JP2007197237A - Low-radiation double glazing - Google Patents
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本発明は、熱線遮蔽積層膜を有する低放射（Ｌｏｗ Ｅｍｉｓｓｉｏｎ，Ｌｏｗ−Ｅ）複層ガラスに関する。 The present invention relates to a low emission (Low Emission, Low-E) multilayer glass having a heat ray shielding laminated film.
熱線遮蔽積層体（以下Ｌｏｗ−Ｅ膜とも称する）は、熱線（赤外光）を反射する機能を有することから、夏季の冷房負荷や冬期の暖房負荷の緩和を目的として、住宅やビルなどの建築用ガラスの表面に形成されてきた。 The heat ray shielding laminate (hereinafter also referred to as “Low-E film”) has a function of reflecting heat rays (infrared light). Therefore, for the purpose of alleviating the cooling load in summer and the heating load in winter, It has been formed on the surface of architectural glass.
Ｌｏｗ−Ｅ膜は、ガラス等の基体上に酸化亜鉛（ＺｎＯ）膜／銀（Ａｇ）等を主成分とする貴金属膜／酸化亜鉛膜をこの順に積層した膜構成を有する積層体である。このうち、銀等を主成分とする貴金属膜は耐湿性、耐酸性などの化学耐久性が劣悪であり、酸化亜鉛膜被覆によっても十分な改善がなされないという問題があった。そこで、貴金属膜と外気を遮断するため、積層膜は複層ガラスの内側、すなわち、二枚のガラスによって形成される間隙側に配置されていた。しかし、この手段では単板の取り扱い時の耐久性や保存期間中の耐久性については解決されず、依然として問題は残されている。 The Low-E film is a laminate having a film configuration in which a zinc oxide (ZnO) film / a noble metal film mainly composed of silver (Ag) / zinc oxide film is laminated in this order on a substrate such as glass. Among these, noble metal films mainly composed of silver or the like have poor chemical durability such as moisture resistance and acid resistance, and there is a problem that sufficient improvement cannot be achieved even by coating with a zinc oxide film. Therefore, in order to shut off the noble metal film and the outside air, the laminated film is disposed inside the multilayer glass, that is, on the gap side formed by two sheets of glass. However, this means does not solve the durability at the time of handling the veneer and the durability during the storage period, and problems still remain.
上記問題を解決するため、たとえば特許文献１では、銀層の直下層に酸化亜鉛層を、銀層の直上層には亜鉛または亜鉛を主成分とした保護金属層がそれぞれ成膜されたものが開示されている。
しかしながら、Ｌｏｗ−Ｅ膜には、その他の問題点も存在している。即ち、前記したようにＬｏｗ−Ｅ膜は通常複層ガラスの状態で用いられているが、Ｌｏｗ−Ｅ膜を使用しない複層ガラスと比較して反射率が高い。したがって複層ガラスに特有の反射像が二重となる現象が、Ｌｏｗ−Ｅ膜を使用しない複層ガラスと比較してより強く現れ、これが利用者に不快感を与えている。 However, there are other problems with the Low-E film. That is, as described above, the Low-E film is usually used in the state of a double-glazed glass, but has a higher reflectance than the double-glazed glass not using the Low-E film. Therefore, the phenomenon that the reflection image peculiar to the multilayer glass is double appears more strongly than the multilayer glass not using the Low-E film, which gives the user unpleasant feeling.
二重反射像がより強く現れる原因は、Ｌｏｗ−Ｅ膜が反射率の高い銀膜を有するためである。銀膜が厚くなると反射率が高くなり、さらに、反射色が赤みを帯びるようになる。このように、遮熱性能をより高くするためには銀膜を厚くしなければならず、厚くすると二重反射像がより強く現れるという矛盾がある。この矛盾は前記特許文献１では解決されていない。 The reason why the double reflection image appears stronger is that the Low-E film has a silver film having a high reflectance. The thicker the silver film, the higher the reflectance, and the reflected color becomes reddish. Thus, there is a contradiction that the silver film has to be thickened in order to further improve the heat shielding performance, and that a double reflection image appears stronger when the silver film is thickened. This contradiction is not solved in Patent Document 1.
上記課題を解決するため本発明は、二枚のガラス板を対向配置した複層ガラスであって、前記二枚のガラス板のうち一方のガラス板の他方のガラス板に対向する表面には、第一の酸化物膜／Ａｇ膜／金属膜／第二の酸化物膜をこの順に積層した熱線遮蔽積層体が形成され、前記第一の酸化物膜の膜厚は３０ｎｍ以上４０ｎｍ以下、前記第二の酸化物膜の膜厚は３０ｎｍ以上５０ｎｍ以下、前記Ａｇ膜の厚さは８ｎｍ以上１０以下、前記金属膜の厚さは１ｎｍ以上８ｎｍ以下であり、且つ前記第一の酸化物膜と第二の酸化物膜の膜厚比は０．９以上１．７以下である構成とした。 In order to solve the above-mentioned problem, the present invention is a multi-layer glass in which two glass plates are arranged to face each other, and on the surface facing the other glass plate of one of the two glass plates, A heat ray shielding laminate is formed by laminating the first oxide film / Ag film / metal film / second oxide film in this order, and the thickness of the first oxide film is 30 nm to 40 nm. The second oxide film has a thickness of 30 nm to 50 nm, the Ag film has a thickness of 8 nm to 10 nm, the metal film has a thickness of 1 nm to 8 nm, and the first oxide film and the second oxide film The thickness ratio of the second oxide film is 0.9 or more and 1.7 or less.
