JP2001089202A - Sunlight shielding laminated glass - Google Patents

Sunlight shielding laminated glass

Info

Publication number
JP2001089202A
JP2001089202A JP22128099A JP22128099A JP2001089202A JP 2001089202 A JP2001089202 A JP 2001089202A JP 22128099 A JP22128099 A JP 22128099A JP 22128099 A JP22128099 A JP 22128099A JP 2001089202 A JP2001089202 A JP 2001089202A
Authority
JP
Japan
Prior art keywords
fine particles
laminated glass
solar
glass
solar shading
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP22128099A
Other languages
Japanese (ja)
Inventor
Kenichi Fujita
賢一 藤田
Kayo Yabuki
佳世 矢吹
Hiromitsu Takeda
広充 武田
Kenji Adachi
健治 足立
Takashi Muromachi
隆 室町
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Metal Mining Co Ltd
Nippon Sheet Glass Co Ltd
Original Assignee
Sumitomo Metal Mining Co Ltd
Nippon Sheet Glass Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sumitomo Metal Mining Co Ltd, Nippon Sheet Glass Co Ltd filed Critical Sumitomo Metal Mining Co Ltd
Priority to JP22128099A priority Critical patent/JP2001089202A/en
Publication of JP2001089202A publication Critical patent/JP2001089202A/en
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/10009—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
    • B32B17/10036—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising two outer glass sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
    • B32B17/10614—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer comprising particles for purposes other than dyeing
    • B32B17/10633—Infrared radiation absorbing or reflecting agents

Abstract

PROBLEM TO BE SOLVED: To provide a sunlight shielding laminated glass improved in sunlight shielding function and having high transmissive performance to visible ray region. SOLUTION: The sunlight shielding laminated glass is formed by interposing an intermediate layer having the sunlight shielding function between 2 glass sheets. The intermediate layers is formed from an intermediate film composed of an adding liquid, which is prepared by dispersing at least one kind of hexaborate fine particle selected from a group composed of LaB6, CeB6, PrB6, NdB6, GdB6, TbB6, DyB6, HoB6, YB6, SmB6, EuB6, ErB6, TmB6, YbB6, LuB6, (La, Ce)B6, SrB6 and CaB6 and if necessary, ITO fine particle and/or ATO fine particle in a plasticizer, and a vinyl resin.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【０００１】[0001]

【発明の属する技術分野】本発明は、自動車などの車両
用の安全ガラス、建物の窓ガラスなどとして用いられる
日射遮蔽用合わせガラスに関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a laminated glass for shielding sunlight, which is used as safety glass for vehicles such as automobiles and window glass of buildings.

【０００２】[0002]

【従来の技術】従来の自動車用などの安全ガラスとして
は、板ガラス間に日射遮蔽膜を挟み込んでガラスから入
る太陽エネルギーを遮断し、冷房負荷や人の熱暑感の軽
減を目的としたものが提案されている。2. Description of the Related Art A conventional safety glass for an automobile or the like has a solar light shielding film interposed between glass sheets to block solar energy from the glass, thereby reducing a cooling load and a feeling of heat and heat of a person. Proposed.

【０００３】従来の自動車用などの安全ガラスとして
は、板ガラス間に日射遮蔽膜を挟み込んでガラスから入
る太陽エネルギーを遮断し、冷房負荷や人の熱暑感の軽
減を目的としたものが提案されている。例えば特開平８
−２１７５００号公報によれば、かかる合わせガラスは
一対の板ガラス間に、０．１μｍ以下の微細な粒径の酸
化錫あるいは酸化インジウムからなる熱線遮蔽性金属酸
化物を含有した軟質樹脂層を介在せしめて構成されてい
る。また特開平８−２５９２７９号公報には、少なくと
も２枚の板ガラスの間に、Ｓｎ、Ｔｉ、Ｓｉ、、Ｚｎ、
Ｚｒ、Ｆｅ、Ａｌ、Ｃｒ、Ｃｏ、Ｃｅ、Ｉｎ、Ｎｉ、Ａ
ｇ、Ｃｕ、Ｐｔ、Ｍｎ、Ｔａ、Ｗ、Ｖ、Ｍｏの金属、酸
化物、窒化物、硫化物あるいはＳｂやＦのドープ物また
はこれらの複合物を分散した中間層を設けて構成した合
わせガラスが開示されている。さらに特開平４−１６０
０４号公報にはＴｉＯ２、ＺｒＯ２、ＳｎＯ２、Ｉｎ ２
Ｏ２からなる超微粒子と有機ケイ素あるいは有機ケイ素
化合物からなるガラス成分性とを透明板状部材の間に介
在させた自動車用窓ガラスが記載されている。さらにま
た特開平１０−２９７９４５号公報には少なくとも２枚
の透明ガラス板状体の間に、３層からなる中間層を設
け、中間層のうち第２層の中間層にはＳｎ、Ｔｉ、Ｓ
ｉ、Ｚｎ、Ｚｒ、Ｆｅ、Ａｌ、Ｃｒ、Ｃｏ、Ｉｎ、Ｎ
ｉ、Ａｇ、Ｃｕ、Ｐｔ、Ｍｎ、Ｔａ、Ｗ、Ｖ、Ｍｏの金
属、酸化物、窒化物、硫化物あるいはＳｂやＦのドープ
物またはこれらの複合物を分散し、また第１層と第３層
の中間層を樹脂層とした合わせガラスを記述している。As a conventional safety glass for automobiles and the like
Is inserted from the glass by sandwiching the solar shading film between the glass sheets.
Cuts off solar energy and reduces the cooling load and the heat and heat of people.
Those aimed at reduction have been proposed. For example, JP-A-8
According to -217500, such a laminated glass is
An acid having a fine particle size of 0.1 μm or less is placed between a pair of glass sheets.
Heat shielding metallic acid composed of tin oxide or indium oxide
Is formed by interposing a soft resin layer containing
You. Also, JP-A-8-259279 discloses at least
Between two glass sheets, Sn, Ti, Si, Zn,
Zr, Fe, Al, Cr, Co, Ce, In, Ni, A
g, Cu, Pt, Mn, Ta, W, V, Mo metal, acid
Or nitride, sulfide or Sb or F dope or
Is a composite that has an intermediate layer in which these composites are dispersed.
Laminated glass is disclosed. Further, JP-A-4-160
No. 04 discloses TiO2, ZrO2, SnO2, In 2
O2Ultra-fine particles consisting of organosilicon or organosilicon
The glass component of the compound is interposed between the transparent plate members.
Window glass for automobiles. Even better
Japanese Patent Laid-Open No. 10-297945 discloses at least two sheets.
An intermediate layer consisting of three layers
The second intermediate layer among the intermediate layers is Sn, Ti, S
i, Zn, Zr, Fe, Al, Cr, Co, In, N
i, Ag, Cu, Pt, Mn, Ta, W, V, Mo gold
Metal, oxide, nitride, sulfide or Sb or F dope
Or a composite thereof, and a first layer and a third layer
Describes a laminated glass in which the intermediate layer is a resin layer.

【０００４】[0004]

【発明が解決しようとする課題】しかしながら、これら
公報に記載された従来の技術に係る合わせガラスは日遮
機能や可視光透過性能が十分ではなく、その改善が求め
られていた。本発明は、日射遮蔽機能を高め、かつ可視
光領域の高い透過性能を有する日射遮蔽合わせガラスを
提供することを目的とするものである。However, the laminated glass according to the prior art described in these publications does not have a sufficient sunshade function and visible light transmission performance, and improvements have been demanded. An object of the present invention is to provide a solar-shielded laminated glass having an enhanced solar-shielding function and having high transmission performance in the visible light region.

【０００５】[0005]

【課題を解決するための手段】上記目的を達成するため
に本発明者らは、２枚の板ガラスの間に介在する中間膜
または該中間膜と日射遮蔽膜からなる中間層について種
々検討した結果、自由電子を多量に保有する６ホウ化物
微粒子に着目し、これを超微粒子化し、所望に応じてＩ
ＴＯやＡＴＯ微粒子とともに可塑剤に分散してなる添加
液を作製し、この添加液をビニル系樹脂に添加したビニ
ル系樹脂組成物をシート状に成形して中間膜を形成する
とともに、２枚の板ガラス間に前記シート状に形成した
中間膜を挟み込むか、または日射遮蔽機能を有する塗布
液を内側に塗布した２枚のガラス、あるいは１枚の板ガ
ラスと日射遮蔽機能を有する塗布液を内側に塗布して日
射遮蔽膜を形成した２枚の板ガラス、あるい１枚の板ガ
ラスと他の通常の１枚の板ガラスの間に前記のように形
成した中間膜、もしくはビニル系樹脂に可塑剤を加えて
シート状に成形した従来の中間膜を挟み込んで中間層と
する方法で日射遮蔽用合わせガラスを作製することによ
り、該日射遮蔽用合わせガラスが可視光領域に透過率の
極大を持つとともに、近赤外領域に強い吸収を発現して
透過率の極小を持つことを見出して本発明を完成するに
至った。Means for Solving the Problems In order to achieve the above object, the present inventors have conducted various studies on an intermediate film interposed between two glass sheets or an intermediate layer comprising the intermediate film and the solar radiation shielding film. Attention was focused on hexaboride fine particles having a large amount of free electrons, which were converted to ultrafine particles.
An additive liquid is prepared by dispersing the additive liquid in a plasticizer together with TO or ATO fine particles. The vinyl resin composition obtained by adding the additive liquid to a vinyl resin is formed into a sheet to form an intermediate film. The intermediate film formed in the form of a sheet is sandwiched between sheet glasses, or two sheets of glass coated with a coating liquid having a solar shading function on the inside, or one sheet glass and a coating liquid having a solar shading function are coated on the inside A plasticizer is added to two sheets of glass on which a solar shading film is formed, or an interlayer formed as described above between one sheet of glass and another normal sheet of glass, or a vinyl resin. By producing a laminated glass for solar shading by sandwiching a conventional interlayer formed into a sheet into an intermediate layer, the laminated glass for solar shading has a transmittance maximum in the visible light region. , And have completed the present invention have found to have a minimum transmittance expressing strong absorption in the near infrared region.

【０００６】すなわち本発明の第１の実施態様に係る日
射遮蔽用合わせガラスは、日射遮蔽機能を有する中間層
を２枚の板ガラス間に介在せしめてなる日射遮蔽合わせ
ガラスであって、前記中間層は、ＬａＢ６、ＣｅＢ６、
ＰｒＢ６、ＮｄＢ６、ＧｄＢ ６、ＴｂＢ６、ＤｙＢ６、
ＨｏＢ６、ＹＢ６、ＳｍＢ６、ＥｕＢ６、ＥｒＢ６、Ｔ
ｍＢ６、ＹｂＢ６、ＬｕＢ６、（Ｌａ、Ｃｅ）Ｂ６、Ｓ
ｒＢ６およびＣａＢ６からなる群から選択された少なく
とも１種の６ホウ化物微粒子を可塑剤に分散させた添加
液と、ビニル系樹脂とからなる中間膜により形成される
ことを特徴とするものである。That is, a date according to the first embodiment of the present invention.
Laminated glass for solar shading is an intermediate layer that has a solar shading function
Of solar radiation between two glass sheets
Glass, wherein the intermediate layer is LaB6, CeB6,
PrB6, NdB6, GdB 6, TbB6, DyB6,
HoB6, YB6, SmB6, EuB6, ErB6, T
mB6, YbB6, LuB6, (La, Ce) B6, S
rB6And CaB6Selected from the group consisting of
Addition of one type of hexaboride fine particles dispersed in a plasticizer
Formed by an intermediate film composed of a liquid and a vinyl resin
It is characterized by the following.

