• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The present invention relates to a mirror comprising a transparent substrate, at least one metal reflective layer and at least one protective paint layer on the back of the mirror, which comprises an overcoating barrier to corrosive elements, such as sulphides and / or chlorides. a thickness of less than or equal to 6 μm and located on the protective layer. The method of manufacturing such a mirror is also described.
    公开号:FR3037060A1
    申请号:FR1555007
    申请日:2015-06-02
    公开日:2016-12-09
    发明作者:Guillaume Lequippe
    申请人:Saint Gobain Glass France SAS；
    IPC主号:
    专利说明:

    [0001] The invention relates to a mirror having improved durability, as well as to its manufacturing method. The mirrors generally comprise a glass substrate on which a metallic reflective layer has been deposited. This reflective layer is most often silver or aluminum and tends to corrode in the air due to the presence of pollutants in the atmosphere. It is therefore essential to protect it to increase the durability of the mirrors. In silver mirrors, a tin treatment is often carried out after silvering, in order to partly promote the adhesion of the upper layers and secondly to potentially improve the resistance to corrosion. money. One or more protective layers, for example based on copper or based on paints, are then deposited on the silver substrate. For example, patent application FR 2 936 340 describes a mirror comprising a protective coating combining two successive layers of paints of different types. These paints can be of organic type or of inorganic type, solvent or aqueous. Typically, the total thickness of this paint-protecting layer when dry is about 50 μm. This thickness makes it possible in particular to ensure the protection against corrosion and therefore improves the durability of the mirror. The paint also makes it possible to obtain the opacity in the rear face of the mirror, sought especially for interior mirrors. The choice or development of the paints and the mirror manufacturing processes make it possible to guarantee a protection against corrosion that meets the thresholds imposed by the European standard EN ISD 1036. The mirrors obtained have, in particular, acceptable values during tests carried out in a copper medium. acetic acid (also known as CASS test or Saline Cupro Acetic mist described in EN ISD 9227). However, it is sought to further improve the durability of the mirrors, especially in real conditions of chemical stresses, especially in the presence of sulfurous corrosion and / or chloride corrosion, while maintaining production costs comparable to solutions currently on the market. This is the context of the present invention. The inventors have surprisingly discovered that it is possible to very significantly improve the durability of mirrors and in particular their resistance to sulphide and chloride corrosion by depositing a thin overlay directly on the protective layer of paint. , thus making it more compact by closing the open porosity or opening on the surface.
    [0002] The present invention relates to a mirror comprising a transparent substrate, at least one metal reflective layer and at least one protective paint layer on the back of the mirror, said mirror comprising an overcoating barrier to corrosive elements, such as sulphides and / or chlorides less than 6 μm thick and located on the protective layer.
    [0003] Preferably, the thickness of the barrier overcoat is less than or equal to 3 μm and even more preferably it is less than or equal to -Ipm. The thickness of the overlayer is advantageously as low as possible. This overlayer is directly positioned on the protective layer placed on the back of the mirror that is to say on the paint layer. Because of its constitution, since the paint is a mixture of different fillers by nature and particle size distribution, the paint has a natural porosity in the microscopic state. This porosity can constitute points of entry for the corrosive elements and thus open preferential channels of diffusion of these species. The overcoat deposited on the paint-protecting layer advantageously makes it possible to close the porosity of the paint layer and thus to limit or even eliminate routes of diffusion of corrosive species. The durability of the mirrors comprising the overcoat placed on the protective layer of paint is thus significantly improved. The barrier overlay may be a layer of uniform thickness. Its thickness is thus regular and identical over the entire rear face of the mirror. 