第一の酸化物膜と第二の酸化物膜の膜厚比を上記のようにほぼ等しいかまたは第一の酸化物膜厚を１とした際の第二の酸化物膜厚が１．７倍以下の厚みとすることで、外観だけでなく内観においても視感度の最も大きい波長５５０ｎｍ付近の反射率を低減でき、反射色を中性にすることができる。 The film thickness ratio of the first oxide film and the second oxide film is substantially equal as described above, or the second oxide film thickness is 1.7 when the first oxide film thickness is 1. By setting the thickness to be twice or less, the reflectance in the vicinity of the wavelength of 550 nm having the highest visibility can be reduced not only in the appearance but also in the interior, and the reflected color can be neutralized.
また、本発明に係る複層ガラスは、室内外境界に設置したときの室外側において、ＪＩＳＲ３１０６で規定する可視光反射率が８％以上２５％以下であり、Ｌ＊ａ＊ｂ＊表色系におけるａ＊が−３．０以上０．０以下、ｂ＊が−９．０以上０．０以下（ほぼ中性色の反射色調）で、且つ遮蔽係数が０．５７以下とすることができる。 Further, the multilayer glass according to the present invention has a visible light reflectance of 8% or more and 25% or less as defined in JIS R3106 at the outdoor side when installed at the indoor / outdoor boundary, and the L * a * b * color system A * in the range from -3.0 to 0.0, b * in the range from -9.0 to 0.0 (substantially neutral reflection color tone), and a shielding coefficient of 0.57 or less. .
また、本発明に係る複層ガラスは、室内外境界に設置したときの室外側において、ＪＩＳＲ３１０６で規定する可視光反射率が８％以上１５％以下であり、Ｌ＊ａ＊ｂ＊表色系におけるａ＊が−１．０以上５．０以下、ｂ＊が−２０．０以上０．０以下とすることができる。また、ＪＩＳ Ｒ３１０６で規定する可視光透過率が５０％以上７５％以下であることも望ましい。 Further, the multilayer glass according to the present invention has a visible light reflectance defined by JIS R3106 of 8% or more and 15% or less on the outdoor side when installed at the indoor / outdoor boundary, and L * a * b * color system A * can be -1.0 or more and 5.0 or less, and b * can be -20.0 or more and 0.0 or less. It is also desirable that the visible light transmittance specified by JIS R3106 be 50% or more and 75% or less.
また、前記第一および第二の酸化物膜が、酸化錫膜とＡｌドープ酸化亜鉛膜との積層体であって、Ａｌドープ酸化亜鉛膜が前記Ａｇ膜側に配置され、かつ、酸化物膜の全膜厚に対するＡｌドープ酸化亜鉛膜厚の比率が１０％より大きく４０％以下であることが好ましい。 The first and second oxide films are a laminate of a tin oxide film and an Al-doped zinc oxide film, the Al-doped zinc oxide film is disposed on the Ag film side, and the oxide film The ratio of the Al-doped zinc oxide film thickness to the total film thickness is preferably greater than 10% and 40% or less.
前記Ａｌドープ酸化亜鉛膜のＡｌ含有量は、Ｚｎに対する原子比で１０％より大きく２５％以下であることが好ましく、前記金属膜はＴｉ膜、または、Ａｌ含有量がＺｎに対する原子比で１％以上２５％以下であるＺｎＡｌ合金膜であることも好ましい。 The Al content of the Al-doped zinc oxide film is preferably greater than 10% and not more than 25% in terms of atomic ratio to Zn, and the metal film is Ti film or Al content is 1% in terms of atomic ratio to Zn. A ZnAl alloy film of 25% or less is also preferable.
本発明によれば、Ｌｏｗ−Ｅ膜として、第一の酸化物膜と第二の酸化物膜との間に、薄いＡｇ膜と少し厚めの金属膜を配置したことにより、可視光反射率を低減し、ぎらつきを抑え、好ましい中間色の複層ガラスとすることができる。しかも、熱遮蔽機能も十分に保持することができる。 According to the present invention, as a Low-E film, a thin Ag film and a slightly thicker metal film are disposed between the first oxide film and the second oxide film, so that the visible light reflectance is increased. It is possible to reduce the glare and suppress the glare and to obtain a preferable intermediate color multilayer glass. Moreover, the heat shielding function can be sufficiently retained.
Ｌｏｗ−Ｅ膜の耐久性はＡｇ膜上層の誘電体の膜応力と関係しており、Ａｌを酸化亜鉛膜中に多くドープすることで、膜応力を低減でき、耐久性が向上する。また膜作製時の放電安定性も一層向上できるが、ドープ量が過多であると生産時に材料が酸化アルミニウムにより被膜されることで成膜速度が遅くなる。よって生産と品質のバランスから、前記Ａｌドープ酸化亜鉛膜のさらに好ましいＡｌ含有量は、Ｚｎに対する原子比で１０％より大きく１５％以下である。 The durability of the Low-E film is related to the film stress of the upper dielectric layer of the Ag film. By doping a large amount of Al in the zinc oxide film, the film stress can be reduced and the durability can be improved. Moreover, although the discharge stability at the time of film production can be further improved, if the amount of dope is excessive, the material is coated with aluminum oxide at the time of production, so that the film formation rate becomes slow. Therefore, from the balance between production and quality, the more preferable Al content of the Al-doped zinc oxide film is more than 10% and not more than 15% in terms of atomic ratio to Zn.
