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WO2016199676A1 - Empilement de films et verre feuilleté - Google Patents

Empilement de films et verre feuilleté Download PDF

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Publication number
WO2016199676A1
WO2016199676A1 PCT/JP2016/066465 JP2016066465W WO2016199676A1 WO 2016199676 A1 WO2016199676 A1 WO 2016199676A1 JP 2016066465 W JP2016066465 W JP 2016066465W WO 2016199676 A1 WO2016199676 A1 WO 2016199676A1
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WIPO (PCT)
Prior art keywords
film
layer
functional layer
dielectric layer
laminated
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PCT/JP2016/066465
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English (en)
Japanese (ja)
Inventor
章代 松本
剛 富澤
秀文 小▲高▼
康幸 滝本
Original Assignee
旭硝子株式会社
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Application filed by 旭硝子株式会社 filed Critical 旭硝子株式会社
Priority to CN201680033831.6A priority Critical patent/CN107614451B/zh
Priority to JP2017523607A priority patent/JP6673349B2/ja
Publication of WO2016199676A1 publication Critical patent/WO2016199676A1/fr

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    • 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
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions

Definitions

  • the present invention relates to a film laminate having a heat shielding property, and a laminated glass having such a film laminate.
  • a film laminate having a heat shielding property is often used.
  • This film laminate is configured by laminating a plurality of layers including a heat ray reflective functional layer on a substrate.
  • heat shielding properties can be obtained by the infrared reflection effect of the heat ray reflective functional layer.
  • Such a film laminate is provided in the form of a film, for example, and is used by adhering the membrane laminate to a member to be installed.
  • membrane laminated body is comprised with the bulk body in which a base
  • the film laminate includes a thin layer (hereinafter referred to as “silver layer”) composed of silver or a silver alloy. This is because silver exhibits a good heat ray reflection function and hardly absorbs light in the visible light wavelength region. That is, by installing a silver layer in the film laminate, good heat shielding properties and high permeability can be obtained.
  • silver layer a thin layer composed of silver or a silver alloy.
  • an index called selectivity Se represented by Tv / g is often used to represent the heat shielding property of the film laminate.
  • Tv (%) is the visible light transmittance (%) of the film stack
  • g (%) is the solar heat gain rate (%) of the film stack.
  • the solar heat acquisition rate g (%) is the heat (transmitted heat) directly transmitted to the opposite side (second side) with respect to the total solar heat incident from the substrate side (first side) of the film laminate. , Expressed as a percentage of the sum of heat absorbed in the film stack and then released to the second side of the film stack.
  • the film laminate including the silver layer as described above generally has a high selectivity Se and is therefore transparent and exhibits good heat shielding properties.
  • the silver layer is not very good in environmental resistance and may oxidize or deteriorate with use. Furthermore, when such a phenomenon occurs in the silver layer, there may arise a problem that the transparency and heat shielding property of the film laminate are lowered.
  • the present invention has been made in view of such a background, and an object of the present invention is to provide a film laminate having high selectivity and good environmental resistance. Moreover, it aims at providing a laminated glass provided with such a film
  • a film laminate having a laminated film on a transparent substrate,
  • the laminated film has one or more functional layers,
  • the stacked film includes a first portion, and the first portion includes a first dielectric layer, a first functional layer on the first dielectric layer, and a second on the functional layer.
  • the first functional layer is a functional layer farthest from the transparent substrate among the one or more functional layers,
  • the first functional layer is composed of zirconium nitride ZrN x ,
  • the first functional layer has a refractive index n of less than 1.2 at a wavelength of 500 nm, an extinction coefficient k of greater than 6 at a wavelength of 1500 nm,
  • Tv visible light transmittance measured from the transparent substrate side toward the outermost layer of the laminated film
  • the solar heat gain is g (%)
  • the selectivity Se represented by the following formula (1): 1.1 ⁇ Se Formula (1)
  • a film stack is provided that satisfies
  • a film laminate having high selectivity and good environmental resistance can be provided.
  • membrane laminated body can be provided.
  • FIG. 1 shows a schematic cross-sectional view of a film stack (hereinafter referred to as “first film stack”) according to an embodiment of the present invention.
  • the first film laminate 100 includes a transparent substrate 110 and a laminate film 120.
  • the transparent substrate 110 has a role of supporting the laminated film 120 installed on the top.
  • the transparent substrate 110 has a first surface 112 and a second surface 114, and the laminated film 120 is disposed on the first surface 112 side of the transparent substrate 110.
  • the laminated film 120 is composed of a plurality of layers.
  • the stacked film 120 includes the first dielectric layer 122, the first seed layer 125, the first functional layer 130, the first sacrificial layer 132, and the second dielectric layer. 135 and the top layer 140 are provided in this order.
  • the laminated film 120 may have other configurations.
  • a sacrificial layer may be provided between the first dielectric layer 122 and the first seed layer 125, or instead of the first seed layer 125.
  • a sacrificial layer may be provided.
  • the top layer 140 can also be omitted if necessary.
  • the first seed layer 125 in the laminated film 120 has a role of promoting crystal growth of the first functional layer 130 disposed immediately above.
  • the first sacrificial layer 132 in the stacked film 120 suppresses deterioration of the adjacent layer (for example, the first functional layer 130) due to heat during the heat treatment of the stacked film 120 (or a part thereof).
  • the top layer 140 is installed as a protective layer of the first film stack 100 and has a role of protecting the stacked film 120.
  • the continuous portion from the first dielectric layer 122 to the second dielectric layer 135 in the stacked film 120 is the most basic main portion of the stacked film 120. Therefore, in the present application, this continuous portion is particularly referred to as the first portion 145.
  • the first seed layer 125 and the first sacrificial layer 132 are layers that are arbitrarily disposed, these layers do not necessarily exist in the first portion 145. .
  • the first functional layer 130 has a heat ray reflecting function. More specifically, the first functional layer 130 is made of zirconium nitride ZrN x , has a refractive index n of less than 1.2 at a wavelength of 500 nm, and has an extinction coefficient k greater than 6 at a wavelength of 1500 nm.