【０００７】また本発明の第２の実施態様に係る日射遮
蔽用合わせガラスは、日射遮蔽機能を有する中間層を２
枚の板ガラス間に介在せしめてなる日射遮蔽合わせガラ
スであって、前記中間層は、ＬａＢ６、ＣｅＢ６、Ｐｒ
Ｂ６、ＮｄＢ６、ＧｄＢ６、ＴｂＢ６、ＤｙＢ６、Ｈｏ
Ｂ６、ＹＢ６、ＳｍＢ６、ＥｕＢ６、ＥｒＢ６、ＴｍＢ
６、ＹｂＢ６、ＬｕＢ６、（Ｌａ、Ｃｅ）Ｂ６、ＳｒＢ
６およびＣａＢ６からなる群から選択された少なくとも
１種の６ホウ化物微粒子、ならびにＩＴＯ微粒子および
／またはＡＴＯ微粒子とを可塑剤に分散させた添加液
と、ビニル系樹脂とからなる中間膜により形成されるこ
とを特徴とするものであり、また前記６ホウ化物微粒子
と、前記ＩＴＯ微粒子および／またはＡＴＯ微粒子との
重量比を０．１：９９．９〜９０：１０の範囲とするこ
とを特徴とするものである。[0007] The laminated glass for solar shading according to the second embodiment of the present invention comprises an intermediate layer having a solar shading function.
A solar-shielding laminated glass interposed between two glass sheets, wherein the intermediate layer is composed of LaB 6 , CeB 6 , Pr
B 6 , NdB 6 , GdB 6 , TbB 6 , DyB 6 , Ho
B 6 , YB 6 , SmB 6 , EuB 6 , ErB 6 , TmB
6, YbB 6, LuB 6, (La, Ce) B 6, SrB
6 and CaB 6, formed by an intermediate film comprising a vinyl resin and an additive liquid in which at least one type of hexaboride fine particles selected from the group consisting of 6 and CaB 6 and ITO fine particles and / or ATO fine particles are dispersed in a plasticizer. Wherein the weight ratio of the hexaboride fine particles to the ITO fine particles and / or ATO fine particles is in the range of 0.1: 99.9 to 90:10. It is assumed that.

【０００８】そして前記本発明の第１の実施態様および
第２の実施態様において、前記可塑剤が、トリエチレン
グリコール−ジ−２−エチルブチレートである。[0008] In the first and second embodiments of the present invention, the plasticizer is triethylene glycol-di-2-ethylbutyrate.

【０００９】さらに本発明の第３の実施態様に係る日射
遮蔽用合わせガラスは、日射遮蔽機能を有する中間層を
２枚の板ガラス間に介在せしめてなる日射遮蔽合わせガ
ラスであって、前記中間層は、少なくとも一方の板ガラ
スの内側に位置する面に形成され、かつＬａＢ６、Ｃｅ
Ｂ６、ＰｒＢ６、ＮｄＢ６、ＧｄＢ６、ＴｂＢ６、Ｄｙ
Ｂ６、ＨｏＢ６、ＹＢ６、ＳｍＢ６、ＥｕＢ６、ＥｒＢ
６、ＴｍＢ６、ＹｂＢ ６、ＬｕＢ６、（Ｌａ、Ｃｅ）Ｂ
６、ＳｒＢ６およびＣａＢ６からなる群から選択された
少なくとも１種の６ホウ化物微粒子を日射遮蔽成分とし
て含有する塗布液を塗布して形成された日射遮蔽膜と、
前記２枚の板ガラス間に介在されるビニル系樹脂を含有
する中間膜により形成されることを特徴とするものであ
る。Further, the solar radiation according to the third embodiment of the present invention.
Laminated glass for shielding has an intermediate layer that has a solar radiation shielding function.
Solar-shielding interlocking gas interposed between two glass sheets
A lath, wherein the intermediate layer has at least one plate glass.
Formed on the surface located inside the6, Ce
B6, PrB6, NdB6, GdB6, TbB6, Dy
B6, HoB6, YB6, SmB6, EuB6, ErB
6, TmB6, YbB 6, LuB6, (La, Ce) B
6, SrB6And CaB6Selected from the group consisting of
At least one type of hexaboride fine particles as a solar radiation shielding component
A solar shading film formed by applying a coating solution containing
Contains vinyl resin interposed between the two glass sheets
Characterized by being formed by an intermediate film
You.

【００１０】さらにまた本発明の第４の実施態様に係る
日射遮蔽用合わせガラスは、日射遮蔽機能を有する中間
層を２枚の板ガラス間に介在せしめてなる日射遮蔽合わ
せガラスであって、前記中間層は、少なくとも一方の板
ガラスの内側に位置する面に形成され、かつＬａＢ６、
ＣｅＢ６、ＰｒＢ６、ＮｄＢ６、ＧｄＢ６、ＴｂＢ６、
ＤｙＢ６、ＨｏＢ６、ＹＢ６、ＳｍＢ６、ＥｕＢ６、Ｅ
ｒＢ６、ＴｍＢ６、ＹｂＢ６、ＬｕＢ６、（Ｌａ、Ｃ
ｅ）Ｂ６、ＳｒＢ６およびＣａＢ６からなる群から選択
された少なくとも１種の６ホウ化物微粒子と、ＩＴＯ微
粒子およびＡＴＯ微粒子のうち１種以上とを日射遮蔽成
分として含有する塗布液を塗布して形成された日射遮蔽
膜と、前記２枚の板ガラス間に介在されるビニル系樹脂
を含有する中間膜により形成されることを特徴とするも
のである。[0010] Furthermore, a laminated glass for solar radiation according to a fourth embodiment of the present invention is a laminated glass for solar radiation wherein an intermediate layer having a solar radiation shielding function is interposed between two glass sheets. The layer is formed on a surface located on the inside of at least one of the sheet glass, and LaB 6 ,
CeB 6 , PrB 6 , NdB 6 , GdB 6 , TbB 6 ,
DyB 6 , HoB 6 , YB 6 , SmB 6 , EuB 6 , E
rB 6 , TmB 6 , YbB 6 , LuB 6 , (La, C
at least one hexaboride particles selected from the group consisting of e) B 6, SrB 6 and CaB 6, a coating solution containing as a solar radiation shielding component and one or more of ITO fine particles and the ATO fine particles was applied And an intermediate film containing a vinyl-based resin interposed between the two glass sheets.

【００１１】そして前記本発明の第３および第４の実施
態様において、前記中間膜が日射遮蔽機能を有すること
が好ましい。In the third and fourth embodiments of the present invention, it is preferable that the intermediate film has a solar shading function.

【００１２】[0012]

【発明の実施の形態】まず本発明においては中間層の形
態としては以下を含むものとする。 ２枚の板ガラス間に介在して両板ガラスを密着すると
ともに、日射遮蔽成分を可塑剤に分散させた添加液をビ
ニル系樹脂に添加してなるビニル系樹脂組成物からなる
中間膜のみからなる中間層。 少なくとも一方の板ガラスの内側に位置する面に形成
され、かつ日射遮蔽成分を可塑剤に分散された添加液に
バインダーを添加してなる塗布液を塗布して形成された
日射遮蔽膜と、２枚の板ガラス間に介在して密着する前
記ビニル系樹脂組成物からなる中間膜とからなる中間
層。 少なくとも一方の板ガラスの内側に位置する面に形成
され、かつ日射遮蔽成分を可塑剤に分散された添加液に
バインダーを添加してなる塗布液を塗布して形成された
日射遮蔽膜と、２枚の板ガラス間に介在して密着するビ
ニル系樹脂に可塑剤を加えてなる従来の中間膜とからな
る中間層。DESCRIPTION OF THE PREFERRED EMBODIMENTS In the present invention, the form of the intermediate layer includes the following. An intermediate film consisting of only a vinyl-based resin composition obtained by adding an additive liquid in which a solar-shielding component is dispersed in a plasticizer to a vinyl-based resin while interposing the two glass plates in close contact with each other between two glass plates. layer. A solar shading film formed by applying a coating liquid formed by adding a binder to an additional liquid in which a solar shading component is dispersed in a plasticizer, which is formed on a surface located inside at least one of the plate glasses, and two sheets And an intermediate film made of the vinyl resin composition and interposed between and adhered to the glass sheets. A solar shading film formed by applying a coating liquid formed by adding a binder to an additional liquid in which a solar shading component is dispersed in a plasticizer, which is formed on a surface located inside at least one of the plate glasses, and two sheets An intermediate layer composed of a conventional interlayer formed by adding a plasticizer to a vinyl resin interposed between and adhered to the sheet glass.

【００１３】つぎに本発明の日射遮蔽合わせガラスに用
いる添加液は、日射遮蔽成分としての６ホウ化物微粒
子、６ホウ化物微粒子とＩＴＯ（錫含有酸化インジウ
ム）微粒子、６ホウ化物微粒子とＡＴＯ（アンチモン含
有酸化錫）微粒子、あるいは６ホウ化物微粒子とＩＴＯ
微粒子とＡＴＯ微粒子を可塑剤と溶媒の混合液に均一に
分散して作製されるものである。Next, the additive liquid used for the solar-shielding laminated glass of the present invention includes fine particles of hexaboride, fine particles of hexaboride and fine particles of ITO (tin-containing indium oxide), fine particles of hexaboride and fine particles of ATO (antimony) as a solar-shielding component. Containing tin oxide) or hexaboride fine particles and ITO
It is produced by uniformly dispersing fine particles and ATO fine particles in a mixture of a plasticizer and a solvent.

【００１４】そして本発明に使用される６ホウ化物微粒
子としては、６ホウ化ランタン（ＬａＢ６）、６ホウ化
セリウム（ＣｅＢ６）、６ホウ化プラセオジム（ＰｒＢ
６）、６ホウ化ネオジム（ＮｄＢ６）、６ホウ化ガドリ
ニウム（ＧｄＢ６）、６ホウ化テルビウム（Ｔｂ
Ｂ６）、６ホウ化ディスプロシウム（ＤｙＢ６）、６ホ
ウ化ホルミウム（ＨｏＢ６）、６ホウ化イットリウム
（ＹＢ６）、６ホウ化サマリウム（ＳｍＢ６）、６ホウ
化ユーロピウム（ＥｕＢ６）、６ホウ化エルビウム（Ｅ
ｒＢ６）、６ホウ化ツリウム（ＴｍＢ６）、６ホウ化イ
ッテルビウム（ＹｂＢ６）、６ホウ化ルテチウム（Ｌｕ
Ｂ６）、６ホウ化ランタンセリウム（（Ｌａ、Ｃｅ）Ｂ
６）、６ホウ化ストロンチウム（ＳｒＢ６）、６ホウ化
カルシウム（ＣａＢ６）の微粒子あるいはこれらの混合
物の微粒子などが、その代表的なものとして挙げられ
る。The fine particles of hexaboride used in the present invention include lanthanum hexaboride (LaB 6 ), cerium hexaboride (CeB 6 ), and praseodymium hexaboride (PrB).
6 ), neodymium hexaboride (NdB 6 ), gadolinium hexaboride (GdB 6 ), terbium hexaboride (Tb)
B 6 ), dysprosium hexaboride (DyB 6 ), holmium hexaboride (HoB 6 ), yttrium hexaboride (YB 6 ), samarium hexaboride (SmB 6 ), europium hexaboride (EuB 6 ) , Erbium hexaboride (E
rB 6 ), thulium hexaboride (TmB 6 ), ytterbium hexaboride (YbB 6 ), lutetium hexaboride (Lu)
B 6 ), lanthanum cerium hexaboride ((La, Ce) B
6 ), strontium hexaboride (SrB 6 ), calcium hexaboride (CaB 6 ) fine particles, or fine particles of a mixture thereof, and the like.