また前記Ａｌドープ酸化亜鉛膜中のＡｌ含有量とＬｏｗ−Ｅ膜の紫外線透過率が比例であり、屈折率と反比例している。Ａｌ含有量が多い場合、屈折率が小さくＬｏｗ−Ｅ膜の反射率を低減できるが、紫外線透過率が増加する。よって紫外線透過率と膜屈折率のバランスに関しても前記Ａｌドープ酸化亜鉛膜のさらに好ましいＡｌ含有量は、Ｚｎに対する原子比で１０％より大きく１５％以下である。 Further, the Al content in the Al-doped zinc oxide film and the ultraviolet transmittance of the Low-E film are proportional and inversely proportional to the refractive index. When the Al content is high, the refractive index is small and the reflectance of the Low-E film can be reduced, but the ultraviolet transmittance increases. Therefore, with respect to the balance between the ultraviolet transmittance and the film refractive index, the more preferable Al content of the Al-doped zinc oxide film is more than 10% and not more than 15% in terms of atomic ratio to Zn.
以下に本発明の好適な実施例を添付図面に基づいて説明する。図１は本発明に係る複層ガラスの断面図であり、複層ガラス１は、対向する一方のガラス板２の表面に、第一の酸化物膜３、Ａｇ膜４、金属膜５および第二の酸化物膜６をこの順に積層し、間隙７を介して二枚組合せたものである。 Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. FIG. 1 is a cross-sectional view of a multi-layer glass according to the present invention. The multi-layer glass 1 has a first oxide film 3, an Ag film 4, a metal film 5 and a first film on the surface of one opposing glass plate 2. Two oxide films 6 are laminated in this order, and two are combined through a gap 7.
これらガラス板２は、通常の窓ガラス等に使用する強化ガラスや平板ガラスを使用することができ、その厚さにも制限はないが、例えば４ｍｍ、６ｍｍ、８ｍｍのものを使用することができる。 These glass plates 2 can use tempered glass or flat glass used for ordinary window glass and the like, and the thickness thereof is not limited. For example, glass plates of 4 mm, 6 mm, and 8 mm can be used. .
ガラス板２の上に形成する第一の酸化物膜３、および、最外層として形成する第二の酸化物膜６の材料としては、酸化錫膜、酸化亜鉛膜等を使用することができるが、酸化錫膜／Ａｌドープ酸化亜鉛膜の積層体を採用し更に酸化錫膜を最下層及び最上層に形成することで、酸化錫膜の緻密性より、耐湿性、化学耐久性の点で好ましく、さらには、Ａｌドープ酸化亜鉛膜がＡｇ膜４側に配置され、かつ、酸化物膜の全膜厚に対するＡｌドープ酸化亜鉛膜厚の比率を１０以上４０％以下とすることが、Ａｇの結晶性を低減させず、酸化錫膜による耐久性向上を維持することができる点で好ましい。また、Ａｌドープ酸化亜鉛膜のＡｌ含有量は、Ｚｎに対する原子比で１０％より大きく２５％以下とすることが、酸化亜鉛膜の光学特性を維持しながら、耐久性が悪くなる原因である膜の応力を効果的に低減できる点で望ましい。 As materials for the first oxide film 3 formed on the glass plate 2 and the second oxide film 6 formed as the outermost layer, a tin oxide film, a zinc oxide film, or the like can be used. By adopting a laminated body of tin oxide film / Al-doped zinc oxide film and further forming a tin oxide film in the lowermost layer and the uppermost layer, it is preferable in terms of moisture resistance and chemical durability from the denseness of the tin oxide film Furthermore, it is possible that the Al-doped zinc oxide film is disposed on the Ag film 4 side and the ratio of the Al-doped zinc oxide film thickness to the total film thickness of the oxide film is 10% to 40%. This is preferable because the durability can be maintained by the tin oxide film without reducing the properties. The Al content of the Al-doped zinc oxide film is a film whose durability is deteriorated while maintaining the optical characteristics of the zinc oxide film when the atomic ratio to Zn is more than 10% and 25% or less. This is desirable because it can effectively reduce the stress.
第一の酸化物膜３および第二の酸化物膜６の厚さはそれぞれ３０ｎｍ以上４０ｎｍ以下、３０ｎｍ以上５０ｎｍ以下とすることが、低反射・中性色という点で好ましい。また、第一の酸化物膜３の厚みを１としたとき、第二の酸化物膜６の厚みは０．９から１．７の範囲に設定することが好ましい。このような膜厚比にすることで外気側からの視感度だけでなく、室内側から見た際の好感度を阻害する５５０ｎｍ付近の波長を有する可視光線の反射率をより効率的に低減し、反射色調を中性色にすることができる。同時に、ＪＩＳ Ｒ３１０６に規定する可視光透過率を高くする効果も期待できる。なお、本発明において中性色とは、色相、彩度および明度がほぼ中間的、すなわち、中間的な明るさ、濁度のグレーをいう。 The thicknesses of the first oxide film 3 and the second oxide film 6 are preferably 30 nm or more and 40 nm or less and 30 nm or more and 50 nm or less, respectively, from the viewpoint of low reflection and neutral color. When the thickness of the first oxide film 3 is 1, the thickness of the second oxide film 6 is preferably set in the range of 0.9 to 1.7. By using such a film thickness ratio, not only the visibility from the outside air side, but also the reflectance of visible light having a wavelength near 550 nm that hinders the favorable sensitivity when viewed from the indoor side is more efficiently reduced. The reflection color tone can be neutral. At the same time, the effect of increasing the visible light transmittance defined in JIS R3106 can be expected. In the present invention, the neutral color means gray having a hue, saturation and lightness that are substantially intermediate, that is, intermediate brightness and turbidity.