  • the selectivity Se represented by Tv / g is expressed by the following formula (1): 1.1 ⁇ Se Formula (1) Meet.
  • a so-called “silver layer” made of thin silver or a silver alloy has a problem that environmental resistance is not so good. For this reason, although a film laminate having a laminated film including a silver layer initially exhibits a good heat ray reflection function, oxidation and deterioration of the silver layer proceed with use time, and thereby the transparency of the film laminate In addition, there may be a problem that the heat shielding property is lowered.
  • the first film stack 100 is characterized in that the first functional layer 130 is composed of zirconium nitride ZrN x instead of silver. That is, in the first film stack 100, zirconium nitride ZrN x is used as the first functional layer 130 for expressing the heat ray reflecting function.
  • This zirconium nitride ZrN x is a material superior in environmental resistance as compared with silver and silver alloys, and the problem that the first functional layer 130 deteriorates with use time hardly occurs. For this reason, in the 1st functional layer 130, a heat ray reflective function can be maintained stably over a long period of time.
  • the film stack may often not exhibit proper permeability and heat shielding properties. It recognized.
  • the zirconium nitride ZrN x constituting the first functional layer 130 has a refractive index n of less than 1.2 at a wavelength of 500 nm and an extinction coefficient k of 6 at a wavelength of 1500 nm. Also configured to be larger.
  • the selectivity Se satisfies the above-described formula (1) and can achieve both high permeability and high heat shielding properties.
  • the first film laminate 100 can stably exhibit high transparency and good heat shielding properties.
  • membrane laminated body 100 may be used with the form of the film affixed on a to-be-installed member, for example.
  • the transparent substrate 110 is formed of a thin member of, for example, 0.5 mm or less so as to have flexibility. Thereby, sticking to the to-be-installed member of the 1st film
  • the installed member may be, for example, a glass plate.
  • the first film laminate 100 may be used as a member such as a building member or a vehicle member in the form of “as is”, for example.
  • the transparent base 110 is composed of, for example, a member of 0.5 mm or more so as to have rigidity.
  • the transparent substrate 110 may be formed of a glass substrate.
  • the first film laminate 100 may be used as one glass member for laminated glass.
  • laminated glass has first and second glass plates and an intermediate film that is disposed between both glass plates and joins both glass plates.
  • the first film laminate 100 can be applied as one or both glass plates of this laminated glass.
  • the first film laminated body 100 may be used so that the transparent substrate 110 side is “inside”, that is, the intermediate film side, or the laminated film 120 side is “inside”. good.
  • the first film laminate 100 may be used as a single glass member for a multilayer glass.
  • the multilayer glass has first and second glass plates and a space layer provided between both glass plates.
  • the first film laminate 100 can be applied as one or both glass plates of the multilayer glass.
  • the first film laminated body 100 may be used so that the transparent substrate 110 side is “inside”, that is, the space layer side, or the laminated film 120 side is “inside”. good.
  • membrane laminated body 100 which has the above characteristics is demonstrated in detail.
  • the reference numerals shown in FIG. 1 are used to represent each member for the sake of clarity.
  • Transparent substrate 110 The material constituting the transparent substrate 110 is not particularly limited.
  • the transparent substrate 110 may be made of glass, resin, plastic, or the like.
  • the thickness of the transparent substrate 110 is not particularly limited, and an appropriate thickness is selected depending on the purpose of use of the first film stack 100.
  • the transparent substrate 110 may have a thickness of 0.01 mm to 1 mm.
  • the transparent substrate 110 is formed of a glass substrate and has a thickness of 0.5 mm. It may have a thickness of ⁇ 20 mm.
  • the first dielectric layer 122 may be composed of, for example, a layer including at least one of silicon nitride, silicon nitride containing aluminum, and silicon nitride containing zirconium.
  • the first dielectric layer 122 may be composed of, for example, a layer containing at least one of ITO (indium tin oxide), tin oxide, titanium oxide, zirconium oxide, zinc oxide, and Zr 3 N 4. good.
  • the first dielectric layer 122 may contain oxygen.
  • the first dielectric layer 122 may be a single layer film or a laminated film made of different kinds of films.
  • the first dielectric layer 122 may have a “crystallinity improving material” in a region in contact with the first functional layer 130 (hereinafter referred to as “upper region”).
  • the “crystallinity-improving material” means a material capable of increasing the crystallinity of the first functional layer 130 disposed on the upper part, for example, ZrN x (where X> 1.2). , NbN x (where X> 1), TiN x (where 0.9 ⁇ X ⁇ 1.1 or X> 1.2), and the like.
  • the refractive index n of the first functional layer 130 at a wavelength of 500 nm can be further reduced, and the extinction coefficient at a wavelength of 1500 nm. k can be further improved.
  • an orientation index P obtained by an in-plane X-ray diffraction method is introduced as an index showing the effect of improving the crystallinity of the first functional layer 130. Note that the in-plane X-ray diffraction method is employed in this method even if the second dielectric layer 135 or the like is present on the first functional layer 130, the crystallinity of the first functional layer 130. This is because it can be properly evaluated.
  • the orientation index P is determined as follows:
  • Max [a, b, c] represents the maximum value of a to c
  • Min [a, b, c] represents the minimum value of a to c
  • Is (111) can be obtained from the peak intensity I (111) at the plane orientation (111) obtained by in-plane X-ray diffraction of the first functional layer 130 (ZrN x ).
  • Is (200) can be obtained from the peak intensity I (200) in the plane orientation (200) obtained by in-plane X-ray diffraction of the first functional layer 130 (ZrN x )
  • Is (220 ) Can be obtained from the peak intensity I (220) at the plane orientation (220) obtained by in-plane X-ray diffraction of the first functional layer 130 (ZrN x ).