【００１５】また本発明に使用される６ホウ化物微粒子
としては、その表面が酸化していないことが好ましい
が、通常は僅かに酸化していることが多く、また微粒子
の分散工程で表面の酸化が起こることはある程度避けら
れない。しかしその場合でも日射遮蔽効果を発現する有
効性には何ら影響を与えない。It is preferable that the surface of the hexaboride fine particles used in the present invention is not oxidized, but usually the surface is often slightly oxidized. Is inevitable to some extent. However, even in that case, there is no effect on the effectiveness of expressing the solar shading effect.

【００１６】さらにこれらの６ホウ化物微粒子は、結晶
としての完全性が高いほど大きい日射遮蔽効果が得られ
るが、結晶性が低くＸ線回折でブロードな回折ピークを
生じるようなものであっても、微粒子内部の基本的な結
合が各金属とホウ素の結合からなり立っているものであ
るならば日射遮蔽効果を発現することができる。Further, these hexaboride fine particles have a higher solar radiation shielding effect as the crystal perfection is higher. However, even if the hexaboride fine particles have low crystallinity and cause a broad diffraction peak in X-ray diffraction, If the basic bond inside the fine particles is composed of the bond between each metal and boron, the solar radiation shielding effect can be exhibited.

【００１７】これらの６ホウ化物微粒子は灰黒色、茶黒
色、緑黒色などに着色した粉末であるが、粒径が可視光
波長に比べて十分小さく中間膜中あるいは日射遮蔽膜中
に分散した状態においては中間膜あるいは日射遮蔽膜に
可視光透過性が生じるが、赤外光遮蔽能は十分強く保持
できる。この理由は詳細には判明していないが、これら
微粒子中の自由電子の量が多く、微粒子内部および表面
の自由電子によるバンド間間接遷移の吸収エネルギーが
まさに可視〜近赤外の付近にあるために、この波長領域
の熱線が選択的に反射・吸収されるものと考えられる。
実験によればこれら微粒子を十分細かく、かつ均一に分
散した膜では、透過率が波長４００ｎｍ〜７００ｎｍの
間に極大値を持ち、また波長７００ｎｍ〜１８００ｎｍ
の間に極小値を持ち、さらにこれらの透過率の極大値と
極小値の差が１５ポイント以上であることが観察され
る。可視光波長が３８０ｎｍ〜７８０ｎｍであり、視感
度が５５０ｎｍ付近をピークとする釣鐘型であることを
考慮すると、このような膜では可視光を有効に透過しそ
れ以外の熱線を有効に反射・吸収する。These hexaboride fine particles are powders colored in gray black, brown black, green black or the like, and have a particle size sufficiently smaller than the wavelength of visible light and dispersed in an intermediate film or a solar shading film. In the above, visible light transmission occurs in the intermediate film or the solar shading film, but the infrared light shading ability can be maintained sufficiently strong. Although the reason for this has not been elucidated in detail, the amount of free electrons in these fine particles is large, and the absorption energy of the indirect interband transition by free electrons inside and on the surface of the fine particles is exactly in the vicinity of the visible to near infrared. In addition, it is considered that heat rays in this wavelength region are selectively reflected and absorbed.
According to experiments, in a film in which these fine particles are sufficiently fine and uniformly dispersed, the transmittance has a maximum value between wavelengths of 400 nm to 700 nm, and a wavelength of 700 nm to 1800 nm.
It is observed that the difference between the maximum value and the minimum value of the transmittance is 15 points or more. Considering that the wavelength of visible light is 380 nm to 780 nm and that the visibility is a bell shape with a peak around 550 nm, such a film effectively transmits visible light and effectively reflects and absorbs other heat rays. I do.

【００１８】つぎに本発明で６ホウ化物微粒子と併せて
使用されるＩＴＯ微粒子およびＡＴＯ微粒子は、可視光
領域で光の反射・吸収が殆どなく、１０００ｎｍ以上の
領域でプラズマ共鳴に由来する反射・吸収が大きい。こ
れらの透過プロファイルは近赤外領域で長波長側に向か
うにしたがって右下がりとなる。Next, the ITO fine particles and the ATO fine particles used in combination with the hexaboride fine particles in the present invention hardly reflect or absorb light in the visible light region, and have a reflection or absorption derived from plasma resonance in a region of 1000 nm or more. Large absorption. These transmission profiles decrease rightward toward the longer wavelength side in the near infrared region.

【００１９】一方、６ホウ化物の透過プロファイルは１
０００ｎｍ付近にボトムをもち、それより長波長側では
徐々に右上がりを示す。このため６ホウ化物とＩＴＯや
ＡＴＯとを併用することによって可視光透過率は減少さ
せずに、近赤外領域の太陽光線を遮蔽することが可能と
なり、ＩＴＯ微粒子やＡＴＯ微粒子をそれぞれ単独ある
いは組合わせて使用するよりも日射遮蔽特性を向上させ
ることができる。On the other hand, the transmission profile of hexaboride is 1
It has a bottom near 000 nm and gradually rises to the right on the longer wavelength side. For this reason, it is possible to shield sunlight rays in the near infrared region without reducing the visible light transmittance by using hexaboride and ITO or ATO in combination, and the ITO fine particles and the ATO fine particles can be used alone or in combination. The solar shading characteristics can be improved as compared with the case of using together.

【００２０】また６ホウ化物の単位重量当たりの日射遮
蔽能力は非常に高く、ＩＴＯやＡＴＯと比較して１０分
の１以下の使用量でその効果を発揮する。さらにＩＴＯ
やＡＴＯと併用することによって、一定の可視光透過率
を保ちながら日射遮蔽特性のみを一層向上させることが
できるのでコストも削減できる。また全微粒子の使用量
を大幅に削減することができるので、中間膜や日射遮蔽
膜の摩耗強度や耐候性を向上させることが可能となる。In addition, the hexaboride has a very high solar shading ability per unit weight, and exhibits its effect with a usage of 1/10 or less as compared with ITO or ATO. More ITO
When used together with ATO or ATO, only the solar shading property can be further improved while maintaining a constant visible light transmittance, so that the cost can be reduced. Further, since the usage amount of all the fine particles can be greatly reduced, it is possible to improve the wear strength and weather resistance of the intermediate film and the solar shading film.

【００２１】さらに６ホウ化物は使用量を増すと可視光
領域に吸収があるため、その添加量を制御することによ
り可視光領域の吸収を自由に制御でき、明るさ調整やプ
ライバシー保護などの応用もできる。Further, since the hexaboride has an absorption in the visible light region when the amount of use is increased, the absorption in the visible light region can be freely controlled by controlling the amount of addition, and the application of brightness adjustment, privacy protection, etc. Can also.

【００２２】そして使用する６ホウ化物微粒子の粒径は
２００ｎｍ以下とすることが好ましく、より好ましくは
１００ｎｍ以下とする。平均粒径が２００ｎｍよりも大
きい微粒子もしくは凝集した粗大粒子は、成形した中間
膜または塗布した日射遮蔽膜からなる中間層の光散乱源
となって該中間層が曇ってしまうからである。The particle size of the hexaboride fine particles used is preferably 200 nm or less, more preferably 100 nm or less. This is because the fine particles or the aggregated coarse particles having an average particle diameter larger than 200 nm serve as a light scattering source of the formed intermediate film or the intermediate layer formed of the applied solar shading film, and the intermediate layer becomes cloudy.

【００２３】またＩＴＯ微粒子やＡＴＯ微粒子も前記同
様の理由で２００ｎｍ以下とすることが好ましく、より
好ましくは１００ｎｍ以下とする。The ITO fine particles and the ATO fine particles are also preferably 200 nm or less, more preferably 100 nm or less for the same reason as described above.

【００２４】そして６ホウ化物微粒子と、ＩＴＯ微粒子
および／またはＡＴＯ微粒子との重量比は０．１：９
９．９〜９０：１０の範囲であることが好ましく、この
重量比範囲よりも６ホウ化物微粒子が少ないと、全微粒
子の使用量をあまり削減できず、コス卜削減効果が小さ
く、日射遮蔽特性も悪くなる。一方前記重量比範囲より
も６ホウ化物微粒子が多くても日射遮蔽特性が悪くな
る。The weight ratio of hexaboride fine particles to ITO fine particles and / or ATO fine particles is 0.1: 9.
It is preferably in the range of 9.9 to 90:10, and if the amount of the hexaboride fine particles is smaller than this weight ratio range, the usage of all the fine particles cannot be reduced so much, the cost reduction effect is small, and the solar shading property is small. Also gets worse. On the other hand, even if the amount of the hexaboride fine particles is larger than the above-mentioned weight ratio range, the solar shading property is deteriorated.

【００２５】前記微粒子を溶媒に分散する方法は、微粒
子が均一に溶媒中に分散する方法であれば任意に選択で
きるが、例としてはビーズミル、ボールミル、サンドミ
ル、超音波分散などの方法を挙げることができ、前記微
粒子を溶媒に分散することによって本発明の日射遮蔽合
わせガラスとして用いる中間膜あるいは日射遮蔽膜用添
加液が作製されることになる。The method of dispersing the fine particles in the solvent can be arbitrarily selected as long as the fine particles are uniformly dispersed in the solvent. Examples of the method include a bead mill, a ball mill, a sand mill, and an ultrasonic dispersion method. By dispersing the fine particles in a solvent, an intermediate film or an additive for a solar shading film used as the solar shading laminated glass of the present invention is produced.

【００２６】なお前記添加液において前記微粒子を添加
して分散するための溶媒は特に限定されるものではな
く、中間膜や日射遮蔽膜を形成する条件やビニル系樹脂
組成物を調製する際に配合されるビニル系樹脂などに合
わせて選択することが可能であり、例えばジオクチルフ
タレート、ジブチルフタレート、ジイソブチルフタレー
ト、アジピン酸−ジ−２−エチルヘキシル、アジピン酸
ジイソデシル、エポキシ脂肪酸モノエステル、トリエチ
レングリコール−ジ−２−エチルブチレート、トリエチ
レングリコール−ジ−２−エチルヘキソエート、セバシ
ン酸ジブチル、ジブチルセバケートなどの可塑剤を挙げ
ることができ、またアルコール、エーテル、エステル、
ケトンなどの一般的な有機溶媒の各種も使用可能であ
る。また必要に応じて酸やアルカリを添加してｐＨを調
整してもよい。The solvent for adding and dispersing the fine particles in the additive solution is not particularly limited, and may be used under the conditions for forming an intermediate film or a solar shading film, or when preparing a vinyl resin composition. It can be selected according to the vinyl resin to be used and the like, for example, dioctyl phthalate, dibutyl phthalate, diisobutyl phthalate, di-2-ethylhexyl adipate, diisodecyl adipate, epoxy fatty acid monoester, triethylene glycol-diethyl Plasticizers such as -2-ethyl butyrate, triethylene glycol-di-2-ethylhexoate, dibutyl sebacate and dibutyl sebacate; and alcohols, ethers, esters,
Various common organic solvents such as ketones can also be used. If necessary, the pH may be adjusted by adding an acid or an alkali.

