WO2008018298A1 - FILM RÉFLÉCHISSANT EN ALLIAGE D'Ag POUR RÉFLECTEUR, RÉFLECTEUR, ET CIBLE DE PULVÉRISATION EN ALLIAGE D'Ag POUR LA FORMATION DU FILM RÉFLÉCHISSANT EN ALLIAGE D'Ag POUR RÉFLECTEUR - Google Patents

FILM RÉFLÉCHISSANT EN ALLIAGE D'Ag POUR RÉFLECTEUR, RÉFLECTEUR, ET CIBLE DE PULVÉRISATION EN ALLIAGE D'Ag POUR LA FORMATION DU FILM RÉFLÉCHISSANT EN ALLIAGE D'Ag POUR RÉFLECTEUR Download PDF

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Publication number
WO2008018298A1
WO2008018298A1 PCT/JP2007/064653 JP2007064653W WO2008018298A1 WO 2008018298 A1 WO2008018298 A1 WO 2008018298A1 JP 2007064653 W JP2007064653 W JP 2007064653W WO 2008018298 A1 WO2008018298 A1 WO 2008018298A1
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WO
WIPO (PCT)
Prior art keywords
reflective film
alloy
reflector
alloy reflective
film
Prior art date
Application number
PCT/JP2007/064653
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English (en)
Japanese (ja)
Inventor
Jun Suzuki
Toshiki Sato
Takao Kawanaka
Original Assignee
Kabushiki Kaisha Kobe Seiko Sho
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 Kabushiki Kaisha Kobe Seiko Sho filed Critical Kabushiki Kaisha Kobe Seiko Sho
Publication of WO2008018298A1 publication Critical patent/WO2008018298A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/08—Mirrors
    • G02B5/0808—Mirrors having a single reflecting layer