本発明に係るＡｇ膜４の厚さは８ｎｍ以上１０ｎｍ以下であり、従来のＬｏｗ−Ｅ膜に使用するＡｇ膜よりも薄くしてある。Ａｇ膜４をこの範囲に設計することで、赤みのある好ましくない光の反射率を低く抑えながら赤外光は反射させることができる。 The thickness of the Ag film 4 according to the present invention is 8 nm or more and 10 nm or less, and is thinner than the Ag film used for the conventional Low-E film. By designing the Ag film 4 in this range, it is possible to reflect infrared light while suppressing the reflectance of undesirable red light.
金属膜５としては、各種金属膜を使用することができるが、特に、Ｔｉ膜、または、Ａｌ含有量がＺｎに対する原子比で１％以上２５％以下であるＺｎＡｌ合金膜を使用することが好ましい。また、ＺｎＡｌ合金膜の組成をＡｌ含有量がＺｎに対する原子比で１％以上６％以下とすると、Ｌｏｗ−Ｅ膜の紫外線透過率を低減できるため、さらに好ましい。金属膜５の酸化されずに金属として膜構成中に存在する部分の厚みは１ｎｍ以上８ｎｍ以下であり、従来のＬｏｗ−Ｅ膜に使用する金属膜よりも厚くなるようにしている。金属膜５をこの範囲の厚さで配置すれば、十分に日射吸収を行うことができるため、反射率を上げずに遮熱性能を向上し、遮熱係数を０．５７以下とすることができる。 Various metal films can be used as the metal film 5, and it is particularly preferable to use a Ti film or a ZnAl alloy film having an Al content of 1% or more and 25% or less in terms of atomic ratio to Zn. . Further, it is more preferable that the composition of the ZnAl alloy film is such that the Al content is 1% or more and 6% or less in terms of atomic ratio to Zn, because the ultraviolet transmittance of the Low-E film can be reduced. The thickness of the portion of the metal film 5 that is not oxidized and exists in the film structure as a metal is 1 nm or more and 8 nm or less, and is thicker than the metal film used for the conventional Low-E film. If the metal film 5 is arranged in a thickness within this range, it is possible to sufficiently absorb solar radiation, so that the heat shielding performance can be improved without increasing the reflectance, and the heat shielding coefficient can be 0.57 or less. it can.
本発明の複層ガラス１を図１の要領で室内外境界に設置したとき、室外側面におけるＪＩＳ Ｒ３１０６に規定の可視光反射率を８％以上２５％以下の範囲に収めることができる。また、Ｌ＊ａ＊ｂ＊表色系におけるａ＊を−３．０以上０．０以下、ｂ＊を−９．０以上０．０以下の範囲とすることが可能となり、ほぼ中性色の反射色調を呈するようにできる。 When the double-glazed glass 1 of the present invention is installed at the indoor / outdoor boundary in the manner shown in FIG. 1, the visible light reflectance prescribed in JIS R3106 on the outdoor side surface can fall within the range of 8% to 25%. Further, L * a * b * -3.0 or more a * in the colorimetric system 0.0 or less, b * and it is possible to -9.0 or 0.0 or less in the range of about neutral color The reflection color tone can be exhibited.
また、室内側面においても、可視光反射率を８％以上１５％以下の範囲に収めることができ、またＬ＊ａ＊ｂ＊表色系におけるａ＊を−１．０以上〜５．０以下、ｂ＊を−２０．０以上−８．０以下の範囲とすることが可能となる。さらに、本発明のＬｏｗ−Ｅ複層ガラスの構成をとれば、ＪＩＳ Ｒ３１０６に規定の可視光透過率を５０％以上７５％以下の範囲とすることができ、高い可視光透過率を確保することができる。 Further, even in the indoor side, can fit visible light reflectance in the range of 15% or less than 8%, also L * a * b * -1.0 or more a * in the color system to 5.0 or less , B * can be in the range of −20.0 or more and −8.0 or less. Furthermore, if the composition of the Low-E double glazing of the present invention is adopted, the visible light transmittance prescribed in JIS R3106 can be in the range of 50% to 75%, and high visible light transmittance can be secured. Can do.
以下に具体的な実施例（図２）および比較例にもとづいて本発明を詳細に説明する。 Hereinafter, the present invention will be described in detail based on specific examples (FIG. 2) and comparative examples.
寸法３００ｍｍ×３００ｍｍ、厚さ６ｍｍのソーダライムガラスを洗浄、乾燥してガラス基体として用いた。前記ガラス基体をスパッタリング成膜装置内に設置し、真空度が５×１０−４Ｐａ以下になるまで排気を行い、以下のようにしてガラス基体表面に熱線反射積層体を成膜した。 Soda lime glass having a size of 300 mm × 300 mm and a thickness of 6 mm was washed and dried to be used as a glass substrate. The glass substrate was placed in a sputtering film forming apparatus and evacuated until the degree of vacuum was 5 × 10 −4 Pa or less, and a heat ray reflective laminate was formed on the glass substrate surface as follows.
（第１層の成膜）
装置内に酸素ガスを導入し、真空度を０．２６Ｐａ以上０．８Ｐａ以下に調整した後、錫ターゲットが備えられたカソードに直流電源より電力を供給してグロー放電を生じさせ、酸素とＳｎを反応させて酸化錫膜を作製できるようにし、電力を０．９ｋＷに調節した。その後、カソード上方を１０．３×１０−３ｍ／ｓの速度でガラス基体を搬送し、膜厚３２．２ｎｍの酸化錫膜を作製した。
(Deposition of the first layer)
After introducing oxygen gas into the apparatus and adjusting the degree of vacuum to 0.26 Pa or more and 0.8 Pa or less, power is supplied from a DC power source to the cathode provided with the tin target to cause glow discharge, and oxygen and Sn Was allowed to react to prepare a tin oxide film, and the power was adjusted to 0.9 kW. Thereafter, the glass substrate was conveyed above the cathode at a speed of 10.3 × 10 −3 m / s to produce a tin oxide film having a thickness of 32.2 nm.