  • the peak intensity I (111) is the maximum intensity within a range of ⁇ 1 ° around the diffraction angle 2 ⁇ (angle between the incident X-ray direction and the diffraction X-ray direction) of 33.9 °
  • the peak intensity I ( 200) is the maximum intensity within a range of ⁇ 1 ° around a diffraction angle 2 ⁇ of 39.4 °
  • the peak intensity I (220) is the maximum within a range of ⁇ 1 ° around a diffraction angle 2 ⁇ of 56.9 °.
  • the divisor (the denominator on the right side) in the equations (4) to (6) is (111), (111), (ZrN powder pattern) obtained from the National Institute for Materials Science (AtomWorks) 200) and (220), which corresponds to the peak intensity ratio in three directions, that is, 99:85:48.
  • Is (111), Is (200), and Is (220) are obtained by normalizing the peak intensity obtained by the in-plane X-ray diffraction of the first functional layer 130 (ZrN x ) with the peak intensity of the powder pattern. Value can be considered.
  • the orientation index P expressed by the above-described equation (3) represents how much the orientation of the first functional layer 130 (ZrN x ) is biased with respect to the powder pattern. Therefore, it can be said that as the orientation index P is larger, the first functional layer 130 (ZrN x ) is oriented in a specific direction.
  • the orientation index P of the first functional layer 130 is about 1.
  • the orientation index P of the first functional layer 130 is 2 or more.
  • the thickness of the first dielectric layer 122 may be in the range of 3 nm to 300 nm, for example.
  • the first dielectric layer 122 may be installed by, for example, physical vapor deposition (physical vapor deposition, PVD, sputtering, etc.) or chemical vapor deposition (CVD, etc.). good.
  • physical vapor deposition physical vapor deposition, PVD, sputtering, etc.
  • CVD chemical vapor deposition
  • the sputtering method is particularly preferable.
  • the second dielectric layer 135 as for the first dielectric layer 122.
  • the material and / or thickness of the second dielectric layer 135 may be the same as or different from those of the first dielectric layer 122.
  • the first functional layer 130 is composed of zirconium nitride ZrN x .
  • x is preferably in the range of 0.9 ⁇ x ⁇ 1.0.
  • the first functional layer 130 preferably has a range of 0.9 ⁇ x ⁇ 1.1.
  • the crystal orientation of the first functional layer 130 is aligned to a certain orientation. As a result, the orientation of the first functional layer 130 is enhanced, and there is no room for excess nitrogen to enter the grain boundary, and an ideal crystal can be obtained in a wider range of x.
  • 0.9 ⁇ x ⁇ 1.0 is relatively close to the stoichiometric ratio, and the amount of nitrogen is also suppressed, so that nitrogen does not enter between the lattices. Can be obtained.
  • the film thickness of the first functional layer 130 is, for example, in the range of 1 nm to 60 nm.
  • the first functional layer 130 may be formed by, for example, a physical vapor deposition method (physical vapor deposition method, PVD method, sputtering method, etc.) or a chemical vapor deposition method (CVD method, etc.). .
  • a physical vapor deposition method physical vapor deposition method, PVD method, sputtering method, etc.
  • CVD method chemical vapor deposition method, etc.
  • the composition of zirconium nitride ZrN x is controlled by controlling film formation conditions (for example, the temperature of the transparent substrate during film formation, the film formation pressure, the composition of the introduced gas, the target composition, the post-heat treatment temperature, etc.) That is, the value of x can be adjusted. Further, by controlling the film forming conditions, it is possible to form the zirconium nitride ZrN x having the refractive index n and the extinction coefficient k as described above relatively easily.
  • film formation conditions for example, the temperature of the transparent substrate during film formation, the film formation pressure, the composition of the introduced gas, the target composition, the post-heat treatment temperature, etc.
  • the zirconium nitride ZrN x constituting the first functional layer 130 may contain a maximum of about 3 at% of impurities (for example, carbon and oxygen) inevitably introduced during film formation.
  • impurities for example, carbon and oxygen
  • the zirconium nitride ZrN x constituting the first functional layer 130 contains impurities contained in the target containing Zr (for example, Hf, Ti, V, Nb, Ta, Cr, Mo, W, O, C or the like) may be included up to about 3 at%.
  • First seed layer 125 and first sacrificial layer 132 are arbitrarily installed layers, and may be formed of a plurality of layers or may be omitted.
  • the first seed layer 125 is made of, for example, a single metal such as Zr, Ti, or Si, or a metal nitride such as TiN.
  • the thickness of the first seed layer 125 may be in the range of 1 nm to 10 nm, for example.
  • the first sacrificial layer 132 is made of, for example, Zn, Zr, Ti, or NiCr. The thickness of the first sacrificial layer 132 may be in the range of 1 nm to 10 nm, for example.
  • first seed layer 125 may contain oxygen.
  • These layers may be formed by, for example, physical vapor deposition (physical vapor deposition, PVD, sputtering, etc.) or chemical vapor deposition (CVD, etc.).
  • physical vapor deposition physical vapor deposition, PVD, sputtering, etc.
  • chemical vapor deposition CVD, etc.
  • the sputtering method is particularly preferable.
  • the first seed layer 125 may be ZrN x (where X> 1.2), NbN x (where X> 1), or TiN x (where 0.9 ⁇ X ⁇ 1.1 or X> 1.2).
  • top layer 140 is a layer that is arbitrarily installed and may be omitted.
  • the top layer 140 need not be provided.
  • the top layer 140 is made of, for example, SiO 2 , TiN, or C.
  • the thickness of the top layer 140 may be in the range of 1 nm to 10 nm, for example.
  • the top layer 140 may be formed by, for example, a physical vapor deposition method (physical vapor deposition method, PVD method, sputtering method, etc.) or a chemical vapor deposition method (CVD method, etc.). Among these film forming methods, the sputtering method is particularly preferable.
  • the laminated film 120 includes a layer made of zirconium nitride ZrN x having the above-described characteristics as the first functional layer 130. This material is superior in mechanical durability and chemical durability compared to silver. Therefore, when the laminated film 120 has only a single functional layer (that is, the first functional layer 130), it is possible to provide the film laminated body 100 having good environmental resistance.