Definitions

  • the present invention belongs to a technical field relating to an Ag alloy reflective film for a reflector, a reflector, and an Ag alloy sputtering target for forming an Ag alloy reflective film for a reflector.
  • automotive lamps and lighting equipment are required to have high heat resistance because they are exposed to a temperature environment of about 100 to 200 ° C. by heat emitted from a light emitter. Furthermore, durability in a high temperature and high humidity environment is required.
  • the Ag thin film is not sufficiently durable to the environment, it has been difficult to use it for a long time due to deterioration due to moisture or the like. For this reason, attempts have been made to prevent deterioration of the Ag thin film by forming a UV curable resin, acrylic resin, or ceramic protective film on the Ag thin film.
  • these methods not only increase the cost, but the protective film of the resin is inferior in barrier properties, and the ceramic protective film infiltrates moisture from a defect such as a pinhole or a crack. Therefore, it has been difficult to obtain sufficient durability.
  • Ag thin films easily aggregate due to heat, it was difficult to use them in a high temperature environment.
  • Japanese Patent Laid-Open No. 9-135096 proposes a technique in which 3 atomic% of one or more elements of Pd, Cu, Au, Ni, Zn, Cd, Mg, and Al are added to Ag. In the 2001-226765 publication, it is proposed to add 0.1 to 3 atomic% of Pd, Cu, Au to Ag to improve durability.
  • Patent Document 1 Japanese Patent Laid-Open No. 2000-106017
  • Patent Document 2 Japanese Patent Laid-Open No. 9-135096
  • Patent Document 3 Japanese Patent Laid-Open No. 2001-226765
  • the reflective film of the reflector is required to have high reflectivity and durability against humidity, heat, and the like.
  • the present invention has been made by paying attention to such a situation, and an object of the present invention is to provide an Ag alloy reflective film for a reflector and a refractor which is difficult to cause aggregation of Ag due to humidity and heat having high reflectivity.
  • the present invention which has been completed in this way and has achieved the above object, is an Ag alloy reflecting film for a reflector, a reflector, and an Ag alloy sputtering target for forming an Ag alloy reflecting film for a reflector.
  • the reflector alloy film for reflectors according to claim 1 to claim 4 (Ag alloy reflector film for reflector according to the first to fourth inventions), the Ag alloy reflector film for reflectors according to claims 5 to 6
  • An Ag alloy sputtering target for forming (a sputtering target according to the fifth to sixth inventions) and a reflector according to claim 7 (the reflector according to the seventh invention), which has the following configuration.
  • the Ag alloy reflective film for a reflector according to claim 1 is an Ag alloy reflective film for a reflector, comprising Ag as a main component and selected from Ti, V, Cr, Mn, Mg, and W.
  • the Ag alloy reflective film for a reflector is characterized by containing a total of more than 3 atom% and not more than 7 atom% [first invention].
  • the Ag alloy reflective film for a reflector according to claim 2, wherein the Ag alloy reflective film for a reflector according to claim 1 contains a total of 0.3 to 2 atomic% of at least one selected from Au, Pt, Pd, and Cu. It is a reflective film [second invention].
  • the Ag alloy reflective film for reflector according to claim 3 is an Ag alloy reflective film for reflector according to claim 1 or 2, wherein the reflectance measured by light having a wavelength of 650 nm is 85% or more. 3 inventions].
  • the Ag alloy reflective film for reflector according to claim 4 is the Ag alloy reflective film for reflector according to any one of claims 1 to 3, which is formed by a sputtering method [fourth invention].
  • the Ag alloy sputtering target for forming an Ag alloy reflective film for a reflector according to claim 5 is mainly composed of Ag, and includes at least one selected from Ti, V, Cr, Mn, Mg, and W.
  • Claim 6. The reflector according to claim 6, wherein the Ag alloy sputtering target for forming an Ag alloy reflective film contains at least one selected from Au, Pt, Pd, and Cu in a total amount of 0.3 to 2 atomic%. 5.
  • a reflector according to claim 7 is a reflector having the Ag alloy reflective film according to any one of claims 1 to 4! [Seventh invention].
  • the Ag alloy reflective film for a reflector according to the present invention hardly causes aggregation of Ag due to humidity or heat having high reflectivity. Therefore, it can be suitably used as an Ag alloy reflecting film for a reflector, and its function and durability can be improved. Since the reflector according to the present invention is provided with such an Ag alloy reflective film, Ag aggregation due to humidity and heat with high reflectivity is difficult to occur, and the function and durability of the reflector are improved. Is peeled off. According to the Ag alloy sputtering target for forming an Ag alloy reflective film for a reflector according to the present invention, an Ag alloy reflective film can be formed.
  • the inventors put metal plates of various elements on an Ag target, produced Ag alloy thin films of various components' composition by sputtering, and determined the composition and characteristics as a reflective film. evaluated.
  • This property evaluation method can be performed after a high-temperature and high-humidity test (left for 1000 hours in an atmosphere of 60 ° C and 90% humidity), or a salt water immersion test [concentration O. Olmol / liter (hereinafter referred to as L After that, the reflective film was evaluated for the occurrence of white turbidity and white spots, and the change in reflectance was investigated.
  • an Ag alloy reflective film in which one or more selected from Ti, V, Cr, Mn, Mg, and W is added to Ag is more turbid than pure Ag thin film. It was found that the generation of white spots was significantly suppressed and the decrease in reflectance was small. As described above, white turbidity and white spots are generated by aggregation of Ag due to humidity and heat, and the Ag alloy reflective film can be said to have excellent durability.
  • the effect of improving the durability due to the addition of one or more selected from Ti, V, Cr, Mn, Mg, and W varies depending on the amount of addition of this element. It is desirable to have it.
  • the total amount of elements added is 3 atomic% or less, the Ag aggregation suppressing effect is small and the required durability cannot be obtained.
  • the added amount of this element increases and exceeds 7 atomic%, the reflectivity decreases and the function as a reflective film is lost. From this point, the addition amount of the above elements for maintaining durability and performance as a reflective film is preferably more than 3 atomic% and 7 atomic% or less, and more preferably 3.5 to 5 atomic%. Is more preferable.
  • the Ag alloy reflective film for a reflector according to the present invention contains Ag as a main component, and one or more selected from Ti, V, Cr, Mn, Mg, and W in total exceeds 3 atomic%. It is characterized by containing not more than atomic% [first invention].
  • the Ag alloy reflective film for a reflector according to the present invention further contains at least one selected from Au, Pt, Pd, and Cu in a total amount of 0.3 to 2 atomic%.
  • Au, Pt, Pd, and Cu in a total amount of 0.3 to 2 atomic%.
  • the Ag alloy reflective film for a reflector according to the present invention has a reflectance measured by light having a wavelength of 650 nm of 85% or more, and can be suitably used as a reflector film for a reflector [Third Invention].