（第２層の成膜）
次に装置内に酸素ガスを導入し、真空度を０．２６Ｐａ以上０．８Ｐａ以下に調整した後、Ｚｎに対する原子比でＡｌが１３．１％（Ｚｎとの合計量に対する原子比でＡｌが１１．６％）ドープされた亜鉛ターゲットが備えられたカソードに直流電源より電力を供給してグロー放電を生じさせ、酸素と亜鉛を反応させて酸化亜鉛膜を作製できるようにし、電力を１ｋＷに調節した。その後、カソード上方を１０．４×１０−３ｍ／ｓの速度でガラス基体を搬送し、第２層として膜厚４．５ｎｍの、Ｚｎに対する原子比でＡｌが１３．１％ドープされた酸化亜鉛膜を作製した。
(Second layer deposition)
Next, after introducing oxygen gas into the apparatus and adjusting the degree of vacuum to 0.26 Pa or more and 0.8 Pa or less, Al was 13.1% in terms of atomic ratio to Zn (Al in terms of atomic ratio relative to the total amount with Zn). 11.6%) A cathode equipped with a doped zinc target is supplied with electric power from a DC power source to generate glow discharge, allowing oxygen and zinc to react to produce a zinc oxide film, and the electric power to 1 kW Adjusted. Thereafter, the glass substrate is transported at a speed of 10.4 × 10 −3 m / s above the cathode, and the second layer is an oxide having a film thickness of 4.5 nm and doped with Al at an atomic ratio to Zn of 13.1%. A zinc film was prepared.
（第３層の成膜）
次に装置内にアルゴンガスを導入し、真空度を０．２６Ｐａ以上０．８Ｐａ以下に調整した後、銀ターゲットが備えられたカソードに直流電源より電力を供給してグロー放電を生じさせ、電力を０．２５ｋＷに調節した。その後、カソード上方を１６．５×１０−３ｍ／ｓの速度でガラス基体を搬送させ、第３層として膜厚９．６ｎｍの銀膜を作製した。
(Deposition of the third layer)
Next, after introducing argon gas into the apparatus and adjusting the degree of vacuum to 0.26 Pa or more and 0.8 Pa or less, power is supplied from a DC power source to the cathode equipped with the silver target to cause glow discharge, Was adjusted to 0.25 kW. Thereafter, the glass substrate was transported at a speed of 16.5 × 10 −3 m / s above the cathode, and a 9.6 nm-thick silver film was produced as the third layer.
（第４層の成膜）
次に装置内にアルゴンガスを導入し、真空度を０．２６Ｐａ以上０．８Ｐａ以下に調整した後、Ｚｎに対する原子比でＡｌが３．５％（Ｚｎとの合計量に対する原子比でＡｌが３．４％）ドープされた亜鉛ターゲットが備えられたカソードに直流電源より電力を供給してグロー放電を生じさせ、電力を０．２ｋＷに調節した。その後、カソード上方を２１．１×１０−３ｍ／ｓの速度でガラス基体を搬送させ、膜厚約５ｎｍの、Ｚｎに対する原子比でＡｌが３．５％ドープされた亜鉛アルミ膜を作製した。
(Fourth layer deposition)
Next, after introducing argon gas into the apparatus and adjusting the degree of vacuum to 0.26 Pa or more and 0.8 Pa or less, Al is 3.5% by atomic ratio to Zn (Al is atomic ratio to the total amount with Zn). 3.4%) The cathode provided with the doped zinc target was supplied with power from a DC power source to cause glow discharge, and the power was adjusted to 0.2 kW. Thereafter, the glass substrate was transported at a speed of 21.1 × 10 −3 m / s above the cathode to produce a zinc aluminum film having a film thickness of about 5 nm and doped with 3.5% Al at an atomic ratio to Zn. .
（第５層の成膜）
次に装置内に酸素ガスを導入し、真空度を０．２６Ｐａ以上０．８Ｐａ以下に調整した後、Ｚｎとの合計量に対し原子比でＡｌが１１．６％ドープされた亜鉛ターゲットが備えられたカソードに直流電源より電力を供給してグロー放電を生じさせ、酸素とＺｎを反応させて酸化亜鉛膜を作製できるようにし、電力を１ｋＷに調節した。その後、カソード上方を６．７×１０−３ｍ／ｓの速度でガラス基体を搬送させ、膜厚１０ｎｍの、Ｚｎに対する原子比でＡｌが１３．１％（Ｚｎとの合計量に対する原子比でＡｌが１１．６％）ドープされた酸化亜鉛膜を作製した。
Ｚｎに対する原子比でＡｌが１３．１％ドープされた酸化亜鉛膜の作製時における第四層金属膜の亜鉛アルミ膜が酸化された膜厚は約３〜５ｎｍであった。
(Fifth layer deposition)
Next, after introducing oxygen gas into the apparatus and adjusting the degree of vacuum to 0.26 Pa or more and 0.8 Pa or less, a zinc target doped with 11.6% of Al by atomic ratio with respect to the total amount with Zn is provided. Electric power was supplied to the cathode from a DC power source to cause glow discharge, and oxygen and Zn were allowed to react to produce a zinc oxide film, and the power was adjusted to 1 kW. Thereafter, the glass substrate was transported at a speed of 6.7 × 10 −3 m / s above the cathode, and Al was 13.1% in atomic ratio with respect to Zn having a film thickness of 10 nm (atomic ratio with respect to the total amount with Zn). A zinc oxide film doped with 11.6% Al was prepared.