  • the functional layer located on the outermost side of the laminated film is composed of zirconium nitride ZrN x .
  • the “inner” functional layer or layers may be made of a material other than zirconium nitride ZrN x .
  • the entire laminated film can exhibit good environmental resistance.
  • FIG. 2 shows a schematic cross-sectional view of another film laminate (hereinafter referred to as “second film laminate”) according to an embodiment of the present invention.
  • the second film laminate 200 includes a transparent substrate 210 and a laminate film 220.
  • the transparent substrate 210 has a role of supporting the laminated film 220 installed on the top.
  • the transparent substrate 210 has a first surface 212 and a second surface 214, and the laminated film 220 is disposed on the first surface 212 side of the transparent substrate 210.
  • the laminated film 220 has a basic portion constituted by the first dielectric layer 222, the first functional layer 230, and the second dielectric layer 235, that is, the first portion 245.
  • the first portion 245 may further include a first seed layer and / or a first sacrificial layer as described above.
  • the first seed layer is disposed between the first dielectric layer 222 and the first functional layer 230
  • the first sacrificial layer is the first functional layer 230 and the second dielectric layer. 235.
  • the orientation index P of the first functional layer 230 becomes 2 or more.
  • the crystallinity of the first functional layer 230 is improved.
  • the laminated film 220 has a top layer 240 on top of the first portion 245.
  • the top layer 240 may be omitted.
  • the role of the top layer 240 is the same as that of the top layer 140 in the first film stack 100 described above.
  • the first functional layer 230 present in the first portion 245 is made of zirconium nitride ZrN x , has a refractive index n of less than 1.2 at a wavelength of 500 nm, and an extinction coefficient k of 6 at a wavelength of 1500 nm. It is characterized by being larger than.
  • the visible light transmittance measured from the second surface 214 side of the transparent substrate 210 toward the outermost layer of the laminated film 220 is Tv (%), and solar heat acquisition is performed.
  • the rate is g (%)
  • the selectivity Se represented by Tv / g is expressed by the following formula (1): 1.1 ⁇ Se Formula (1) Meet.
  • the second film stack 200 can stably exhibit high transparency and good heat shielding properties.
  • the laminated film 220 further includes a third dielectric layer 250 and a second functional layer in the order closer to the first surface 212 on the lower side than the first portion 245, that is, on the side closer to the transparent substrate 210. 255.
  • the laminated film 220 has such a configuration, it is possible to adjust the color and / or selectivity Se relatively easily as compared with the first film laminated body 100.
  • the third dielectric layer 250 may have an upper region made of a crystallinity improving material, as in the case of the first dielectric layer described above.
  • the second functional layer 255 is composed of a ZrN x material
  • the third dielectric layer 250 having the upper region of the crystallinity improving material as described above is disposed, whereby the crystal of the second functional layer 255 is formed. Can increase the sex.
  • membrane laminated body 200 shown in FIG. 2 is demonstrated in detail.
  • the transparent substrate 210, the first portion 245, and the top layer 240 are described with respect to each member of the first film laminate 100 as shown in FIG. You can refer to it. Therefore, only the third dielectric layer 250 and the second functional layer 255 will be described here. Further, in the following description, the reference numerals shown in FIG. 2 are used for representing each member for the sake of clarity.
  • the third dielectric layer 250 may be composed of, for example, a layer including at least one of silicon nitride, silicon nitride containing aluminum, and silicon nitride containing zirconium.
  • the third dielectric layer 250 may be formed of a layer containing at least one of ITO (indium tin oxide), tin oxide, titanium oxide, zirconium oxide, zinc oxide, and Zr 3 N 4 , for example. good.
  • the thickness of the third dielectric layer 250 may be in the range of 3 nm to 300 nm, for example.
  • the third dielectric layer 250 may be formed by, for example, a physical vapor deposition method (physical vapor deposition method, PVD method, sputtering method, etc.) or a chemical vapor deposition method (CVD method, etc.). good.
  • a physical vapor deposition method physical vapor deposition method, PVD method, sputtering method, etc.
  • CVD method chemical vapor deposition method, etc.
  • the third dielectric layer 250 may have the same composition as the first dielectric layer 222 and / or the second dielectric layer 235.
  • the second functional layer 255 is a transparent and conductive material, any material may be used.
  • the second functional layer 255 may be, for example, ITO (Indium Tin Oxide). Further, the second functional layer 255 may be made of zirconium nitride ZrN x similar to the first functional layer 230.
  • the second functional layer 255 may be a thin layer made of silver or a silver alloy, that is, a “silver layer”. Even when such a silver layer is used for the second functional layer 255, the first portion 245 having good environmental resistance exists above the second functional layer 255. This is because H.245 functions as a protective barrier for the second functional layer 255.
  • the 2nd functional layer 255 may be comprised by several layers.
  • the second functional layer 255 may have a three-layer structure of first metal layer / silver layer / second metal layer.
  • the film thickness of the second functional layer 255 is, for example, in the range of 1 nm to 500 nm.
  • the second functional layer 255 may be formed by, for example, a physical vapor deposition method (physical vapor deposition method, PVD method, sputtering method, etc.) or a chemical vapor deposition method (CVD method, etc.). .
  • a physical vapor deposition method physical vapor deposition method, PVD method, sputtering method, etc.
  • CVD method chemical vapor deposition method, etc.
  • the second film stack 200 may have other configurations.
  • the third dielectric layer 250 may be omitted.
  • the second functional layer 255 is directly installed on the first surface 212 of the transparent substrate 210.
  • another functional layer and dielectric layer set is provided below the third dielectric layer 250 and from the side closer to the first surface 212.
  • one or more may be installed.
  • the number of such sets may be 2, 3, or 4 or more, for example. In this case, it becomes easier to adjust the color and / or selectivity Se of the film laminate.
  • the film laminate can take various layer configurations in addition to this.