【００２７】さらに前記ビニル系樹脂組成物を調製する
当たり、ビニル系樹脂中に前記微粒子を含有させる際に
その分散安定性を一層向上させるために、以下の可塑剤
や各種の界面活性剤、カップリング剤などを添加するこ
とも可能である。In preparing the vinyl resin composition, the following plasticizers, various surfactants, and cups may be used in order to further improve the dispersion stability when the fine particles are contained in the vinyl resin. It is also possible to add a ring agent and the like.

【００２８】そして前記ビニル系樹脂に添加される可塑
剤としては特に限定されず、例えばジオクチルフタレー
ト、ジブチルフタレート、ジイソブチルフタレート、ア
ジピン酸−ジ−２−エチルヘキシル、アジピン酸ジイソ
デシル、エポキシ脂肪酸モノエステルトリエチレングリ
コール−ジ−２−エチルブチレート、トリエチレングリ
コール−ジ−２−エチルヘキソエート、セバシン酸ジブ
チル、ジブチルセバケートなどが挙げられる。The plasticizer added to the vinyl resin is not particularly restricted but includes, for example, dioctyl phthalate, dibutyl phthalate, diisobutyl phthalate, di-2-ethylhexyl adipate, diisodecyl adipate, and monoester triethylene fatty acid. Glycol-di-2-ethylbutyrate, triethylene glycol-di-2-ethylhexoate, dibutyl sebacate, dibutyl sebacate, and the like are included.

【００２９】さらに前記のようにして調製された添加液
を用いてビニル系樹脂組成物を調製する場合に使用され
るビニル系樹脂としては、例えばポリビニルブチラー
ル、ポリ塩化ビニル、塩化ビニル−エチレン共重合体、
塩化ビニル−エチレン−グリシジルメタクリレート共重
合体、塩化ビニル−エチレン−グリシジルアクリレート
共重合体、塩化ビニル−グリシジルメタクリレート共重
合体、塩化ビニル−グリシジルアクリレート共重合体、
ポリ塩化ビニリデン、塩化ビニリデン−アクリロニトリ
ル共重合体、ポリ酢酸ビニルエチレン−酢酸ビニル共重
合体、ポリビニルアセタール−ポリビニルブチラール混
合物などが挙げられる。特にポリビニルブチラールが好
ましい。The vinyl resin used when preparing the vinyl resin composition using the additive solution prepared as described above includes, for example, polyvinyl butyral, polyvinyl chloride, and vinyl chloride-ethylene copolymer. Coalescing,
Vinyl chloride-ethylene-glycidyl methacrylate copolymer, vinyl chloride-ethylene-glycidyl acrylate copolymer, vinyl chloride-glycidyl methacrylate copolymer, vinyl chloride-glycidyl acrylate copolymer,
Examples thereof include polyvinylidene chloride, a vinylidene chloride-acrylonitrile copolymer, a polyvinyl acetate ethylene-vinyl acetate copolymer, a polyvinyl acetal-polyvinyl butyral mixture, and the like. Particularly, polyvinyl butyral is preferable.

【００３０】つぎに本発明に係る中間膜の形成方法には
公知の方法が用いられ、例えばカレンダーロール法、押
出法、キャスティング法、インフレーション法などを用
いることができる。特に本発明の日射遮蔽合わせガラス
用中間層としてビニル系樹脂組成物からなる中間膜を用
いる場合、該ビニル系樹脂組成物はビニル系樹脂に前記
添加液を添加して、混練して微粒子が均一に分散してな
るものであり、このように調製されたビニル系樹脂組成
物をシート状に成形することができる。ビニル系樹脂組
成物をシート状に成形する際には、必要に応じて熱安定
剤、酸化防止剤などを配合し、またシートの貫通性を高
めるために接着力調整剤（例えば金属塩）を配合しても
よい。Next, a known method is used for forming the intermediate film according to the present invention. For example, a calender roll method, an extrusion method, a casting method, an inflation method and the like can be used. In particular, when an interlayer made of a vinyl-based resin composition is used as the interlayer for solar radiation-shielded laminated glass of the present invention, the vinyl-based resin composition is obtained by adding the additive liquid to a vinyl-based resin, kneading the mixture, and uniformly dispersing the fine particles. The vinyl resin composition thus prepared can be formed into a sheet. When the vinyl resin composition is formed into a sheet, a heat stabilizer, an antioxidant, and the like may be added as necessary, and an adhesive force modifier (eg, a metal salt) may be added to enhance the sheet penetration. You may mix.

【００３１】また日射遮蔽用合わせガラスを構成する前
記２枚の板ガラスの少なくとも一方の内側に位置する面
に、日射遮蔽成分として６ホウ化物微粒子をエチルシリ
ケートなどのバインダーに分散させてなる塗布液を塗布
して日射遮蔽膜を形成したり、あるいは日射遮蔽成分と
して６ホウ化物微粒子と、ＩＴＯ微粒子およびＡＴＯ微
粒子のうち１種以上とを前記バインダーに分散させてな
る塗布液を塗布して日射遮蔽膜を形成し、ついで両板ガ
ラス間にビニル系樹脂に可塑剤を添加して軟化・液状化
したものをシート状に成形した従来の中間膜あるいは前
記ビニル系樹脂組成物からなるシート状の中間膜を介在
せしめて密着させて日射遮蔽用合わせガラスを形成する
こともできる。Further, a coating liquid obtained by dispersing hexaboride fine particles as a solar radiation shielding component in a binder such as ethyl silicate is coated on at least one of the two glass sheets constituting the laminated glass for solar radiation shielding. A solar shading film is formed by coating, or a coating solution obtained by dispersing hexaboride fine particles as a solar shading component and at least one of ITO fine particles and ATO fine particles in the binder is applied. A conventional interlayer or a sheet-like interlayer made of the vinyl-based resin composition is formed by adding a plasticizer to a vinyl resin between the two glass sheets and then softening and liquefying the resultant into a sheet. It is also possible to form a laminated glass for solar shading by interposing and closely contacting.

【００３２】このように本発明によれば、日射遮蔽成分
として６ホウ化物微粒子を含有する添加液をビニル系樹
脂に添加し、さらに可塑剤を加えて均一に分散させて調
製されたビニル系樹脂組成物をシート状に成形した中間
膜を用いて合わせガラスを作製したり、または前記添加
液にバインダーを添加してなる塗布液を２枚の板ガラス
の少なくとも一方の内側に位置する面に塗布して日射遮
蔽膜を形成し、前記ビニル系樹脂組成物からなる中間膜
あるいは従来の中間膜を用いて合わせガラスを作製する
ことで高コストの物理成膜法や複雑な工程を用いずに日
射遮蔽機能を有し、かつ可視光域の高い透過性能を有す
る日射遮蔽用合わせガラスを提供することが可能とな
る。As described above, according to the present invention, a vinyl resin prepared by adding an additive solution containing hexaboride fine particles as a solar shading component to a vinyl resin, further adding a plasticizer, and uniformly dispersing the vinyl resin. A laminated glass is produced using an intermediate film obtained by molding the composition into a sheet shape, or a coating solution obtained by adding a binder to the additive solution is applied to at least one surface of two plate glasses located on the inner side. Forming a solar-shielding film by using an intermediate film made of the vinyl resin composition or a laminated glass using a conventional intermediate film, thereby eliminating the need for high-cost physical film-forming methods and complicated processes. It is possible to provide a laminated glass for solar shading which has a function and has a high transmission performance in a visible light region.

【００３３】また日射遮蔽成分として、近赤外領域に強
い吸収を持つ６ホウ化物微粒子と、ＡＴＯ微粒子および
／またはＩＴＯ微粒子とを併用して調製された添加液を
ビニル系樹脂に添加しさらに可塑剤を加えて均一に分散
させて調製されたビニル系樹脂組成物をシート状に成形
した中間膜を用いて合わせガラスを作製したり、または
前記添加液にバインダーを添加してなる塗布液を２枚の
板ガラスの少なくとも一方の内側に位置する面に塗布し
て日射遮蔽膜を形成し、前記ビニル系樹脂組成物からな
る中間膜あるいは従来の中間膜を用いて合わせガラスを
作製することでＡＴＯやＩＴＯそれぞれの微粒子を単独
あるいは組合わせて使用するよりも日射遮蔽特性を向上
させ、中間膜や日射遮蔽膜の作製時のＡＴＯ微粒子やＩ
ＴＯ微粒子の使用量を減少させ、材料コストを低減させ
ることも可能となる。Further, as a solar shading component, an additive liquid prepared by using a combination of hexaboride fine particles having strong absorption in the near infrared region and ATO fine particles and / or ITO fine particles is added to a vinyl resin, followed by further plasticization. A laminated glass is produced using an interlayer formed by sheeting a vinyl-based resin composition prepared by adding and uniformly dispersing a vinyl resin composition, or a coating solution obtained by adding a binder to the above-mentioned additive solution is used. ATO or the like by forming a solar radiation shielding film by applying to at least one surface located inside one of the sheet glass to form a laminated glass using an intermediate film made of the vinyl resin composition or a conventional intermediate film. The solar shading characteristics are improved as compared with the use of individual fine particles of ITO alone or in combination.
It is also possible to reduce the use amount of the TO fine particles and reduce the material cost.

【００３４】[0034]

【実施例】以下に本発明の実施例を比較例とともに説明
する。EXAMPLES Examples of the present invention will be described below together with comparative examples.

【００３５】（実施例１）平均粒径６７ｎｍのＬａＢ６
微粒子２０ｇ、ジアセトンアルコール（ＤＡＡ）５０
ｇ、トリエチレングリコール−ジ−２−エチルブチレー
ト２０ｇ、水および分散剤を適量混合し、直径４ｍｍの
ジルコニアボールを用いて１００時間ボールミル混合し
て、ＬａＢ６微粒子が分散した中間膜用添加液１００ｇ
を作製した（Ａ液）。Example 1 LaB 6 having an average particle size of 67 nm
Fine particles 20 g, diacetone alcohol (DAA) 50
g, triethylene glycol - di-2-ethyl butyrate 20g, water and a dispersing agent mixed with an appropriate amount, and mixing 100 hours in a ball mill containing zirconia balls having a diameter of 4 mm, the intermediate layer additive liquid LaB 6 fine particles are dispersed 100g
Was prepared (Solution A).

【００３６】一方平均粒径８０ｎｍのＩＴＯ微粒子２０
ｇ、トリエチレングリコール−ジ−２−エチルブチレー
ト７０ｇ、水および分散剤を適量混合し、直径４ｍｍの
ジルコニアボールを用いて１００時間ボールミル混合し
て、ＩＴＯ微粒子が分散した中間膜用添加液１００ｇを
作製した（Ｂ液）。On the other hand, ITO fine particles 20 having an average particle size of 80 nm
g, 70 g of triethylene glycol-di-2-ethyl butyrate, water and a suitable amount of a dispersing agent, and ball milling using a zirconia ball having a diameter of 4 mm for 100 hours to obtain 100 g of an additive liquid for an intermediate film in which ITO fine particles are dispersed. Was prepared (Solution B).