01 can then also talk about continuous overlay. The barrier overlay may also be a discontinuous layer, the thickness of which may not be uniform. It is essential that this overlayer block the existing porosity in the paint-protecting layer, without necessarily having a uniform thickness. The overlay barrier is the outermost layer located at the back of the mirror. This is the layer in contact with the ambient air. This overlay is a resin. Preferably, this resin is organic. Examples include 3037060 3 acrylic, vinyl, polyurethane, polyester, epoxy, alkyd or styrene resins. The choice of the material used is guided by the fact that this type of resin preferably belongs to the family of polymers. It is not necessary for the overlay to give the mirror any chemical functionality. The essential role of the overlay is to fill the porous cavities that may exist in the paint protection layer. Preferably, the overlay is based on an alkyd, acrylic, epoxy or polyester resin. Advantageously, the overlay is based on an alkyd resin, acrylic or polyester. The resins may be of the same chemical nature as the organic binders contained in the paint formulations. It is thus possible to choose an overlayer based on a resin identical to the binders contained in the protective layer of paint, which also ensures a good chemical compatibility between the species contained in the protective layer in paint and in the overlay. The paint used to form the protective layer is an aqueous or organic paint. The thickness of this protective layer is at most 100 μm. Preferably, it is at most 50 pm. Its thickness may vary depending on the type of paint used. The role of this protective layer is essentially an optical and mechanical role. It also contributes to improving the durability of the mirror in relation to chemical and corrosive aggression. It is possible to use low-cost paints whose essential function is to ensure the desired opacity in the rear face of the mirror. In order to comply with the EHS standards and in particular the European directive 2004/42 / CE "Decopaint", it is advisable to use paints containing less than 130g / L of organic solvents, thus limiting the emission of organic compounds 25 volatile (VOC) at the place of manufacture. The transparent substrate is generally a sheet of glass, mineral or organic, curved or not. Its thickness varies between 2 and 8 mm. The glass is preferably extra-clear, that is to say having a light transmission greater than 85 ° / 9 or even greater than 89% for a thickness of 3.2 mm. The glass 30 is organic, it may in particular be polycarbonate, polymethyl methacrylate, polyethylene terephthalate or poly (ethylene-co-tetrafluoroethylene). The set of layers constituting the mirror is deposited on the same side of the transparent substrate, the overlayer being the outermost layer of the stack. The metal reflective layer, preferably silver, has a thickness varying between 500 and 1600 mg / m2. For applications as home mirrors, such as bathroom mirrors, a conventional silver layer has a thickness of 700 to 1000 mg / m 2. On the other hand, for applications as solar mirrors in which it is necessary for the maximum of the light of the solar spectrum to be reflected, the silver layer has a thickness of between 900 and 1600 mg / m 2.
    [0004] The reflective layer may also be aluminum for applications as home mirrors. In order to improve the adhesion of the different layers to one another and / or to the substrate, the mirror may comprise a layer of primer, conventionally based on silane. This layer may be deposited between the reflective metal layer and the protective paint layer, between the substrate and the reflective metal layer, or possibly between the paint layer and the barrier overcoat. In the case where an adhesion primer is deposited on the paint layer to improve the adhesion of the overcoat, it is still considered that the corrosive barrier overcoat is located directly on the paint-based protective layer. Indeed, the adhesion primer layer is a very thin layer, very often monoatomic, which does not necessarily by itself to close the porosity of the paint layer. The present invention also relates to the method of manufacturing the mirror described above.