  • Examples 1 to 9, Examples 31 to 39, and Examples 41 to 44 are examples.
  • Examples 21 to 26, Examples 51 to 55, and Examples 65 to 67 are examples.
  • Examples 56 to 64 are examples.
  • Example 1 A laminated film was produced by forming a laminated film on one surface of the glass substrate by the following method.
  • soda lime glass having dimensions of 100 mm long ⁇ 100 mm wide ⁇ 2.8 mm thick was used.
  • the laminated film has a three-layer structure of a first dielectric layer / first functional layer / second dielectric layer from the side close to the glass substrate.
  • the first dielectric layer is silicon nitride containing aluminum (target film thickness 46 nm)
  • the first functional layer is ZrN x (target film thickness 42 nm)
  • the second dielectric layer is silicon nitride containing aluminum. (Target film thickness 56 nm).
  • the pressure during film formation was 0.26 Pa. Note that the glass substrate was heated to 300 ° C. during the formation of the first functional layer.
  • the pressure during film formation was 0.4 Pa.
  • film laminate according to Example 1 a film laminate (hereinafter referred to as “film laminate according to Example 1”) was manufactured.
  • Example 2 and Example 3 A film stack (referred to as “film stack according to example 2” and “film stack according to example 3”, respectively) was manufactured in the same manner as in example 1.
  • Example 2 the thickness of each layer was changed from that in Example 1.
  • Example 4 to Example 6 By the same method as in Example 1, film laminates (each referred to as “film laminates according to Examples 4 to 6”) were produced.
  • Example 4 to 6 the thickness of each layer was changed from that in Example 1.
  • the glass substrate was not heated during the formation of the first functional layer. Further, after the formation of the second dielectric layer was completed, the glass substrate was heated to 600 ° C. and held at 600 ° C. for 20 minutes.
  • Example 7 to Example 9 In the same manner as in Example 1, film laminates (each referred to as “film laminates according to Examples 7 to 9”) were produced.
  • Example 7 to 9 the thickness of each layer was changed from that in Example 1.
  • the glass substrate was not heated during the formation of the first functional layer. Further, the heat treatment was not performed after the second dielectric layer was formed.
  • Example 21 to Example 22 By the same method as in Example 1, film laminates (referred to as “film laminates according to Examples 21 to 22”, respectively) were produced.
  • Example 21 to 22 the thickness of each layer was changed from that in Example 1.
  • the pressure during film formation was 0.35 Pa.
  • the glass substrate was not heated during the formation of the first functional layer. Further, the heat treatment was not performed after the second dielectric layer was formed.
  • Example 23 to Example 24 In the same manner as in Example 1, film laminates (referred to as “film laminates according to Examples 23 to 24”, respectively) were produced.
  • Example 23 to 24 the thickness of each layer was changed from that in Example 1.
  • the pressure during film formation was 0.26 Pa.
  • the glass substrate was not heated during the formation of the first functional layer. Further, the heat treatment was not performed after the second dielectric layer was formed.
  • Example 25 A laminated film was produced by forming a laminated film on one surface of the glass substrate by the following method.
  • soda lime glass having dimensions of 100 mm long ⁇ 100 mm wide ⁇ 2.8 mm thick was used.
  • the configuration of the laminated film was a structure of the first dielectric layer / first functional layer / second dielectric layer from the side close to the glass substrate.
  • the first dielectric layer has a two-layer structure of silicon nitride (target film thickness 20 nm) and silicon oxide (target film thickness 40 nm).
  • the first functional layer was niobium nitride (target film thickness 30 nm)
  • the second dielectric layer was silicon nitride containing aluminum (target film thickness 30 nm).
  • the pressure during film formation was 0.4 Pa.
  • the pressure during film formation was 0.4 Pa.
  • the pressure during film formation was 0.4 Pa.
  • film laminate according to Example 25 a film laminate (hereinafter referred to as “film laminate according to Example 25”) was produced.
  • Example 26 A film laminate (hereinafter referred to as “film laminate according to Example 26”) was produced in the same manner as in Example 7 above.
  • Example 26 the thickness of each layer was changed from that in Example 7. Further, chromium nitride (target film thickness: 10 nm) was used as the first functional layer.
  • the pressure during film formation was 0.28 Pa. Note that the glass substrate was not heated during the formation of the first functional layer.
  • Example 31 A laminated film was produced by forming a laminated film on one surface of the glass substrate by the following method.
  • soda lime glass having dimensions of 100 mm long ⁇ 100 mm wide ⁇ 2.8 mm thick was used.
  • the laminated film has a five-layer structure of third dielectric layer / second functional layer / first dielectric layer / first functional layer / second dielectric layer from the side close to the glass substrate. did.
  • the third dielectric layer is silicon nitride containing aluminum (target film thickness 25 nm), the second functional layer is ZrN x (target film thickness 19 nm), and the first dielectric layer is silicon nitride containing aluminum. (Target film thickness 91 nm), the first functional layer was ZrN x (target film thickness 40 nm), and the second dielectric layer was silicon nitride containing aluminum (target film thickness 38 nm).
  • the pressure during film formation was 0.26 Pa. Note that the glass substrate was heated to 300 ° C. during the formation of the second functional layer.
  • the pressure during film formation was 0.4 Pa.
  • the pressure during film formation was 0.26 Pa. Note that the glass substrate was heated to 300 ° C. during the formation of the first functional layer.
  • the pressure during film formation was 0.4 Pa.
  • film laminate according to Example 31 a film laminate (hereinafter referred to as “film laminate according to Example 31”) was manufactured.
  • Example 32 and Example 33 A film stack (referred to as “film stack according to example 32” and “film stack according to example 33”, respectively) was manufactured in the same manner as in example 31.
  • Example 34 to Example 36 A film stack (referred to as “film stacks according to Examples 34 to 36”) was produced in the same manner as in Example 31.
  • Example 34 to 36 the thickness of each layer was changed from that in Example 31.
  • the glass substrate was not heated during the formation of the first functional layer.