【００３７】Ａ液とＢ液を混合して調製した中間膜用添
加液をポリビニルブチラールに添加し、可塑剤としてト
リエチレングリコール−ジ−２−エチルブチレートを加
え、ＩＴＯ濃度が０．６１重量％、ＬａＢ６濃度が０．
００３８重量％、ポリビニルブチラール濃度が７０重量
％となるようにビニル系樹脂組成物を調製した。Addition solution for an intermediate film prepared by mixing Solution A and Solution B was added to polyvinyl butyral, and triethylene glycol-di-2-ethylbutyrate was added as a plasticizer to give an ITO concentration of 0.61% by weight. %, LaB 6 concentration is zero.
A vinyl resin composition was prepared so that the concentration of 0038% by weight and the concentration of polyvinyl butyral became 70% by weight.

【００３８】このビニル系樹脂組成物をロールで混練し
て０．７６ｍｍ厚のシート状に成形して中間膜を作製し
た。この中間膜を厚さ２．５ｍｍの透明なフロートガラ
ス２枚の間に挟み込み、８０℃に加熱して仮接着した
後、１４０℃、１４ｋｇ／ｃｍ ２のオートクレーブによ
り本接着を行い、合わせガラスを作製した。This vinyl resin composition is kneaded with a roll.
Into a 0.76 mm thick sheet to form an interlayer
Was. This intermediate film is transparent float glass with a thickness of 2.5 mm.
Sandwiched between two pieces of paper and heated to 80 ° C. for temporary bonding
After, 140 ° C, 14kg / cm 2By autoclave
The main bonding was performed to produce a laminated glass.

【００３９】作製された合わせガラスの分光特性は日立
製作所製の分光光度計を用いて測定し、ＪＩＳ Ｒ ３
１０６にしたがって日射透過率、またＪＩＳ Ｒ ３２
１１にしたがって可視光透過率を算出し、その結果を表
１に示す。The spectral characteristics of the laminated glass thus produced were measured using a spectrophotometer manufactured by Hitachi, Ltd.
Insolation transmittance according to 106, JIS R 32
The visible light transmittance was calculated according to No. 11, and the results are shown in Table 1.

【００４０】また作製された合わせガラスについて下記
の要領でパンメル値を測定した結果、パンメル値は５で
あり、板ガラスと中間膜との密着性は十分であった。パ
ンメル試験：合わせガラスを１時間以上−１８℃に保っ
て恒温にした後、ハンマー（頭の部分が１ポンドであ
る）粉砕試験機にかけ、被着ガラス粒子径が最大６ｍｍ
以下になるまで粉砕した。割れたガラス片を振り落と
し、中間膜の露出した部分を０〜８のランクに分けて、
露出度が低いほど値が大きくなるように判定した。これ
は板ガラスと中間膜との密着力が所定の範囲内にあるか
どうかを判定する試験方法であり、その値は３〜６の範
囲内が望ましい。１以下では剥離し易く、一方８以上で
は耐貫通性が小さくなる。The Pummel value of the produced laminated glass was measured in the following manner. As a result, the Pummel value was 5, and the adhesion between the plate glass and the interlayer film was sufficient. Pummel test: After keeping the laminated glass at -18 ° C. for at least 1 hour and keeping it at a constant temperature, the laminated glass was subjected to a hammer (head portion is 1 lb.) crushing tester, and the particle diameter of the adhered glass was at most 6 mm.
Crushed until below. Shake off the broken glass pieces, divide the exposed part of the interlayer film into 0-8 ranks,
It was determined that the lower the degree of exposure, the larger the value. This is a test method for determining whether or not the adhesion between the sheet glass and the intermediate film is within a predetermined range, and the value is desirably in the range of 3 to 6. If it is 1 or less, it is easy to peel off, while if it is 8 or more, the penetration resistance becomes small.

【００４１】（実施例２〜５）Ａ液、Ｂ液、ポリビニル
ブチラール、トリエチレングリコール−ジ−２−エチル
ブチレートを表１の組成になるようにビニル系樹脂組成
物を調製した。これを実施例１と同様の方法で中間膜を
作製して目的とする合わせガラスを作製した。この合わ
せガラスの光学特性を表１に併せて示す。(Examples 2 to 5) A vinyl resin composition was prepared from solution A, solution B, polyvinyl butyral, and triethylene glycol di-2-ethyl butyrate so as to have the composition shown in Table 1. This was used to produce an intermediate film in the same manner as in Example 1 to produce the intended laminated glass. Table 1 also shows the optical characteristics of the laminated glass.

【００４２】（実施例６）Ａ液、ポリビエルブチラー
ル、トリエチレングリコール−ジ−２−エチルブチレー
トを表１の組成になるようにビニル系樹脂組成物を調製
した。これを実施例１と同様の方法で中間膜を作製して
目的とする合わせガラスを作製した。この合わせガラス
の光学特性を表１に併せて示す。Example 6 A vinyl resin composition was prepared from solution A, polybierbutyral, and triethylene glycol-di-2-ethyl butyrate so as to have the composition shown in Table 1. This was used to produce an intermediate film in the same manner as in Example 1 to produce the intended laminated glass. Table 1 also shows the optical characteristics of the laminated glass.

【００４３】（比較例１）Ｂ液、ポリビニルブチラー
ル、トリエチレングリコール−ジ−２−エチルブチレー
トを表１の組成になるようにビニル系樹脂組成物を調製
した。これを実施例１と同様の方法で中間膜を作製して
目的とする合わせガラスを作製した。この合わせガラス
の光学特性を表１に併せて示す。Comparative Example 1 A vinyl resin composition was prepared from Solution B, polyvinyl butyral, and triethylene glycol-di-2-ethyl butyrate so as to have the composition shown in Table 1. This was used to produce an intermediate film in the same manner as in Example 1 to produce the intended laminated glass. Table 1 also shows the optical characteristics of the laminated glass.

【００４４】つぎに比較例１および実施例１〜５の組成
と光学特性の変化を図１に示す。図１よりＬａＢ６微粒
子をごく微量添加することで、従来のＩＴＯの特性に比
べて可視光透過率を下げずに、さらに日射透過率を減少
させることが可能となり、またこの時ＩＴＯ微粒子量を
大幅に削減できることが分った。例えば比較例１と実施
例２とを比較すると、ＬａＢ６微粒子を中間膜中の全微
粒子に対して１．３８重量％添加したことによって、可
視光透過率は７８％に維持したまま日射透過率を３ポイ
ント以上下げることができ、さらにＩＴＯ添加量を半分
以下に軽減できる。これよりＬａＢ６微粒子の微量添加
で日射遮蔽特性の向上と、さらにコスト削減とが同時に
行なえることが明らかであった。Next, changes in the composition and optical characteristics of Comparative Example 1 and Examples 1 to 5 are shown in FIG. By trace amount added LaB 6 fine particles than 1, without lowering the visible light transmittance in comparison with the characteristics of the conventional ITO, it is possible to further reduce the solar radiation transmittance and the time ITO fine amount It turns out that it can be reduced significantly. For example, comparing the Comparative Example 1 and Example 2, LaB by the addition 1.38 wt% relative to the 6 particles all particles in the intermediate layer, while solar transmittance visible light transmittance was maintained at 78% Can be reduced by 3 points or more, and the amount of ITO added can be reduced to half or less. This and improve the solar radiation shielding properties in slight amount of LaB 6 fine particles from further and reduce costs was clear that performed simultaneously.

【００４５】（比較例２）平均粒径５５ｎｍのＡＴＯ微
粒子２０ｇ、トリエチレングリコール−ジ−２−エチル
ブチレート７０ｇ、水および分散剤を適量を混合して直
径４ｍｍのジルコニアボールを用いて１００時間ボール
ミル混合して、ＡＴＯ微粒子が分散した中間膜用添加液
１００ｇを作製した（Ｃ液）。(Comparative Example 2) 20 g of ATO fine particles having an average particle size of 55 nm, 70 g of triethylene glycol di-2-ethyl butyrate, water and a suitable amount of a dispersant were mixed, and the mixture was used for 100 hours using zirconia balls having a diameter of 4 mm. The mixture was mixed with a ball mill to prepare 100 g of an intermediate film additive liquid in which ATO fine particles were dispersed (Solution C).

【００４６】Ｃ液、ポリビニルブチラール、トリエチレ
ングリコール−ジ−２−エチルブチレートを表１の組成
になるようにビニル系樹脂組成物を調製した。これを実
施例１と同様の方法で中間膜を作製して目的とする合わ
せガラスを作製した。この合わせガラスの光学特性を表
１に併せて示す。Solution C, polyvinyl butyral, and triethylene glycol-di-2-ethyl butyrate were prepared into a vinyl resin composition so as to have the composition shown in Table 1. This was used to produce an intermediate film in the same manner as in Example 1 to produce the intended laminated glass. Table 1 also shows the optical characteristics of the laminated glass.

【００４７】（実施例７〜１０）Ａ液、Ｃ液、ポリビニ
ルブチラール、トリエチレングリコール−ジ−２−エチ
ルブチレートを表１の組成になるようにビニル系樹脂組
成物を調製した。これを実施例１と同様の方法で中間膜
を作製して目的とする合わせガラスを作製した。この合
わせガラスの光学特性を表１に併せて示す。(Examples 7 to 10) A vinyl resin composition was prepared from the solutions A, C, polyvinyl butyral, and triethylene glycol-di-2-ethyl butyrate so as to have the composition shown in Table 1. This was used to produce an intermediate film in the same manner as in Example 1 to produce the intended laminated glass. Table 1 also shows the optical characteristics of the laminated glass.

【００４８】つぎに比較例２および実施例７〜１０の組
成と光学特性の変化を図２に示す。図２よりＬａＢ６微
粒子をごく微量添加していくことで、従来のＡＴＯの特
性に比べて可視光透過率を下げずに、さらに日射透過率
を減少させることが可能となった。またこの時ＡＴＯ微
粒子量を大幅に削減できることが分った。例えば比較例
２と実施例８とを比較すると、ＬａＢ６微粒子を中間膜
中の全微粒子に対して１０．７１重量％添加したことに
よって、可視光透過率は７８％に維持したまま、日射透
過率を２ポイント程度下げることができ、さらにＡＴＯ
添加量を６０％以上削減できることが分った。Next, changes in the composition and optical characteristics of Comparative Example 2 and Examples 7 to 10 are shown in FIG. By going to trace amount added LaB 6 fine particles than 2, without lowering the visible light transmittance in comparison with the characteristic of the conventional ATO, it becomes possible to further reduce the solar transmittance. At this time, it was found that the amount of ATO fine particles could be significantly reduced. For example, comparing with Comparative Example 2 and Example 8, by the addition 10.71% by weight relative to the total particles in the intermediate layer the LaB 6 fine particles, while the visible light transmittance was maintained at 78%, a solar radiation transmittance Rate can be reduced by about 2 points, and ATO
It was found that the addition amount could be reduced by 60% or more.

