslinking reaction promoter through light or heat.

4. The void layer according to claim 3, wherein, The cross-linking reaction promoter is an acidic or alkaline substance.

5. The void layer according to claim 3, wherein, The total content of the crosslinking reaction promoter and its precursor is 1 mol% or more, relative to the total amount of the 1-3 functional silane compounds and the 4 functional silane compounds.

6. The void layer according to claim 1, wherein, The void layer is formed by the chemical bonding of the pulverized gel-like silicon compound under the coexistence of additives. The additive includes a cross-linking aid.

7. The void layer according to claim 6, wherein, The total content of the crosslinking aid is 1 mol% or more relative to the total amount of the 1-3 functional silane compounds and the 4 functional silane compounds.

8. A porous layer, which is a porous layer formed by the chemical bonding of pulverized gel-like silicon compounds in the presence of additives. The gel-like silicon compound is a compound formed by the condensation or partial condensation of silane compounds. The additive comprises at least one of a crosslinking reaction promoter and its precursor, and a crosslinking auxiliary agent. Relative to the total mass of the silane compound, the total content of the crosslinking reaction promoter and its precursor is 1.5 mol% or more, and the total content of the crosslinking auxiliaries is 2.0 mol% or more. The refractive index of the void layer is below 1.

30.

9. A method for manufacturing a porous layer, comprising a gel-like silica synthesis step, a gel pulverization step, and a bonding step. The process for synthesizing gel-like silica includes a step of synthesizing a gel-like silicon compound by condensing or partially condensing a silane compound. The silane compounds include 1-3 functional silane compounds and 4 functional silane compounds. The gel pulverization process includes the step of pulverizing the gel-like silicon compound to obtain pulverized material. The bonding process includes a step of chemically bonding the pulverized materials.

10. A method for manufacturing a porous layer, comprising a gel-like silica synthesis step, a gel pulverization step, and a bonding step. The process for synthesizing gel-like silica includes a step of synthesizing a gel-like silicon compound by condensing or partially condensing a silane compound. The gel pulverization process includes the step of pulverizing the gel-like silicon compound to obtain pulverized material. The bonding process includes a step of chemically bonding the pulverized materials under conditions of coexistence of additives. The additive includes at least one of a crosslinking reaction promoter and its precursor, and a crosslinking auxiliary agent.

11. A laminate comprising: The void layer according to any one of claims 1 to 8, and Adhesive layer, The adhesive layer is directly stacked on one or both sides of the void layer.

12. An optical component comprising a void layer according to any one of claims 1 to 8.

13. An optical component comprising the laminate of claim 11.

14. An optical device comprising the optical component of claim 12.

15. The optical device according to claim 14, wherein it is an image display device or an illumination device.

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