  • the glass substrate was heated to 600 ° C. after the formation of the second dielectric layer was completed.
  • Example 37 to Example 39 A film stack (referred to as “film stacks according to Examples 37 to 39”) was manufactured in the same manner as in Example 31.
  • Example 37 to 39 the thickness of each layer was changed from that in Example 31.
  • the glass substrate was not heated during the formation of any layer. Furthermore, no heat treatment was performed even after all layers were formed.
  • Example 41 A laminated film was produced by forming a laminated film on one surface of the glass substrate by the following method.
  • soda lime glass having dimensions of 100 mm long ⁇ 100 mm wide ⁇ 2.8 mm thick was used.
  • the configuration of the laminated film was a structure of third dielectric layer / second functional layer / first dielectric layer / first functional layer / second dielectric layer from the side close to the glass substrate.
  • the third dielectric layer was silicon nitride containing aluminum (target film thickness 28 nm).
  • the second functional layer was made of silver (target film thickness 15.5 nm), and two sacrificial layers of nickel chromium alloy (target film thickness 1 nm) were provided so as to sandwich the second functional layer.
  • the first dielectric layer was silicon nitride containing aluminum (target film thickness 97.5 nm).
  • the first functional layer was ZrN x (target film thickness 25.5 nm), and the second dielectric layer was silicon nitride containing aluminum (target film thickness 48 nm).
  • Ni-20 wt% Cr and an Ag target were used, and argon was used as a discharge gas.
  • the pressure during film formation was 0.47.
  • the pressure during film formation was 0.4 Pa.
  • the pressure during film formation was 0.26 Pa. Note that the glass substrate was heated to 300 ° C. during the formation of the first functional layer.
  • the pressure during film formation was 0.4 Pa.
  • film laminate according to Example 41 a film laminate (hereinafter referred to as “film laminate according to Example 41”) was manufactured.
  • Example 42 A film laminate (hereinafter referred to as “film laminate according to Example 42”) was produced in the same manner as in Example 41 described above.
  • Example 42 the thickness of each layer was changed from that in Example 41.
  • the glass substrate was not heated during the formation of the first functional layer. Instead, the glass substrate was heated to 600 ° C. after all layers were formed.
  • Example 43 A laminated film was produced by forming a laminated film on one surface of the glass substrate by the following method.
  • soda lime glass having dimensions of 100 mm long ⁇ 100 mm wide ⁇ 2.8 mm thick was used.
  • the configuration of the laminated film was a four-layer structure of second functional layer / first dielectric layer / first functional layer / second dielectric layer from the side close to the glass substrate.
  • the second functional layer was tin-doped indium oxide (target film thickness 55 nm).
  • the first dielectric layer was silicon nitride containing aluminum (target film thickness 13 nm).
  • the first functional layer was ZrN x (target film thickness 20 nm), and the second dielectric layer was silicon nitride containing aluminum (target film thickness 54 nm).
  • These layers were all formed by sputtering. More specifically, an ITO target was used for forming the second functional layer.
  • the pressure during film formation was 0.4 Pa.
  • the pressure during film formation was 0.26 Pa.
  • the pressure during film formation was 0.4 Pa.
  • a heat treatment at 300 ° C. was performed for 2 hours after all layers of the sex film.
  • film laminate according to Example 43 a film laminate (hereinafter referred to as “film laminate according to Example 43”) was manufactured.
  • Example 44 A film laminate (hereinafter referred to as “film laminate according to Example 44”) was produced in the same manner as in Example 43 described above.
  • Example 44 the thickness of each layer was changed from that in Example 43.
  • Zr 3 N 4 target film thickness: 5 nm
  • the glass substrate was heated to 600 ° C. after the formation of all the layers was completed.
  • Example 51 to Example 52 A film stack (referred to as “film stacks according to Examples 51 to 52”) was manufactured in the same manner as in Example 31.
  • Example 51 to 52 the thickness of each layer was changed from that in Example 31.
  • the glass substrate was not heated during the formation of the first functional layer. Further, the heat treatment was not performed after the second dielectric layer was formed.
  • Example 53 to Example 54 A film stack (referred to as “film stacks according to Examples 53 to 54”) was produced in the same manner as in Example 31.
  • Example 53 to 54 the thickness of each layer was changed from that in Example 31.
  • the glass substrate was not heated during the formation of the first functional layer. Further, the heat treatment was not performed after the second dielectric layer was formed.
  • Example 55 A laminated film was produced by forming a laminated film on one surface of the glass substrate by the following method.
  • soda lime glass having dimensions of 100 mm long ⁇ 100 mm wide ⁇ 2.8 mm thick was used.
  • the configuration of the laminated film was configured as a third dielectric layer / second functional layer / first dielectric layer / first functional layer / second dielectric layer from the side close to the glass substrate.
  • the third dielectric layer was silicon nitride containing aluminum (target film thickness 40 nm).
  • the second functional layer was niobium nitride (target film thickness 12 nm).
  • the second dielectric layer was silicon nitride containing aluminum (target film thickness 80 nm).
  • the first functional layer was niobium nitride (target film thickness 13 nm), and the second dielectric layer was silicon nitride containing aluminum (target film thickness 35 nm).
  • the pressure during film formation was 0.25 Pa.
  • the pressure during film formation was 0.4 Pa.
  • the pressure during film formation was 0.4 Pa.
  • film laminate according to Example 55 a film laminate (hereinafter referred to as “film laminate according to Example 55”) was produced.
  • Table 1 below summarizes the structure and layer thickness of the film stack according to each example.
  • Zr: N ratio Zirconium nitride ZrN constituting the first functional layer using the film laminates according to Example 4 to Example 9, Example 21 to Example 24, Example 34 to Example 39, Example 42 to Example 44, and Example 51 to Example 54
  • the element ratio of Zr and N in x was measured using Rutherford Backscattering Spectrometry (RBS).