    [0005] The method of manufacturing said mirror comprises: a. an optional sensitization step, b. an optional step of activating the surface of the substrate to be coated, c. a step of depositing at least one reflective metal layer on a transparent substrate, d. a step of depositing at least one paint-protecting layer, e. a step of depositing a barrier overcoat on corrosive species, such as sulphides and chlorides, with a thickness of less than 3037060 by 6 μm on said protective layer making it possible to block the porosity thereof and f. a step of drying said overcoat. As known to those skilled in the art, the manufacture of a mirror comprises several steps before the deposition of the metal reflective layer: the substrate surface is brightened, then one of its faces is sensitized, for example by a solution of stannous chloride. It is then possible to activate this same face with a solution of palladium chloride. These steps are optional in the manufacturing method according to the present invention. The deposition of the reflective metal layer, like silver, is then carried out by techniques known to those skilled in the art. The deposition may be carried out in the vapor phase, in particular by CVD, PVD or magnetron, or by a liquid route, in particular from a silvering solution. The method of manufacturing a mirror according to the present invention comprises an optional sensitization step, an optional step of activating the surface of the substrate to be coated, a step of depositing the reflective metal layer and a step of depositing the protective layer of paint. It further comprises a step of depositing a barrier overcoat on corrosive species, such as sulphides and chlorides, with a thickness of less than 6 μm on said protective layer making it possible to close the surface porosity thereof. then a step of drying said overcoat. The paint-protecting layer can be applied by various techniques: for example, spraying techniques, curtain technique, film-pulling technique, or roller technique. The temperatures and drying times of the paint layer are variable depending on the type of paint used and the thickness of the paint layer. The drying can be carried out under hot air, or by IR 9 baking the paint is crosslinkable to UV, the drying step can be carried out under UV lamps. It is also possible to combine these different drying methods and to carry out the drying step under UV lamps with hot air and IR baking. The step of depositing the barrier overcoat is carried out by liquid spraying, by roller, by dipping, curtain coating or spraying. This depositing step can also be performed by screen printing. The deposition is carried out by methods known to those skilled in the art. It is sometimes necessary for the deposition step to be followed by a dewatering or scraping step making it possible to remove the excess material that may have been deposited during the deposition step of the overlay. The deposition step may also be followed by an air knife passage to remove any excess material. Indeed, the barrier overlay must be as thin as possible and preferably has a thickness of less than 3 μm and even more preferably less than 1 μm. It makes it possible to increase the compactness of the protective layer by painting by closing its open porosity. Thus, when the step of depositing the overlay is carried out by spraying or curtain coating, it is followed by a scraping step so as to obtain the finest possible overlayer. According to some embodiments, the deposition and scraping steps can be performed simultaneously, using a roller whose direction of rotation can vary. The method according to the invention further comprises a step of drying the barrier overcoat which can be carried out in hot air, by IR baking and / or UV. The choice of the drying mode is preferentially according to the type of organic resin used. For example, if the barrier overcoat is based on a resin that is UV curable, the drying step can be performed under UV lamps. Each of steps c) d) and / or e) may be preceded by an optional step of depositing an adhesion primer, for example of the silane type, by any technique known to those skilled in the art.
    [0006] The examples below illustrate the invention without limiting its scope. Examples Samples were prepared and various tests were performed on these samples to verify their durability. A test has been developed to evaluate the resistance of the barrier layer and the protective layer to diffusion paint of sulfur compounds. To carry out this test, the percentage of luminous reflection as a function of time is analyzed on samples whose layer to be analyzed is covered with rubber. The samples on which the rubber is placed are placed in an oven at 130 ° C to accelerate the diffusion process of the sulfur compounds contained in the rubber. Light reflection measurements are then made after 60 and 180 minutes, and the percentage of light reflection loss is estimated with respect to a value measured at T = 0 (before positioning of the rubber). Corrosion tests were carried out according to EN ISD 9227. The thickness measurements of the layers are carried out by measurement methods by micrometric section (Apparatus Paint Borer 518 from Erichsen). The deposited resin thicknesses were measured on a Taylor Hobson 2D / 3D profilometer. The adhesion measurements of the layers are determined by the automated grid apparatus of the Erichsen company (type 430), and correspond to the grid test described in the NF ISD 2409 standard for paints and varnishes. This test consists of a visual interpretation of the surface of the grid on which flaking can occur with a 1 mm comb. The classification is done on a scale of 0 to 5 depending on whether the layer comes off more or less. A value of 0 indicates a very good adhesion of the layer.