【００４９】（実施例１１）平均粒径８５ｎｍのＣｅＢ
６微粒子２０ｇ、ジアセトンアルコール（ＤＡＡ）５０
ｇ、トリエチレングリコール−ジ−２−エチルブチレー
ト２０ｇ、水および分散剤を適量混合し、直径４ｍｍの
ジルコニアボールを用いて１００時間ボールミル混合し
て、ＣｅＢ６微粒子が分散した中間膜用添加液１００ｇ
を作製した（Ｄ液）。Example 11 CeB having an average particle size of 85 nm
6 Fine particles 20 g, diacetone alcohol (DAA) 50
g, 20 g of triethylene glycol-di-2-ethyl butyrate, water and a dispersant are mixed in appropriate amounts, and ball-mixed with zirconia balls having a diameter of 4 mm for 100 hours to obtain an additive solution for an intermediate film in which CeB 6 fine particles are dispersed. 100g
Was prepared (D solution).

【００５０】Ｄ液、Ｂ液、ポリビニルブチラール、トリ
エチレングリコール−ジ−２−エチルブチレートを表１
の組成になるようにビニル系樹脂組成物を調製した。こ
れを実施例１と同様の方法で中間膜を作製して目的とす
る合わせガラスを作製した。この合わせガラスの光学特
性を表１に併せて示す。Liquid D, Liquid B, polyvinyl butyral, and triethylene glycol-di-2-ethyl butyrate are shown in Table 1.
A vinyl resin composition was prepared so as to have the following composition. This was used to produce an intermediate film in the same manner as in Example 1 to produce the intended laminated glass. Table 1 also shows the optical characteristics of the laminated glass.

【００５１】（実施例１２）平均粒径８５ｎｍのＰｒＢ
６微粒子２０ｇ、ジアセトンアルコール（ＤＡＡ）５０
ｇ、トリエチレングリコール−ジ−２−エチルブチレー
ト２０ｇ、水および分散剤を適量混合し、直径４ｍｍの
ジルコニアボールを用いて１００時間ボールミル混合し
て、ＰｒＢ６微粒子が分散した中間膜用添加液１００ｇ
を作製した（Ｅ液）。Example 12 PrB having an average particle size of 85 nm
6 Fine particles 20 g, diacetone alcohol (DAA) 50
g, 20 g of triethylene glycol-di-2-ethyl butyrate, water and a dispersant are mixed in appropriate amounts, and ball milled using zirconia balls having a diameter of 4 mm for 100 hours to obtain an additive solution for an intermediate film in which PrB 6 fine particles are dispersed. 100g
Was prepared (Solution E).

【００５２】Ｅ液、Ｂ液、ポリビニルブチラール、トリ
エチレングリコール−ジ−２−エチルブチレートを表１
の組成になるようにビニル系樹脂組成物を調製した。こ
れを実施例１と同様の方法で中間膜を作製して目的とす
る合わせガラスを作製した。この合わせガラスの光学特
性を表１に併せて示す。Solution E, Solution B, polyvinyl butyral, and triethylene glycol-di-2-ethyl butyrate are shown in Table 1.
A vinyl resin composition was prepared so as to have the following composition. This was used to produce an intermediate film in the same manner as in Example 1 to produce the intended laminated glass. Table 1 also shows the optical characteristics of the laminated glass.

【００５３】（実施例１３）平均粒径８５ｎｍのＮｄＢ
６微粒子２０ｇ、ジアセトンアルコール（ＤＡＡ）５０
ｇ、トリエチレングリコール−ジ−２−エチルブチレー
ト２０ｇ、水および分散剤を適量混合し、直径４ｍｍの
ジルコニアボールを用いて１００時間ボールミル混合し
て、ＮｄＢ６微粒子が分散した中間膜用添加液１００ｇ
を作製した（Ｆ液）。(Example 13) NdB having an average particle size of 85 nm
6 Fine particles 20 g, diacetone alcohol (DAA) 50
g, 20 g of triethylene glycol-di-2-ethyl butyrate, water and a dispersant are mixed in an appropriate amount, and the mixture is ball-milled using zirconia balls having a diameter of 4 mm for 100 hours to obtain an additive for an intermediate film in which NdB 6 fine particles are dispersed. 100g
Was prepared (Solution F).

【００５４】Ｆ液、Ｃ液、ポリビニルブチラール、トリ
エチレングリコール−ジ−２−エチルブチレートを表１
の組成になるようにビニル系樹脂組成物を調製した。こ
れを実施例１と同様の方法で中間膜を作製して目的とす
る合わせガラスを作製した。この合わせガラスの光学特
性を表１に併せて示す。The solutions F, C, polyvinyl butyral, and triethylene glycol di-2-ethyl butyrate are shown in Table 1.
A vinyl resin composition was prepared so as to have the following composition. This was used to produce an intermediate film in the same manner as in Example 1 to produce the intended laminated glass. Table 1 also shows the optical characteristics of the laminated glass.

【００５５】（実施例１４）平均粒径８５ｎｍのＧｄＢ
６微粒子２０ｇ、ジアセトンアルコール（ＤＡＡ）５０
ｇ、トリエチレングリコール−ジ−２−エチルブチレー
ト２０ｇ、水および分散剤を適量混合し、直径４ｍｍの
ジルコニアボールを用いて１００時間ボールミル混合し
て、ＧｄＢ６微粒子が分散した中間膜用添加液１００ｇ
を作製した（Ｇ液）。(Example 14) GdB having an average particle size of 85 nm
6 Fine particles 20 g, diacetone alcohol (DAA) 50
g, triethylene glycol - di-2-ethyl butyrate 20g, water and a dispersing agent mixed with an appropriate amount, and mixing 100 hours in a ball mill containing zirconia balls having a diameter of 4 mm, the intermediate layer additive liquid GdB 6 fine particles are dispersed 100g
Was prepared (G solution).

【００５６】Ｇ液、Ｃ液、ポリビニルブチラール、トリ
エチレングリコール−ジ−２−エチルブチレートを表１
の組成になるようにビニル系樹脂組成物を調製した。こ
れを実施例１と同様の方法で中間膜を作製して目的とす
る合わせガラスを作製した。この合わせガラスの光学特
性を表１に併せて示す。Solution G, Solution C, polyvinyl butyral, and triethylene glycol-di-2-ethyl butyrate are shown in Table 1.
A vinyl resin composition was prepared so as to have the following composition. This was used to produce an intermediate film in the same manner as in Example 1 to produce the intended laminated glass. Table 1 also shows the optical characteristics of the laminated glass.

【００５７】（実施例１５）平均粒径８５ｎｍのＹＢ６
微粒子２０ｇ、ジアセトンアルコール（ＤＡＡ）５０
ｇ、トリエチレングリコール−ジ−２−エチルブチレー
ト２０ｇ、水および分散剤を適量混合し、直径４ｍｍの
ジルコニアボールを用いて１００時間ボールミル混合し
て、ＹＢ６微粒子が分散した中間膜用添加液１００ｇを
作製した（Ｈ液）。Example 15 YB 6 having an average particle size of 85 nm
Fine particles 20 g, diacetone alcohol (DAA) 50
g, triethylene glycol - di-2-ethyl butyrate 20g, water and a dispersing agent mixed with an appropriate amount, and mixing 100 hours in a ball mill containing zirconia balls having a diameter of 4 mm, the intermediate layer additive liquid YB 6 fine particles are dispersed 100 g was prepared (H solution).

【００５８】Ｈ液、Ｂ液、ポリビニルブチラール、トリ
エチレングリコール−ジ−２−エチルブチレートを表１
の組成になるようにビニル系樹脂組成物を調製した。こ
れを実施例１と同様の方法で中間膜を作製して目的とす
る合わせガラスを作製した。この合わせガラスの光学特
性を表１に併せて示す。The liquids H, B, polyvinyl butyral, and triethylene glycol-di-2-ethyl butyrate are shown in Table 1.
A vinyl resin composition was prepared so as to have the following composition. This was used to produce an intermediate film in the same manner as in Example 1 to produce the intended laminated glass. Table 1 also shows the optical characteristics of the laminated glass.

【００５９】（実施例１６）平均粒径８５ｎｍのＳｍＢ
６微粒子２０ｇ、ジアセトンアルコール（ＤＡＡ）５０
ｇ、トリエチレングリコール−ジ−２−エチルブチレー
ト２０ｇ、水および分散剤を適量混合し、直径４ｍｍの
ジルコニアボールを用いて１００時間ボールミル混合し
て、ＳｍＢ６微粒子が分散した中間膜用添加液１００ｇ
を作製した（Ｉ液）。(Example 16) SmB having an average particle size of 85 nm
6 Fine particles 20 g, diacetone alcohol (DAA) 50
g, triethylene glycol - di-2-ethyl butyrate 20g, water and a dispersing agent mixed with an appropriate amount, and mixing 100 hours in a ball mill containing zirconia balls having a diameter of 4 mm, the intermediate layer additive liquid SmB 6 fine particles are dispersed 100g
Was prepared (Solution I).

【００６０】Ｉ液、Ｃ液、ポリビニルブチラール、トリ
エチレングリコール−ジ−２−エチルブチレートを表１
の組成になるようにビニル系樹脂組成物を調製した。こ
れを実施例１と同様の方法で中間膜を作製して目的とす
る合わせガラスを作製した。この合わせガラスの光学特
性を表１に併せて示す。Solution I, Solution C, polyvinyl butyral, and triethylene glycol-di-2-ethyl butyrate are shown in Table 1.
A vinyl resin composition was prepared so as to have the following composition. This was used to produce an intermediate film in the same manner as in Example 1 to produce the intended laminated glass. Table 1 also shows the optical characteristics of the laminated glass.

【００６１】（実施例１７）平均粒径８５ｎｍのＥｕＢ
６微粒子２０ｇ、ジアセトンアルコール（ＤＡＡ）５０
ｇ、トリエチレングリコール−ジ−２−エチルブチレー
ト２０ｇ、水および分散剤を適量混合し、直径４ｍｍの
ジルコニアボールを用いて１００時間ボールミル混合し
て、ＥｕＢ６微粒子が分散した中間膜用添加液１００ｇ
を作製した（Ｊ液）。Example 17 EuB having an average particle size of 85 nm
6 Fine particles 20 g, diacetone alcohol (DAA) 50
g, 20 g of triethylene glycol-di-2-ethyl butyrate, water and a dispersant are mixed in appropriate amounts, and ball milled using zirconia balls having a diameter of 4 mm for 100 hours to obtain an additive solution for an intermediate film in which EuB 6 fine particles are dispersed. 100g
Was prepared (Solution J).

【００６２】Ｊ液、Ｃ液、ポリビニルブチラール、トリ
エチレングリコール−ジ−２−エチルブチレートを表１
の組成になるようにビニル系樹脂組成物を調製した。こ
れを実施例１と同様の方法で中間膜を作製して目的とす
る合わせガラスを作製した。この合わせガラスの光学特
性を表１に併せて示す。Table 1 shows solutions J, C, polyvinyl butyral, and triethylene glycol-di-2-ethyl butyrate.
A vinyl resin composition was prepared so as to have the following composition. This was used to produce an intermediate film in the same manner as in Example 1 to produce the intended laminated glass. Table 1 also shows the optical characteristics of the laminated glass.

【００６３】[0063]

【表１】 [Table 1]

【００６４】（実施例１８）平均重合度で４〜５量体で
あるエチルシリケート４０（多摩化学工業株式会社製：
商品名）を１０ｇ、エタノール２７ｇ、５％塩酸水溶液
８ｇ、水５ｇで調製したエチルシリケート溶液をよく混
合・撹拌してエチルシリケート混合液５０ｇを調製した
（Ｋ液）。Example 18 Ethyl silicate 40 having an average degree of polymerization of 4 to 5 mer (manufactured by Tama Chemical Industry Co., Ltd .:
(Trade name), ethanol 27 g, 5% hydrochloric acid aqueous solution 8 g, and water 5 g, an ethyl silicate solution was well mixed and stirred to prepare an ethyl silicate mixed solution 50 g (liquid K).