  • A1 thin film is used for the conventional reflective film for reflectors, and the wavelength is 650nm.
  • the reflectance measured by the light is around 85%.
  • the A1 thin film is very weak against acids and alkalis, it is essential to coat a protective layer of a transparent resin on the A1 reflective film. Since the formation of this protective layer is expensive, there is a need for a reflective film that can be used for a long time without providing a protective layer.
  • the Ag alloy reflective film for a reflector according to the present invention is a reflective film made of an Ag alloy that is stable against acids and alkalis, and has excellent durability, so a protective layer such as a resin is not required! / Because of this, the cost merit is great.
  • the Ag alloy reflective film for a reflector according to the present invention is formed (deposited) by a sputtering method! /, [Fourth Invention]. This is because the Ag alloy reflective film formed by sputtering is dense and excellent in adhesion!
  • the thickness of the Ag alloy reflective film for a reflector according to the present invention is preferably in the range of 70 nm to 300 nm, more preferably in the range of 100 nm to 200 nm.
  • the Ag alloy reflective film for a reflector according to the present invention hardly causes aggregation of Ag due to humidity or heat with high reflectivity. Therefore, it can be suitably used as an Ag alloy reflecting film for a reflector, and its function and durability can be improved.
  • the reflector according to the present invention is provided with such an Ag alloy reflective film. Therefore, Ag aggregation due to humidity or heat with high reflectivity is unlikely to occur, and the function of the reflector is improved. And improved durability [seventh invention].
  • the Ag alloy reflective film is formed on a base material made of resin or the like.
  • An Ag alloy sputtering target for forming an Ag alloy reflective film for a reflector according to the present invention contains Ag as a main component and a total of one or more selected from Ti, V, Cr, Mn, Mg, and W.
  • an Ag alloy sputtering target for forming an Ag alloy reflective film for a reflector according to the present invention further containing at least one selected from Au, Pt, Pd, and Cu in an amount of 0.3 to 2 atomic% Can form an Ag alloy reflective film for an optical information recording medium according to the second invention of the present invention [Sixth Invention].
  • Example [0026] Examples and comparative examples of the present invention will be described below. It should be noted that the present invention is not limited to these examples, and can be implemented with appropriate modifications within a range that can be adapted to the gist of the present invention, all of which fall within the technical scope of the present invention. included.
  • an Ag alloy thin film having a thickness of 120 nm was formed on a glass substrate (Counging # 1737) having a diameter of 50 mm and a thickness of 0.7 mm.
  • the sputtering target used was an Ag target (diameter 101.6 mm, thickness 5 mm) on which metal chips of various additive elements were placed.
  • Deposition conditions are: substrate temperature: room temperature, Ar gas pressure:;! ⁇ 3m Torr (0.13-0.40Pa), distance between electrodes: 55mm, sputtering power: DC 580W, film formation speed: 5-6 nm / sec film before ultimate vacuum: 3.0 was X 10- 6 ⁇ (4 ⁇ 0 X 10- 4 Pa).
  • the content of the additive element was measured by ICP emission spectroscopic analysis. In addition, a durability evaluation test was performed.
  • the durability evaluation test was performed by a high temperature and high humidity test and a salt water immersion test.
  • the surface of the Ag alloy thin film was visually observed after being left for 1000 hours in an atmosphere at a temperature of 60 ° C and a humidity of 90% RH, and the occurrence of white turbidity and white spots on the film was evaluated.
  • the salt water immersion test the sample was immersed in an aqueous solution of NaCl with a concentration of O. Olmol / L for 1 hour, washed in pure water, and the surface of the Ag alloy thin film was visually observed to evaluate the occurrence of white turbidity and white spots on the film. went.
  • the reflectance before and after the high temperature and high humidity test was measured. At this time, light having a wavelength of 650 nm was used as incident light, and the reflectance was measured.
  • Table 1 shows the results of measurement of the content of the additive element, durability evaluation test, and reflectance measurement.
  • each mark in the Ag Aggregation Status column indicates the occurrence of white turbidity and white spots, “ ⁇ ” indicates the absence of white turbidity and white spots, and “ ⁇ ” indicates some.
  • “X” in the column after the salt water immersion test includes a state in which the film peeling is remarkable.
  • the samples No. l, 2, 10 had a very high initial reflectivity (reflectance before the high-temperature and high-humidity test) of 91.7 to 96.2%.
  • High humidity test and salt water immersion test Many white turbidity and white spots were generated after the test, and the reflectivity was greatly reduced by the high temperature and high humidity test.
  • the reflectivity after the high temperature and high humidity test was lower than 85%.
  • the Ag alloy thin films of ⁇ ⁇ 3 to 5, 7, 8, 11 to 14, 16 to 19 have an initial reflectivity of 87 to 95%, Even after the humidity test and the salt water immersion test, the reflectance decreases due to the high-temperature and high-humidity test where no white turbidity or white spots are generated on the film surface. Therefore, the durability is good and the film has sufficient performance as a reflective film.
  • the Ag alloy thin film of the present invention has a sufficiently high initial reflectivity, and Ag aggregation is hardly caused by the high-temperature and high-humidity test and the salt water immersion test. Since the decrease is slight, it can be suitably used as a reflective film for a reflector.
  • an Ag alloy thin film having a thickness of 120 nm was formed on the same glass substrate under the same conditions.
  • one type of metal chip selected from Ti, V, Cr, and Mn and one type of metal chip selected from Au, Pt, Pd, and Cu are simultaneously placed on the Ag target.
  • a ternary Ag alloy thin film was deposited.
  • the content of the additive element was measured by ICP emission spectrometry.
  • a high-temperature and high-humidity test was performed under the same conditions (atmosphere and test time) as in Example 1, and durability was evaluated by the change in reflectance before and after the test.
  • Table 2 shows the measurement results of the content of the above-mentioned additive elements and the reflectance measurement results before and after the high-temperature and high-humidity test.
  • the reflectance before high-temperature and high-humidity test is slightly reduced by adding Au, Pt, Pd, and Cu to Ag-Ti, Ag-V, Ag-Cr, and Ti-Mn, respectively.
  • the decrease in reflectivity after the high temperature and high humidity test is clearly suppressed. No.32, 34, 37
  • the initial reflectivity is lower than 85% when the amount of Au added is large (over 2 atomic%).
  • the Ag alloy reflective film for a reflector according to the present invention is less likely to cause aggregation of Ag due to humidity or heat having a high reflectivity, and can be suitably used as an Ag alloy reflective film for a reflector. .