    [0007] Various mirrors having a size of 400 mm × 300 mm were prepared by depositing a silver metallic reflective layer with a thickness of about 750 mg / m 2 on a PLANILUX®-type glass substrate, after a step of sensitizing the substrate to the substrate. using a solution based on SiC12. The mirrors 25 comprise a liquid-deposited tin passivation layer of a thickness of about ten nanometers and a silane-based primer layer with a thickness of about 10 nm located between the silver reflective metal layer and the protective layer in paint. Several samples were thus prepared by changing the paints used for the protective layer: paint 1: organic alkyd paint (One Coat LF3 Gray marketed by Fenzi). 3037060 8 -Paint 2: aqueous acrylic paint (WBLF4 LPB Blue 3025 marketed by Fenzi). Two different resins were tested to form the barrier overcoat: 5 - resin A: acrylate resin (G1000UV sold by Henkel) - resin B: melamine alkyd resin corresponding to the binder of the paint One Coat LF3 Gray sold by Fenzi) The resins are applied with the film shooter then are raked. Resin B is dried by being placed in an oven at 180 ° C for 15 minutes to allow its recovery. Resin A is crosslinked under UV for 90 seconds (120 W / cm) The sulfurizing corrosion performance of the various samples was evaluated in oven at 130 ° C. Table 1 below summarizes the percentages of light reflection loss of the different samples tested at 60 minutes and 180 minutes.
    [0008] Sample% loss of reflection% loss of luminous to light reflection at 60 min 180 min IViroir 1 (non-compliant): 83 83 20 pm Paint 1 IViroir 2 according to the invention: 51 80 20 pm of paint 1 covered with 1 μm resin A IViroir 3 according to the invention: 54 80 20 μm of paint 1 covered with 2 μm of resin B IViroir 4 (not in accordance with the invention)> 80> 80 20 μm of paint 2 IViroir 5 (According to the invention) 1 1 20 pm of paint 2 coated with 6 pm of resin A Table 1 Comparing respectively the mirror 1 with the mirrors 2 and 3, then the mirror 4 with the mirror 5, we see that after 60 min, the percentage of decrease is much smaller for the mirrors according to the present invention than for the mirrors not in accordance with the invention. After 180 min, the values obtained for the mirrors of the invention are lower than those of the comparative mirrors. This shows the beneficial effect of the barrier overcoat on the sulphurous corrosion resistance.
    [0009] Table 2 summarizes the results obtained for the various mirrors after a test CASS cycle (120 h at 50 ° C., aqueous solution of 50 g / l of NaCl and 0.26 g / l of anhydrous CuCl 2, the pH being between 3.2 and 3.3).
    [0010] 5 Sample Corrosion at the edges (pm) Corrosion full face IViroir 1 (non conform): very strong Very strong 20 pm paint 1 IViroir 2 according to the invention: 200 Very light 20 pm of paint 1 covered with 1 pm of resin A IViroir 3 according to the invention: 113 average 20 pm of paint 1 covered with 2pm of resin B IViroir 4 (not in accordance with the invention) 750 average 20 pm of paint 2 iviroir 5 (according to the invention) 300 very light 20 pm of paint The results obtained in the CASS tests show that the corrosion is significantly improved when a thin barrier overcoat is applied to the protective paint layer. Indeed, the size of the zone attacked on the edges of the mirror decreases when removing the barrier overlay. The full face corrosion is also improved and becomes very light or medium for the mirrors according to the invention.
    [0011] Adhesion measurements made to the grid test for each of the samples showed that the values obtained were 0 for all the mirrors according to the invention. The barrier overlayer layer thus adheres satisfactorily to the protective layers of paint. To meet the 5 specifications imposed by the ISD 2409 standard, the mirrors must have a score of less than 2 on the adhesion test. All of these measures show a clear improvement in the durability of the mirrors according to the present invention.
    权利要求:
    Claims (16)
    [0001]
    REVENDICATIONS1. Mirror comprising a transparent substrate, at least one metallic reflective layer and at least one protective layer in paint on the back of the mirror, characterized in that it comprises a barrier overcoating for corrosive elements, such as sulphides and / or chlorides, a thickness of less than or equal to 6 μm and located on the protective layer.
    [0002]
    2. Mirror according to claim 1 characterized in that the overlayer has a thickness of less than or equal to 3 μm, preferably less than or equal to 1 μm.
    [0003]
    3. Mirror according to one of the preceding claims characterized in that the overlayer is the outer layer of the mirror, located at the back of the mirror.