【００６５】Ａ液とＢ液とＫ液を混合し、さらにジアセ
トンアルコールで希釈して、ＩＴＯ濃度が７．２５重量
％、ＬａＢ６濃度が０．０４５重量％、ＳｉＯ２濃度が
２．５重量％となるように日射遮蔽膜用塗布液を作製し
た。この塗布液１５ｇをスピンコーターで厚さ２．５ｍ
ｍのフロートガラス上に塗布して１８０℃の電気炉に入
れて３０分間加熱し、前記フロートガラス上に日射遮蔽
膜を形成させた日射遮蔽ガラスを作製した。[0065] mixing the liquids A and B and K solution, and further diluted with diacetone alcohol, ITO concentration of 7.25 wt%, LaB 6 concentration of 0.045 wt%, SiO 2 concentration of 2.5 A coating solution for a solar shading film was prepared so as to have a weight%. 15 g of this coating solution was applied to a thickness of 2.5 m using a spin coater.
m, and placed in a 180 ° C. electric furnace and heated for 30 minutes to prepare a solar shading glass having a solar shading film formed on the float glass.

【００６６】この日射遮蔽ガラスと厚さ２．５ｍｍのフ
ロートガラスとを前記日射遮蔽膜が内側に面するように
して０．７６ｍｍの中間膜用ポリビニルブチラール膜で
挟み込んで通常の合わせガラス製造法にしたがって加熱
・圧着して合わせガラスを作製した。The solar shading glass and the float glass having a thickness of 2.5 mm were sandwiched between a 0.76 mm polyvinyl butyral film for an interlayer so that the solar shading film faced inward, and a normal laminated glass manufacturing method was performed. Therefore, a laminated glass was produced by heating and pressing.

【００６７】作製された合わせガラスの分光特性を実施
例１と同様にして測定し、日射透過率および可視光透過
率を算出し、表２に示す。また作製された合わせガラス
について実施例１同様のパンメル試験を実施してパンメ
ル値を測定した結果、パンメル値は５であり、板ガラス
と中間膜との密着性は十分であった。The spectral characteristics of the laminated glass thus produced were measured in the same manner as in Example 1, and the solar transmittance and visible light transmittance were calculated. In addition, the prepared laminated glass was subjected to the same Pummel test as in Example 1 and the Pummel value was measured. As a result, the Pummel value was 5, and the adhesion between the plate glass and the interlayer film was sufficient.

【００６８】（実施例１９〜２２）Ａ液とＢ液とＫ液を
混合し、さらにジアセトンアルコールで希釈して表２の
組成になるように日射遮蔽膜用塗布液を作製した。この
塗布液を用いて実施例１８と同様の方法で日射遮蔽ガラ
スを作製しこれを用いて目的とする合わせガラスを作製
した。この合わせガラスの光学特性を表２に併せて示
す。(Examples 19 to 22) The solution A, the solution B and the solution K were mixed and further diluted with diacetone alcohol to prepare a coating solution for a solar shading film so as to have the composition shown in Table 2. Using this coating liquid, a solar shading glass was produced in the same manner as in Example 18, and a target laminated glass was produced using this. Table 2 also shows the optical characteristics of the laminated glass.

【００６９】（実施例２３）Ａ液とＫ液を混合し、さら
にジアセトンアルコールで希釈して表２の組成になるよ
うに日射遮蔽膜用塗布液を作製した。この塗布液を用い
て実施例１８と同様の方法で日射遮蔽ガラスを作製しこ
れを用いて目的とする合わせガラスを作製した。この合
わせガラスの光学特性を表２に併せて示す。Example 23 A solution and a K solution were mixed, and further diluted with diacetone alcohol to prepare a coating solution for a solar shading film so as to have a composition shown in Table 2. Using this coating liquid, a solar shading glass was produced in the same manner as in Example 18, and a target laminated glass was produced using this. Table 2 also shows the optical characteristics of the laminated glass.

【００７０】（実施例２４）Ａ液とＢ液とＫ液を混合
し、さらにジアセトンアルコールで希釈して、ＩＴＯ濃
度が３．６３重量％、ＬａＢ６濃度が０．０２３重量
％、ＳｉＯ２濃度が１．２５重量％となるように日射遮
蔽膜用塗布液を作製した。この塗布液１５ｇをスピンコ
ーターで厚さ２．５ｍｍのフロートガラス上に塗布して
１８０℃の電気炉に入れて３０分間加熱し、前記フロー
トガラス上に日射遮蔽膜を形成させて日射遮蔽ガラスを
作製した。[0070] (Example 24) were mixed liquids A and B and K solution, and further diluted with diacetone alcohol, ITO concentration of 3.63 wt%, LaB 6 concentration of 0.023 wt%, SiO 2 A coating solution for a solar shading film was prepared so that the concentration was 1.25% by weight. 15 g of this coating solution was applied on a float glass having a thickness of 2.5 mm with a spin coater, placed in an electric furnace at 180 ° C., and heated for 30 minutes to form a solar shading film on the float glass to form a solar shading glass. Produced.

【００７１】一方Ａ液とＢ液にビニル系樹脂としてポリ
ビニルブチラール、可塑剤としてトリエチレングリコー
ル−ジ−２−エチルブチレートを混合し、ＩＴＯ濃度が
０．１８重量％、ＬａＢ６濃度が０．００２５重量％、
ポリビニルブチラール濃度が７０重量％となるようにビ
ニル系樹脂組成物を調製し、実施例１と同様の方法で成
形された中間膜を作製した。[0071] On the other hand polyvinyl butyral as vinyl resin liquids A and B, triethylene glycol as a plasticizer - mixed di-2-ethyl butyrate, ITO concentration of 0.18 wt%, LaB 6 concentration is zero. 0025% by weight,
A vinyl-based resin composition was prepared such that the polyvinyl butyral concentration was 70% by weight, and an intermediate film was formed in the same manner as in Example 1.

【００７２】そして前記日射遮蔽ガラスと厚さ２．５ｍ
ｍのフロートガラスとを前記日射遮蔽膜が内側に面する
ようにして前記中間膜を挟み込んで通常の合わせガラス
製造法にしたがって加熱・圧着して、合わせガラスを作
製した。この合わせガラスの光学特性を表２に併せて示
す。The solar shading glass and a thickness of 2.5 m
m of float glass was heated and pressed in accordance with a normal laminated glass manufacturing method by sandwiching the intermediate film with the solar shading film facing inward, to produce a laminated glass. Table 2 also shows the optical characteristics of the laminated glass.

【００７３】作製された合わせガラスについてパンメル
値を測定した結果、パンメル値は５であり、板ガラスと
中間膜との密着性は十分であった。The Pummel value of the produced laminated glass was measured. As a result, the Pummel value was 5, and the adhesion between the plate glass and the interlayer film was sufficient.

【００７４】（実施例２５）Ａ液とＫ液を混合し、さら
にジアセトンアルコールで希釈して、ＬａＢ６濃度が
０．２４重量％、ＳｉＯ２濃度が１．２５重量％となる
ように日射遮蔽膜用塗布液を作製した。この塗布液１５
ｇをスピンコーターで厚さ２．５ｍｍのフロートガラス
上に塗布し１８０℃の電気炉に入れて３０分間加熱し、
前記フロートガラス上に日射遮蔽膜を形成させ日射遮蔽
ガラスを作製した。[0074] (Example 25) were mixed liquid A and K solution, further diluted with diacetone alcohol, LaB 6 concentration of 0.24 wt%, the solar radiation as SiO 2 concentration of 1.25 wt% A coating solution for a shielding film was prepared. This coating liquid 15
g on a 2.5 mm thick float glass with a spin coater, and placed in a 180 ° C. electric furnace and heated for 30 minutes.
A solar shading film was formed on the float glass to produce a solar shading glass.

【００７５】一方Ａ液とＢ液にビニル系樹脂としてポリ
ビニルブチラール、可塑剤としてトリエチレングリコー
ル−ジ−２−エチルブチレートを混合し、ＩＴＯ濃度が
０．１９重量％、ＬａＢ６濃度が０．００２５重量％、
ポリビニルブチラール濃度が７０重量％となるようにビ
ニル系樹脂組成物を調製し、実施例１と同様の方法で成
形されたシート状中間膜を作製した。[0075] On the other hand polyvinyl butyral as vinyl resin liquids A and B, triethylene glycol as a plasticizer - mixed di-2-ethyl butyrate, ITO concentration of 0.19 wt%, LaB 6 concentration is zero. 0025% by weight,
A vinyl-based resin composition was prepared so that the polyvinyl butyral concentration was 70% by weight, and a sheet-like interlayer film formed in the same manner as in Example 1 was produced.

【００７６】そして前記日射遮蔽ガラスと厚さ２．５ｍ
ｍのフロートガラスとにより前記日射遮蔽膜が内側に面
するようにして前記中間膜を挟み込んで通常の合わせガ
ラス製造法にしたがって加熱・圧着して、合わせガラス
を作製した。この合わせガラスの光学特性を表２に併せ
て示す。The solar shading glass and a thickness of 2.5 m
Then, the intermediate film was sandwiched between the glass and the float glass of m in such a manner that the solar shading film faced inward, and heated and pressed in accordance with a normal laminated glass manufacturing method to produce a laminated glass. Table 2 also shows the optical characteristics of the laminated glass.

【００７７】[0077]

【表２】 [Table 2]

【００７８】以上の各実施例に示されるように、２枚の
板ガラスの間に合わせガラス用中間層が介在されている
合わせガラスにおいて、高コストの物理成膜法を用いず
に簡便な方法で６ホウ化物微粒子、所望に応じてＩＴＯ
微粒子および／またはＡＴＯ微粒子を含有する添加液を
ビニル系樹脂に添加して調製されるビニル系樹脂組成物
から形成される中間膜を用いるか、または前記添加液に
バインダーを添加してなる塗布液を板ガラスの内側に面
する面に塗布して日射遮蔽膜を形成し、ついで前記中間
膜または従来の中間膜を介在させることにより、日射遮
蔽機能を有し、かつ可視光域に高い透過性能を有する日
射遮蔽合わせガラスを製造することが可能となった。As shown in the above examples, in a laminated glass in which an interlayer for laminated glass is interposed between two sheet glasses, a simple method can be used without using an expensive physical film forming method. Boride fine particles, if desired ITO
A coating solution using an intermediate film formed from a vinyl-based resin composition prepared by adding an additive solution containing fine particles and / or ATO fine particles to a vinyl-based resin, or adding a binder to the additive solution Is applied to the surface facing the inside of the plate glass to form a solar shading film, and then by interposing the intermediate film or a conventional intermediate film, has a solar shading function, and has a high transmission performance in the visible light region. It has become possible to produce a solar-shielded laminated glass having the same.