When the zinc oxide film doped with 13.1% Al by atomic ratio to Zn was produced, the film thickness of the oxidized fourth layer metal film of zinc aluminum film was about 3 to 5 nm.
（第６層の成膜）
次に装置内に酸素ガスを導入し、真空度を０．２６Ｐａ以上０．８Ｐａ以下に調整した後、錫ターゲットが備えられたカソードに直流電源より電力を供給してグロー放電を生じさせ、酸素と錫を反応させて酸化錫膜を作製できるようにし、電力を１ｋＷに調節した。その後、カソード上方を８．５×１０−３ｍ／ｓの速度でガラス基体を搬送させ、膜厚２４．５ｎｍの酸化錫膜を作製した。
(Film formation of the sixth layer)
Next, after introducing oxygen gas into the apparatus and adjusting the degree of vacuum to 0.26 Pa or more and 0.8 Pa or less, power is supplied from a DC power source to a cathode equipped with a tin target to cause glow discharge, And tin were allowed to react to produce a tin oxide film, and the power was adjusted to 1 kW. Thereafter, the glass substrate was transported at a speed of 8.5 × 10 −3 m / s above the cathode to produce a tin oxide film having a thickness of 24.5 nm.
形成した熱線反射積層体の膜構成を表１に示す。本実施例において、第１層の酸化錫（ＳｎＯ２）と第２層のＡｌドープ酸化亜鉛層を組み合わせたものが前記第一の酸化物膜に相当し、第５層のＡｌドープ酸化亜鉛層と第６層の酸化錫層を組み合わせたものが前記第二の酸化物膜に相当する。以下、第一の酸化物層、第二の酸化物層は同様に解釈される。 Table 1 shows the film configuration of the formed heat ray reflective laminate. In this embodiment, a combination of the first layer of tin oxide (SnO 2 ) and the second layer of Al-doped zinc oxide layer corresponds to the first oxide film, and the fifth layer of Al-doped zinc oxide layer. And the sixth tin oxide layer correspond to the second oxide film. Hereinafter, a 1st oxide layer and a 2nd oxide layer are interpreted similarly.
前記の熱線遮蔽積層体を形成したガラス基体と、同じ寸法で同じ厚みのガラス基体を用い、常法により図１に示す構成の低放射複層ガラスを製造した。ここで、前記低放射複層ガラスのガラス基体の間隔を１２ｍｍとし、その内部（図１中７の部分）には乾燥空気を充填した。前記低放射複層ガラスについて、以下の評価を行った。結果を表２に示す。 Using a glass substrate having the same dimensions and the same thickness as the glass substrate on which the heat ray shielding laminate was formed, a low radiation multilayer glass having the configuration shown in FIG. 1 was produced by a conventional method. Here, the interval between the glass substrates of the low emission multilayer glass was 12 mm, and the inside (portion 7 in FIG. 1) was filled with dry air. The following evaluation was performed about the said low radiation multilayer glass. The results are shown in Table 2.
（可視光反射率）
日立製作所製Ｕ−４０００型分光光度計を使用して、実施例１の低放射複層ガラスの室外側面と室内側面の反射スペクトルを測定し、ＪＩＳ Ｒ３１０６に基づいて可視光反射率（単位％）を算出した。
(Visible light reflectance)
Using a U-4000 type spectrophotometer manufactured by Hitachi, Ltd., the reflection spectrum of the outdoor side surface and the indoor side surface of the low radiation multilayer glass of Example 1 was measured, and the visible light reflectance (unit%) based on JIS R3106. Was calculated.
（色度）
日立製作所製Ｕ−４０００型分光光度計を使用して、前記低放射複層ガラスの室外側面と室内側面の反射スペクトルを測定し、ＪＩＳ Ｚ８７２２に基づいて前記低放射複層ガラスのそれぞれの面についてのＬ＊ａ＊ｂ＊表色系におけるａ＊およびｂ＊を算出した。
(Chromaticity)
Using a U-4000 type spectrophotometer manufactured by Hitachi, Ltd., the reflection spectrum of the outdoor side surface and the indoor side surface of the low radiation multilayer glass is measured, and each surface of the low radiation multilayer glass is measured based on JIS Z8722. The a * and b * values in the L * a * b * color system were calculated.
（可視光透過率）
日立製作所製Ｕ−４０００型分光光度計を使用して、前記低放射複層ガラスの透過スペクトルを測定し、ＪＩＳ Ｒ３１０６に基づいて前記低放射複層ガラスの可視光透過率（単位％）を算出した。
(Visible light transmittance)
Using a U-4000 spectrophotometer manufactured by Hitachi, Ltd., the transmission spectrum of the low emission multilayer glass is measured, and the visible light transmittance (unit%) of the low emission multilayer glass is calculated based on JIS R3106. did.
（紫外線透過率）
日立製作所製Ｕ−４０００型分光光度計を使用して、前記低放射複層ガラスの透過スペクトルを測定し、ＩＳＯ ９０５０：２００３に基づいて前記低放射複層ガラスの紫外線透過率（単位％）を算出した。
(UV transmittance)
Using a U-4000 spectrophotometer manufactured by Hitachi, Ltd., the transmission spectrum of the low emission multilayer glass is measured, and the ultraviolet transmittance (unit%) of the low emission multilayer glass is measured based on ISO 9050: 2003. Calculated.