  • the refractive index n of the first functional layer at a wavelength of 500 nm and the extinction coefficient k at a wavelength of 1500 nm were determined as follows. About each laminated body, the spectrum was measured using the spectrophotometer (U-4100: made by Hitachi), and the polarization information was measured using the spectroscopic ellipsometer (M-2000: made by JA Woollam). . Using the obtained spectral transmission and reflection spectra and polarization information, fitting of the optical model was performed to determine the refractive index n and the extinction coefficient k.
  • the visible light transmittance Tv is calculated in accordance with JIS R3106 using the measured spectral transmission spectrum, and the emissivity is calculated using an emissivity measuring machine (TSS-5X: manufactured by Japan Sensor). Measured and calculated the solar heat gain rate g according to ISO 9050.
  • selectivity Se was calculated according to the above-mentioned equation (1).
  • Table 2 below collectively shows the evaluation results obtained for the film stacks according to the respective examples.
  • the first functional layers according to Examples 21 to 26 and Examples 51 to 55 have a light refractive index n of 1.2 or more at a wavelength of 500 nm, and an extinction coefficient of light at a wavelength of 1500 nm. k is less than 6.
  • the first functional layer ZrN x according to Examples 1 to 9, 31 to 39, and 41 to 44 has a light refractive index n of less than 1.2 at a wavelength of 500 nm, and the wavelength of the light The extinction coefficient k at 1500 nm is larger than 6.
  • FIG. 3 shows the relationship between the visible light transmittance Tv (%) and the solar heat gain rate g (%) obtained in the film laminate according to each example.
  • FIG. 3 shows that Tv / g ⁇ 1.1 in the film laminates according to Examples 21 to 26 and Examples 51 to 55.
  • the relationship of Tv / g ⁇ 1.1 is satisfied, and high permeability and good heat shielding properties are satisfied. It was found to have both.
  • a film was formed.
  • the film formation conditions for the ZrN x layer are the same as in the case of Example 1 described above.
  • the film forming conditions of the NiCr layer / Ag layer / NiCr layer are the same as in the case of Example 42 described above.
  • the film laminate was immersed in water using an Eriksen tester (model 494 tester: manufactured by Eriksen).
  • an abrasive (Scotch Bright # 7448B: manufactured by Sumitomo 3M Limited) was brought into contact with the laminated film side of the film laminated body.
  • the abrasive has a dimension of 90 mm ⁇ 40 mm.
  • a load of 324 g was applied to the abrasive, and the abrasive was reciprocated 1000 times on the laminated film.
  • the film laminate was collected, and the state of the laminate film was observed from the surface side with an optical microscope. The observation location was a 5 mm ⁇ 5 mm region in the approximate center of the membrane laminate.
  • Table 3 below shows the evaluation results of the mechanical durability of each of the film laminates A to C.
  • the film laminates A and B having the ZrN x layer as the functional layer exhibit better mechanical durability than the film laminate C having the silver layer as the functional layer.
  • the sweat resistance test was performed by a method according to ISO12870.
  • Artificial sweat was injected into a sealed container.
  • Artificial sweat contains 50 g / L of lactic acid and 100 g / L of sodium chloride.
  • Membrane laminates A to C were introduced into this sealed container while being separated from the artificial sweat.
  • the sealed container was sealed and kept for one day with the inside maintained at 55 ° C. ⁇ 5 ° C. Thereafter, the film laminates A to C were taken out from the sealed container and visually observed for appearance.
  • Each film laminate was immersed in a 1N NaOH solution at 23 ° C. for 6 hours.
  • the membrane laminate was washed with pure water and then immersed in a 1N HCl solution at 23 ° C. for 6 hours. Thereafter, the membrane laminate was washed with pure water and visually observed for appearance.
  • Each film laminate was held for 2 weeks in a constant temperature and humidity tester (KCH-1000: manufactured by Tokyo Rika Kikai Co., Ltd.) set to a temperature of 60 ° C. and a humidity of 95% RH. Then, the film
  • KCH-1000 manufactured by Tokyo Rika Kikai Co., Ltd.
  • Table 4 summarizes the chemical durability evaluation results for each of the film laminates A to C.
  • the film laminates A and B having the ZrN x layer as the functional layer exhibit better chemical durability than the film laminate C having the silver layer as the functional layer.
  • Example 56 A laminated film was produced by forming a laminated film on one surface of the glass substrate by the following method.
  • soda lime glass having dimensions of 100 mm long ⁇ 100 mm wide ⁇ 2.8 mm thick was used.
  • the laminated film has a structure in which the third dielectric layer (including the upper region) / second functional layer / first dielectric layer (including the upper region) / first functional layer from the side close to the glass substrate. / The structure of the second dielectric layer.
  • the first functional layer was ZrN x (film thickness 20 nm), and the second functional layer was ZrN x (film thickness 21 nm).
  • the pressure during film formation was 0.26 Pa. Note that the glass substrate was not heated during the formation of any functional layer.
  • the first dielectric layer was aluminum-containing silicon nitride (film thickness 80 nm) having an upper region (film thickness 10 nm) made of ZrN x (x> 1.2).
  • the second dielectric layer was aluminum-containing silicon nitride (film thickness 80 nm).
  • the third dielectric layer was aluminum-containing silicon nitride (film thickness 25 nm) having an upper region (film thickness 5 nm) made of ZrN x (x> 1.2).
  • the following two stages of processing were performed for forming the first dielectric layer.
  • an aluminum-containing silicon nitride film was formed using a Si-10 wt% Al target.
  • an upper region was formed on the aluminum-containing silicon nitride film.
  • a Zr target was used for film formation in the upper region, and nitrogen gas (100 sccm) was used as the discharge gas.
  • the pressure during film formation was 0.5 Pa.
  • the third dielectric layer was formed in the same manner.
  • the second dielectric layer was formed using a Si-10 wt% Al target.
  • film laminate according to Example 56 a film laminate (hereinafter referred to as “film laminate according to Example 56”) was produced.
  • Example 57 to Example 58 A film stack (referred to as “film stack according to example 57” and “film stack according to example 58”) was manufactured in the same manner as in example 56.