    [0004]
    4. Mirror according to one of the preceding claims characterized in that the overlay is an organic resin. 15
    [0005]
    5. Mirror according to claim 4 characterized in that the overlayer is an acrylic resin, vinyl, polyurethane, polyester, epoxy, alkyd or styrene.
    [0006]
    6. Mirror according to one of the preceding claims characterized in that the overlayer is a layer of uniform thickness. 20
    [0007]
    7. Mirror according to one of claims 1 to 5 overlay is a discontinuous layer.
    [0008]
    8. Mirror according to one of the preceding claims characterized in that the protective layer is a layer of paint, aqueous or organic.
    [0009]
    9. Mirror according to one of the preceding claims, characterized in that the thickness of the protective layer is at most 100 μm, preferably at most 50 μm.
    [0010]
    10. Mirror according to one of the preceding claims characterized in that the substrate is made of mineral or organic glass.
    [0011]
    11. Mirror according to one of the preceding claims, characterized in that the metal reflective layer is a silver layer.
    [0012]
    12. A method of manufacturing a mirror characterized in that it comprises: a. an optional sensitization step, b. an optional step of activating the surface of the substrate to be coated, characterized in that the 3037060 13 c. a step of depositing at least one reflective metal layer on a transparent substrate, d. a step of depositing at least one protective layer, e. a step of depositing an overlayer having a thickness of less than 6 μm on said protective layer making it possible to block the porosity of the latter and f. a step of drying said overcoat.
    [0013]
    13. Process according to claim 12, characterized in that the overcoat deposition step is carried out by spraying, rolling, quenching, curtain coating or spraying, or by screen printing techniques.
    [0014]
    14. The method of claim 13 characterized in that the deposition step of the overcoat is carried out by spraying, or by curtain coating and is followed by a scraping step so as to obtain a thinest possible overlayer.
    [0015]
    15. The method of claim 13 characterized in that the step of depositing the overlay is carried out with a roller for simultaneously performing a scraping step by rotating the roller in the opposite direction, so as to obtain an overlay the finest possible . 20
    [0016]
    16. Method according to one of claims 12 to 15 characterized in that the drying step is carried out in hot air, by IR baking and / or UV
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    引用文献:
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    法律状态:
    2016-06-14| PLFP| Fee payment|Year of fee payment: 2 |
    2016-12-09| PLSC| Search report ready|Effective date: 20161209 |
    2017-06-23| PLFP| Fee payment|Year of fee payment: 3 |
    2018-06-25| PLFP| Fee payment|Year of fee payment: 4 |
    2019-06-21| PLFP| Fee payment|Year of fee payment: 5 |
    2020-06-29| PLFP| Fee payment|Year of fee payment: 6 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1555007|2015-06-02|
    FR1555007A|FR3037060B1|2015-06-02|2015-06-02|MIRROR WITH IMPROVED DURABILITY|FR1555007A| FR3037060B1|2015-06-02|2015-06-02|MIRROR WITH IMPROVED DURABILITY|
    KR1020177037375A| KR20180015172A|2015-06-02|2016-05-31|Mirror with improved durability|
    EP16734419.1A| EP3303243B1|2015-06-02|2016-05-31|Mirror with improved durability|
    CN201680032126.4A| CN107667078A|2015-06-02|2016-05-31|Mirror with improved durability|
    US15/579,048| US10746902B2|2015-06-02|2016-05-31|Mirror with improved durability|
    PL16734419T| PL3303243T3|2015-06-02|2016-05-31|Mirror with improved durability|
    PCT/FR2016/051296| WO2016193611A1|2015-06-02|2016-05-31|Mirror with improved durability|
    DK16734419.1T| DK3303243T3|2015-06-02|2016-05-31|MIRROR WITH IMPROVED DURABILITY|
    MX2017015354A| MX2017015354A|2015-06-02|2016-05-31|Mirror with improved durability.|
    BR112017024718-6A| BR112017024718A2|2015-06-02|2016-05-31|mirror with improved durability|
    ES16734419T| ES2757054T3|2015-06-02|2016-05-31|Mirror with improved durability|
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