（遮蔽係数）
前記低放射複層ガラスについて、ＪＩＳ Ｒ３１０６に基づいて遮蔽係数を測定した。ここで遮蔽係数とは、３ｍｍの透明板ガラス（単板）の透過、及び再放射による室内流入熱量を１とした時の流入熱量を表す相対値であり、ＪＩＳ Ｒ３１０６で規定される日射熱取得率との間には、遮蔽係数＝日射熱取得率／０．８８の関係がある。
(Shielding coefficient)
About the said low radiation multilayer glass, the shielding coefficient was measured based on JISR3106. Here, the shielding coefficient is a relative value representing the inflow heat amount when the inflow heat amount in the room due to the transmission and re-radiation of 3 mm transparent plate glass (single plate) is 1, and the solar heat gain rate defined in JIS R3106 There is a relation of shielding factor = solar heat acquisition rate / 0.88.
（耐久性）
実施例１の熱線反射積層体の耐久性を評価するため、前記熱線反射積層体を形成したガラス基体を、環境試験機（スガ製作所製)を用いて８５℃、湿度９５％の環境に４８時間保持し、膜の劣化度合いを観察た。ここで劣化とは、銀層が凝集し、膜に白点が生じることをいう。白点を目視で判別した結果を表に示す。凝集数が２個／１ｃｍ２以下であれば耐久性が良として○で示し、３個／１ｃｍ２以上であれば耐久性が劣るとして×と表示した。
(durability)
In order to evaluate the durability of the heat ray reflective laminate of Example 1, the glass substrate on which the heat ray reflective laminate was formed was subjected to an environment of 85 ° C. and 95% humidity for 48 hours using an environmental tester (manufactured by Suga Seisakusho). The film was held and the degree of deterioration of the film was observed. Here, the deterioration means that the silver layer is aggregated and white spots are formed on the film. The results of visual discrimination of white spots are shown in the table. When the aggregation number was 2/1 cm 2 or less, the durability was indicated as “good”, and when it was 3/1 cm 2 or more, the durability was inferior.
各層の膜厚が異なる以外は実施例１と同様に、ガラス基体上に熱線反射積層体を形成した。各層の膜厚は放電電力を調整することにより変更した。膜構成は表１に記載の通りであった。また、実施例１と同様に、低放射複層ガラスを製造した。前記低放射複層ガラスについて実施例１と同様に評価した結果を表２に示す。 A heat ray reflective laminate was formed on a glass substrate in the same manner as in Example 1 except that the thickness of each layer was different. The film thickness of each layer was changed by adjusting the discharge power. The film configuration was as shown in Table 1. Moreover, the low radiation | emission multilayer glass was manufactured similarly to Example 1. FIG. Table 2 shows the evaluation results of the low emission multilayer glass in the same manner as in Example 1.
（実施例３〜６）
実施例２と同様に、膜構成の異なる低放射複層ガラスを製造し、評価した。膜構成は表１に記載の通りである。評価結果を表２に示す。
(Examples 3 to 6)
In the same manner as in Example 2, low-radiation multilayer glass having a different film configuration was produced and evaluated. The film structure is as shown in Table 1. The evaluation results are shown in Table 2.
（比較例１〜６）
膜構成が異なる以外は実施例１と同様に、ガラス基体上に熱線反射積層体を形成した。各層の厚みは放電電力を調整することにより変更した。膜構成は表１に記載の通りであった。また、実施例１と同様に、低放射複層ガラスを製造した。前記低放射複層ガラスについて実施例１と同様に評価した結果を表２に示す。
(Comparative Examples 1-6)
A heat ray reflective laminate was formed on a glass substrate in the same manner as in Example 1 except that the film configuration was different. The thickness of each layer was changed by adjusting the discharge power. The film configuration was as shown in Table 1. Moreover, the low radiation | emission multilayer glass was manufactured similarly to Example 1. FIG. Table 2 shows the evaluation results of the low emission multilayer glass in the same manner as in Example 1.
実施例１〜６においては、前記第一の酸化物膜に相当する部分と前記第二の酸化物膜に相当する部分の厚さを、それぞれ３０ｎｍ以上４０ｎｍ以下と３０ｎｍ以上５０ｎｍ以下の範囲にしたため、非膜面側の可視光反射率、特に視感度の最も高い５５０ｎｍの反射率を低く抑えることができた。これにより、非膜面側の反射によるぎらつき感を抑え、中性反射色を実現することができた。 In Examples 1 to 6, the thickness corresponding to the first oxide film and the thickness corresponding to the second oxide film were in the range of 30 nm to 40 nm and 30 nm to 50 nm, respectively. The visible light reflectance on the non-film surface side, particularly the reflectance at 550 nm, which has the highest visibility, could be kept low. As a result, the glare caused by reflection on the non-film surface side was suppressed, and a neutral reflection color could be realized.
また、第３層のＡｇ膜の厚さを８ｎｍ以上１０ｎｍ以下の範囲にすることにより反射率を低減し、さらに第４層の金属膜の厚さを１ｎｍ以上８ｎｍ以下の範囲にすることによって遮蔽係数を０．５７以下に抑えることができ、中性反射色と遮熱性能向上を同時に満たすことができた。 Further, the reflectance is reduced by setting the thickness of the Ag film of the third layer to be in the range of 8 nm to 10 nm, and further the shielding is achieved by setting the thickness of the metal film of the fourth layer to be in the range of 1 nm to 8 nm. The coefficient could be suppressed to 0.57 or less, and the neutral reflection color and the improvement of the heat shielding performance could be satisfied at the same time.