【００７９】[0079]

【発明の効果】以上述べた通り本発明によれば、２枚の
板ガラスの間に中間層を介在させてなる日射遮蔽合わせ
ガラスにおいて、６ホウ化物微粒子、および所望に応じ
てＩＴＯ微粒子および／またはＡＴＯ微粒子を含有する
添加液をビニル系樹脂に添加して調製されるビニル系樹
脂組成物から形成される中間膜、または前記添加液をバ
インダーに添加してなる塗布液を板ガラスの内側に面す
る面に塗布して日射遮蔽膜を形成した後、前記中間膜あ
るいは従来の中間膜を介在させることによって、日射遮
蔽機能を有し、かつ可視光域に高い透過性能を有する日
射遮蔽合わせガラスを、高コストの物理成膜法を用いず
に簡便な方法で、極めて容易に製造することが可能とな
った。As described above, according to the present invention, in a solar-shielding laminated glass having an intermediate layer interposed between two sheet glasses, hexaboride fine particles and, if desired, ITO fine particles and / or An intermediate film formed from a vinyl-based resin composition prepared by adding an additive solution containing ATO fine particles to a vinyl-based resin, or a coating solution obtained by adding the additive solution to a binder faces the inside of the plate glass. After forming a solar shading film by applying to the surface, by interposing the interlayer or a conventional interlayer, having a solar shading function, and a solar shading laminated glass having a high transmission performance in the visible light region, It has become possible to manufacture the semiconductor device very easily by a simple method without using an expensive physical film forming method.

【図面の簡単な説明】[Brief description of the drawings]

【図１】比較例１および実施例１〜５におけるＩＴＯ微
粒子の濃度と光学特性の変化を示すグラフ図である。FIG. 1 is a graph showing changes in the concentration of ITO fine particles and optical characteristics in Comparative Example 1 and Examples 1 to 5.

【図２】比較例２および実施例７〜１０におけるＡＴＯ
微粒子の濃度と光学特性の変化を示すグラフ図である。FIG. 2 shows ATO in Comparative Example 2 and Examples 7 to 10.
FIG. 4 is a graph showing changes in the concentration of fine particles and optical characteristics.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 矢吹 佳世 千葉県市川市中国分３−18−５ 住友金属 鉱山株式会社中央研究所内 (72)発明者 武田 広充 千葉県市川市中国分３−18−５ 住友金属 鉱山株式会社中央研究所内 (72)発明者 足立 健治 千葉県市川市中国分３−18−５ 住友金属 鉱山株式会社中央研究所内 (72)発明者 室町 隆 大阪府大阪市中央区道修町３丁目５番11号 日本板硝子株式会社内 Ｆターム(参考） 4G061 AA09 AA20 BA01 BA02 CB05 CB12 CB19 CD02 CD18  ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Yoshiyo Yabuki 3-18-5, China, Ichikawa, Chiba Prefecture Sumitomo Metal Mining Co., Ltd. Central Research Laboratory (72) Inventor Hiromitsu Takeda 3-18, China, Ichikawa, Chiba −5 Sumitomo Metal Mining Co., Ltd. Central Research Laboratory (72) Inventor Kenji Adachi 3-18-5 China, Ichikawa City, Chiba Pref. Sumitomo Metal Mining Co., Ltd. Central Research Laboratory (72) Inventor Takashi Muromachi Michio Chuo-ku, Osaka City, Osaka 3-5-11, Nippon Sheet Glass Co., Ltd. F-term (reference) 4G061 AA09 AA20 BA01 BA02 CB05 CB12 CB19 CD02 CD18

Claims (7)

【特許請求の範囲】[Claims] 【請求項１】 日射遮蔽機能を有する中間層を２枚の板
ガラス間に介在せしめてなる日射遮蔽合わせガラスであ
って、前記中間層は、ＬａＢ６、ＣｅＢ６、ＰｒＢ６、
ＮｄＢ６、ＧｄＢ６、ＴｂＢ６、ＤｙＢ６、ＨｏＢ６、
ＹＢ６、ＳｍＢ６、ＥｕＢ６、ＥｒＢ６、ＴｍＢ６、Ｙ
ｂＢ６、ＬｕＢ６、（Ｌａ、Ｃｅ）Ｂ ６、ＳｒＢ６およ
びＣａＢ６からなる群から選択された少なくとも１種の
６ホウ化物微粒子を可塑剤に分散させた添加液と、ビニ
ル系樹脂とからなる中間膜により形成されることを特徴
とする日射遮蔽用合わせガラス。1. An intermediate layer having a solar shading function comprising two plates
A solar-shielded laminated glass that is interposed between glass
Thus, the intermediate layer is LaB6, CeB6, PrB6,
NdB6, GdB6, TbB6, DyB6, HoB6,
YB6, SmB6, EuB6, ErB6, TmB6, Y
bB6, LuB6, (La, Ce) B 6, SrB6And
And CaB6At least one member selected from the group consisting of
An additive liquid in which hexaboride fine particles are dispersed in a plasticizer;
It is characterized by being formed by an intermediate film consisting of
Laminated glass for solar shading. 【請求項２】 日射遮蔽機能を有する中間層を２枚の板
ガラス間に介在せしめてなる日射遮蔽合わせガラスであ
って、前記中間層は、ＬａＢ６、ＣｅＢ６、ＰｒＢ６、
ＮｄＢ６、ＧｄＢ６、ＴｂＢ６、ＤｙＢ６、ＨｏＢ６、
ＹＢ６、ＳｍＢ６、ＥｕＢ６、ＥｒＢ６、ＴｍＢ６、Ｙ
ｂＢ６、ＬｕＢ６、（Ｌａ、Ｃｅ）Ｂ ６、ＳｒＢ６およ
びＣａＢ６からなる群から選択された少なくとも１種の
６ホウ化物微粒子、ならびにＩＴＯ微粒子および／また
はＡＴＯ微粒子とを可塑剤に分散させた添加液と、ビニ
ル系樹脂とからなる中間膜により形成されることを特徴
とする日射遮蔽用合わせガラス。2. An intermediate layer having a solar shading function comprising two plates
A solar-shielded laminated glass that is interposed between glass
Thus, the intermediate layer is LaB6, CeB6, PrB6,
NdB6, GdB6, TbB6, DyB6, HoB6,
YB6, SmB6, EuB6, ErB6, TmB6, Y
bB6, LuB6, (La, Ce) B 6, SrB6And
And CaB6At least one member selected from the group consisting of
Hexaboride fine particles, and ITO fine particles and / or
Is an additive liquid in which ATO fine particles are dispersed in a plasticizer;
It is characterized by being formed by an intermediate film consisting of
Laminated glass for solar shading. 【請求項３】 前記６ホウ化物微粒子と、前記ＩＴＯ微
粒子および／またはＡＴＯ微粒子との重量比を０．１：
９９．９〜９０：１０の範囲とすることを特徴とする請
求項２記載の日射遮蔽用合わせガラス。3. The weight ratio of said hexaboride fine particles to said ITO fine particles and / or ATO fine particles is 0.1:
3. The laminated glass for solar shading according to claim 2, wherein the range is 99.9 to 90:10. 【請求項４】 前記可塑剤が、トリエチレングリコール
−ジ−２−エチルブチレートであることを特徴とする請
求項１〜３のいずれか１項記載の日射遮蔽用合わせガラ
ス。4. The laminated glass for solar shading according to claim 1, wherein the plasticizer is triethylene glycol-di-2-ethyl butyrate. 【請求項５】 日射遮蔽機能を有する中間層を２枚の板
ガラス間に介在せしめてなる日射遮蔽合わせガラスであ
って、前記中間層は、少なくとも一方の板ガラスの内側
に位置する面に形成され、かつＬａＢ６、ＣｅＢ６、Ｐ
ｒＢ６、ＮｄＢ６、ＧｄＢ６、ＴｂＢ６、ＤｙＢ６、Ｈ
ｏＢ６、ＹＢ６、ＳｍＢ６、ＥｕＢ６、ＥｒＢ６、Ｔｍ
Ｂ６、ＹｂＢ６、ＬｕＢ６、（Ｌａ、Ｃｅ）Ｂ６、Ｓｒ
Ｂ６およびＣａＢ６からなる群から選択された少なくと
も１種の６ホウ化物微粒子を日射遮蔽成分として含有す
る塗布液を塗布して形成された日射遮蔽膜と、前記２枚
の板ガラス間に介在されるビニル系樹脂を含有する中間
膜により形成されることを特徴とする日射遮蔽用合わせ
ガラス。5. A solar-shielded laminated glass in which an intermediate layer having a solar-shielding function is interposed between two glass sheets, wherein the intermediate layer is formed on a surface located inside at least one of the glass sheets, And LaB 6 , CeB 6 , P
rB 6 , NdB 6 , GdB 6 , TbB 6 , DyB 6 , H
oB 6 , YB 6 , SmB 6 , EuB 6 , ErB 6 , Tm
B 6 , YbB 6 , LuB 6 , (La, Ce) B 6 , Sr
A solar shading film formed by applying a coating solution containing at least one type of hexaboride fine particles selected from the group consisting of B 6 and CaB 6 as a solar shading component, and interposed between the two sheet glasses; A laminated glass for shielding sunlight, characterized by being formed of an interlayer containing a vinyl resin. 【請求項６】 日射遮蔽機能を有する中間層を２枚の板
ガラス間に介在せしめてなる日射遮蔽合わせガラスであ
って、前記中間層は、少なくとも一方の板ガラスの内側
に位置する面に形成され、かつＬａＢ６、ＣｅＢ６、Ｐ
ｒＢ６、ＮｄＢ６、ＧｄＢ６、ＴｂＢ６、ＤｙＢ６、Ｈ
ｏＢ６、ＹＢ６、ＳｍＢ６、ＥｕＢ６、ＥｒＢ６、Ｔｍ
Ｂ６、ＹｂＢ６、ＬｕＢ６、（Ｌａ、Ｃｅ）Ｂ６、Ｓｒ
Ｂ６およびＣａＢ６からなる群から選択された少なくと
も１種の６ホウ化物微粒子と、ＩＴＯ微粒子およびＡＴ
Ｏ微粒子のうち１種以上とを日射遮蔽成分として含有す
る塗布液を塗布して形成された日射遮蔽膜と、前記２枚
の板ガラス間に介在されるビニル系樹脂を含有する中間
膜により形成されることを特徴とする日射遮蔽用合わせ
ガラス。6. A solar-shielded laminated glass in which an intermediate layer having a solar-shielding function is interposed between two glass sheets, wherein the intermediate layer is formed on a surface located inside at least one of the glass sheets, And LaB 6 , CeB 6 , P
rB 6 , NdB 6 , GdB 6 , TbB 6 , DyB 6 , H
oB 6 , YB 6 , SmB 6 , EuB 6 , ErB 6 , Tm
B 6 , YbB 6 , LuB 6 , (La, Ce) B 6 , Sr
At least one type of hexaboride fine particles selected from the group consisting of B 6 and CaB 6 , ITO fine particles and AT
A solar-shielding film formed by applying a coating solution containing at least one of the O fine particles as a solar-shielding component, and an intermediate film containing a vinyl-based resin interposed between the two glass sheets; A laminated glass for shielding sunlight. 【請求項７】 前記中間膜が日射遮蔽機能を有すること
を特徴とする請求項５または６記載の日射遮蔽用合わせ
ガラス。7. The laminated glass for solar shading according to claim 5, wherein the intermediate film has a solar shading function.
JP22128099A 1999-05-17 1999-08-04 Sunlight shielding laminated glass Pending JP2001089202A (en)

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JP11-135989 1999-05-17
JP13598999 1999-05-17
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