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Physical Vapour Deposition (AREA)
  • Optical Elements Other Than Lenses (AREA)

Abstract

La présente invention concerne : un film réfléchissant en alliage d'Ag pour une utilisation dans la formation d'un réflecteur qui présente une réflectivité élevée et entraîne très peu de coagulation de l'Ag par humidité ou chaleur ; un réflecteur ; et une cible de pulvérisation en alliage d'Ag pour une utilisation dans la formation d'un film réfléchissant en alliage d'Ag pour réflecteur. (1) L'invention concerne un film réfléchissant en alliage d'Ag pour réflecteur, qui comprend de l'Ag en tant qu'ingrédient principal et un ou plusieurs éléments choisis parmi Ti, V, Cr, Mn, Mg et W en une quantité totale supérieure à 3 % atomique et non supérieure à 7 % atomique. (2) Le film réfléchissant en alliage d'Ag peut contenir un ou plusieurs éléments choisis parmi Au, Pt, Pd et Cu en une quantité totale de 0,3 à 2 % atomique. (3) Le film réfléchissant en alliage d'Ag peut avoir une réflectivité supérieure ou égale à 85 % mesurée avec une lumière ayant une longueur d'onde de 650 nm. (4) Le film réfléchissant en alliage d'Ag peut être formé par un procédé de pulvérisation. (5) L'invention concerne également un réflecteur ayant le film réfléchissant en alliage d'Ag. (6) L'invention concerne en outre une cible pour une utilisation dans la formation d'un film réfléchissant en alliage d'Ag.
PCT/JP2007/064653 2006-08-10 2007-07-26 FILM RÉFLÉCHISSANT EN ALLIAGE D'Ag POUR RÉFLECTEUR, RÉFLECTEUR, ET CIBLE DE PULVÉRISATION EN ALLIAGE D'Ag POUR LA FORMATION DU FILM RÉFLÉCHISSANT EN ALLIAGE D'Ag POUR RÉFLECTEUR WO2008018298A1 (fr)

Applications Claiming Priority (2)

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JP2006-218593 2006-08-10
JP2006218593A JP2008046149A (ja) 2006-08-10 2006-08-10 リフレクター用Ａｇ合金反射膜、リフレクター、および、リフレクター用Ａｇ合金反射膜の形成用のＡｇ合金スパッタリングターゲット

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1152366A (ja) * 1997-08-04 1999-02-26 Toppan Printing Co Ltd 半透過型液晶表示装置
JP2001226765A (ja) * 1999-12-07 2001-08-21 Furuya Kinzoku:Kk 高耐熱性反射膜及びこの反射膜を用いた積層体
JP2002129314A (ja) * 2000-10-31 2002-05-09 Furuya Kinzoku:Kk スパッタリングターゲット及びその製造方法、反射型ｌｃｄ用反射板、反射配線電極、薄膜及びその製造方法
JP2002226927A (ja) * 2001-01-31 2002-08-14 Hitachi Metals Ltd 平面表示装置用Ａｇ合金系反射膜
JP2004272245A (ja) * 2003-02-21 2004-09-30 Mitsui Chemicals Inc 反射体

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1152366A (ja) * 1997-08-04 1999-02-26 Toppan Printing Co Ltd 半透過型液晶表示装置
JP2001226765A (ja) * 1999-12-07 2001-08-21 Furuya Kinzoku:Kk 高耐熱性反射膜及びこの反射膜を用いた積層体
JP2002129314A (ja) * 2000-10-31 2002-05-09 Furuya Kinzoku:Kk スパッタリングターゲット及びその製造方法、反射型ｌｃｄ用反射板、反射配線電極、薄膜及びその製造方法
JP2002226927A (ja) * 2001-01-31 2002-08-14 Hitachi Metals Ltd 平面表示装置用Ａｇ合金系反射膜
JP2004272245A (ja) * 2003-02-21 2004-09-30 Mitsui Chemicals Inc 反射体

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