実施例２および５の結果から、金属膜として、Ａｌ含有量がＺｎに対する原子比で１％以上６％以下の範囲のＺｎＡｌ合金膜を使用することで、紫外線透過率を低減できることがわかる。 From the results of Examples 2 and 5, it is understood that the ultraviolet transmittance can be reduced by using a ZnAl alloy film having an Al content in the range of 1% or more and 6% or less in terms of atomic ratio to Zn as the metal film.
一方、比較例１においては酸化物の膜厚が薄いため、また比較例３では酸化物の膜厚が厚いために、非膜面色調が中性色から外れて不快感を与える色合いとなった。 On the other hand, in Comparative Example 1, the oxide film was thin, and in Comparative Example 3, the film thickness of the oxide was thick. .
また、比較例２においては、Ａｇ膜を厚く、金属膜を薄くしたが、遮蔽係数を効果的に低減することはできず、非膜面色調が中性色から外れることとなった。 In Comparative Example 2, although the Ag film was thick and the metal film was thin, the shielding coefficient could not be effectively reduced, and the non-film surface color tone deviated from the neutral color.
比較例４においては、Ａｇ膜厚を薄くすることにより色調を中性色として不快感を低減することができたが、遮蔽係数が高くなった。 In Comparative Example 4, it was possible to reduce the discomfort by making the color tone neutral by reducing the Ag film thickness, but the shielding coefficient increased.
比較例５においては、Ａｇ膜に接するようにＡｌドープ酸化亜鉛膜を作製していないために、耐久性が悪い結果となった。 In Comparative Example 5, since an Al-doped zinc oxide film was not produced so as to be in contact with the Ag film, the durability was poor.
比較例６においては、Ａｇ層の上に酸化錫膜のみを成膜したために、耐久性が悪い結果となった。 In Comparative Example 6, because only the tin oxide film was formed on the Ag layer, the durability was poor.
本発明の低放射複層ガラスによれば、遮熱性能を維持しながら、高い可視光透過率を確保することが可能なため、好適に窓等の室内外境界に設置することができる。 According to the low radiation multilayer glass of the present invention, it is possible to ensure high visible light transmittance while maintaining the heat shielding performance, and therefore it can be suitably installed at the indoor / outdoor boundary such as a window.
１ 複層ガラス
２ ガラス板
３ 第一の酸化物膜
４ Ａｇ膜
５ 金属膜
６ 第二の酸化物膜
７ 間隙
DESCRIPTION OF SYMBOLS 1 Multi-layer glass 2 Glass plate 3 1st oxide film 4 Ag film 5 Metal film 6 2nd oxide film 7 Gaps
Claims (9)
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006016048A JP2007197237A (en) | 2006-01-25 | 2006-01-25 | Low-radiation double glazing |
| PCT/JP2006/316464 WO2007029494A1 (en) | 2005-09-06 | 2006-08-23 | Low-radiation double glazing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006016048A JP2007197237A (en) | 2006-01-25 | 2006-01-25 | Low-radiation double glazing |
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| Publication Number | Publication Date |
|---|---|
| JP2007197237A true JP2007197237A (en) | 2007-08-09 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2006016048A Pending JP2007197237A (en) | 2005-09-06 | 2006-01-25 | Low-radiation double glazing |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011063500A (en) * | 2009-08-17 | 2011-03-31 | Central Glass Co Ltd | Heat ray shielding laminated film |
| JP2011173764A (en) * | 2010-02-25 | 2011-09-08 | Central Glass Co Ltd | Low radiation film |
| JP2017081787A (en) * | 2015-10-29 | 2017-05-18 | セントラル硝子株式会社 | Multiple glass |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10182192A (en) * | 1996-12-25 | 1998-07-07 | Central Glass Co Ltd | Heat insulating glass |
| JPH1134216A (en) * | 1997-05-21 | 1999-02-09 | Asahi Glass Co Ltd | Laminate and glass laminate for window |
| JPH11157881A (en) * | 1997-09-18 | 1999-06-15 | Central Glass Co Ltd | Low radiation glass-laminated body |
| JP2000044290A (en) * | 1998-07-31 | 2000-02-15 | Central Glass Co Ltd | Low pressure double layer glass and its production |
| JP2006159580A (en) * | 2004-12-06 | 2006-06-22 | Nippon Sheet Glass Co Ltd | Heat ray blocking laminate |
-
2006
- 2006-01-25 JP JP2006016048A patent/JP2007197237A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10182192A (en) * | 1996-12-25 | 1998-07-07 | Central Glass Co Ltd | Heat insulating glass |
| JPH1134216A (en) * | 1997-05-21 | 1999-02-09 | Asahi Glass Co Ltd | Laminate and glass laminate for window |
| JPH11157881A (en) * | 1997-09-18 | 1999-06-15 | Central Glass Co Ltd | Low radiation glass-laminated body |
| JP2000044290A (en) * | 1998-07-31 | 2000-02-15 | Central Glass Co Ltd | Low pressure double layer glass and its production |
| JP2006159580A (en) * | 2004-12-06 | 2006-06-22 | Nippon Sheet Glass Co Ltd | Heat ray blocking laminate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011063500A (en) * | 2009-08-17 | 2011-03-31 | Central Glass Co Ltd | Heat ray shielding laminated film |
| JP2011173764A (en) * | 2010-02-25 | 2011-09-08 | Central Glass Co Ltd | Low radiation film |
| JP2017081787A (en) * | 2015-10-29 | 2017-05-18 | セントラル硝子株式会社 | Multiple glass |
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