  • Example 59 A laminated film was produced by forming a laminated film on one surface of the glass substrate by the following method.
  • soda lime glass having dimensions of 100 mm long ⁇ 100 mm wide ⁇ 2.8 mm thick was used.
  • the structure of the laminated film is as follows: third dielectric layer / second functional layer / first dielectric layer (including upper region) / first functional layer / second dielectric from the side close to the glass substrate Layered structure.
  • the first functional layer was ZrN x (film thickness 13 nm), and the second functional layer was ZrN x (film thickness 15 nm).
  • the pressure during film formation was 0.26 Pa. Note that the glass substrate was not heated during the formation of any functional layer.
  • the first dielectric layer was aluminum-containing silicon nitride (film thickness 96 nm) having an upper region (film thickness 5 nm) made of NbN x .
  • the second dielectric layer was aluminum-containing silicon nitride (film thickness 42 nm).
  • the third dielectric layer was aluminum-containing silicon nitride (film thickness 10 nm).
  • the following two stages of processing were performed for forming the first dielectric layer.
  • an aluminum-containing silicon nitride film was formed using a Si-10 wt% Al target.
  • an upper region was formed on the aluminum-containing silicon nitride film.
  • An Nb target was used for film formation in the upper region, and nitrogen gas (80 sccm) was used as the discharge gas.
  • the pressure during film formation was 0.4 Pa.
  • the second and third dielectric layers were formed using a Si-10 wt% Al target.
  • film laminate according to Example 59 a film laminate (hereinafter referred to as “film laminate according to Example 59”) was manufactured.
  • Example 60 A film stack (referred to as “film stack according to Example 60”) was produced in the same manner as in Example 59.
  • Example 60 the thickness of each layer was changed from that in Example 59.
  • Example 61 A film laminate (referred to as “film laminate according to Example 61”) was produced in the same manner as in Example 56.
  • Example 61 the upper region of the upper region, and a third dielectric layer of the first dielectric layer are all set to TiN x.
  • Example 61 the thickness of each layer was changed from that in Example 56.
  • a Ti target was used, and nitrogen gas (80 sccm) was used as the discharge gas.
  • the pressure during film formation was 0.4 Pa.
  • the upper region of the third dielectric layer was also formed by the same method.
  • Example 62 A film stack (referred to as “film stack according to Example 62”) was manufactured in the same manner as in Example 61.
  • Example 62 the thickness of each layer was changed from that in Example 61.
  • Example 63 A film laminate (referred to as “a film laminate according to Example 63”) was produced in the same manner as in Example 61.
  • Example 64 A film laminate (referred to as “a film laminate according to Example 64”) was produced in the same manner as in Example 63.
  • Example 64 the thickness of each layer was changed from that in Example 63.
  • Example 65 to Example 67 The film stacks according to Example 65, Example 66, and Example 67 were produced by the same method as the film stacks according to Example 37, Example 38, and Example 39, respectively.
  • Table 5 below summarizes the configuration and layer thickness of the film stack according to each example.
  • an in-plane XRD apparatus (ATX-G manufactured by Rigaku Corporation: radiation source CuK ⁇ ) was used.
  • the measurement conditions are as follows: CuCu removal with a multilayer mirror; 2 ⁇ / ⁇ scan in the in-plane direction with a constant incident angle; Incident angle 0.5 degree; X-ray divergence angle in the in-plane direction is 0.5 degrees (limited by slit).
  • the orientation index P was calculated from the obtained in-plane X-ray diffraction result using the above-described equation (3).
  • Table 7 below collectively shows the orientation index P obtained in the film laminates according to Examples 56 to 67.
  • the orientation index P of the first functional layer is about 1.35. I found out that it was not so big. In contrast, in the film stacks according to Examples 56 to 64 in which the first dielectric layer has an upper region made of the crystallinity improving material, the orientation index P of the first functional layer may exceed at least 2. all right.
  • FIG. 4 also shows the in-plane X-ray diffraction results of the first functional layer obtained in the film stacks according to Example 56 and Example 65.
  • the crystallinity of the first functional layer was improved by using the first dielectric layer having the upper region made of the crystallinity improving material.

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  • Geochemistry & Mineralogy (AREA)
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Abstract

Dans un empilement de films qui comprend un film stratifié sur un substrat transparent, le film stratifié comprend une ou plusieurs couche(s) fonctionnelle(s) et une première partie, cette dernière comprenant une série de parties qui comprennent une première couche diélectrique, une première couche fonctionnelle sur la première couche diélectrique et une seconde couche diélectrique sur la couche fonctionnelle. La première couche fonctionnelle est la couche fonctionnelle sur le côté le plus éloigné du substrat transparent de la ou des couche(s) fonctionnelle(s). La première couche fonctionnelle est composée de ZrNx, et présente un indice de réfraction n inférieur à 1,2 à une longueur d'onde de 500 nm et un coefficient d'extinction k de plus de 6 à une longueur d'onde de 1500 nm. Dans l'empilement de films, une sélectivité Se représentée par Tv/g satisfait 1,1 ≤ Se, où la transmission de lumière visible est Tv (%) et un coefficient de gain de chaleur solaire est g (%).
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WO2019181421A1 (fr) * 2018-03-20 2019-09-26 Ａｇｃ株式会社 Substrat de verre à films stratifiés et verre à vitre
JPWO2019181421A1 (ja) * 2018-03-20 2021-03-18 Ａｇｃ株式会社 積層膜付きガラス基板及び窓ガラス
WO2021014977A1 (fr) * 2019-07-25 2021-01-28 Ａｇｃ株式会社 Corps en couches et procédé de production de corps en couches
EP4005790A4 (fr) * 2019-07-25 2023-08-02 Agc Inc. Corps en couches et procédé de production de corps en couches
JP7476898B2 (ja) 2019-07-25 2024-05-01 Ａｇｃ株式会社 積層体および積層体の製造方法

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