WO2016039060A1 - ガスバリア性フィルム、及び、有機エレクトロルミネッセンス素子 - Google Patents
ガスバリア性フィルム、及び、有機エレクトロルミネッセンス素子 Download PDFInfo
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- WO2016039060A1 WO2016039060A1 PCT/JP2015/072665 JP2015072665W WO2016039060A1 WO 2016039060 A1 WO2016039060 A1 WO 2016039060A1 JP 2015072665 W JP2015072665 W JP 2015072665W WO 2016039060 A1 WO2016039060 A1 WO 2016039060A1
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Definitions
- the present invention relates to a gas barrier film and an organic electroluminescence device using the gas barrier film.
- Organic electroluminescence devices using organic electroluminescence are thin-film, completely solid-state devices that can emit light at a low voltage of several volts to several tens of volts. It has many excellent features such as brightness, high luminous efficiency, thinness, and light weight. For this reason, organic EL using a gas barrier film having a gas barrier layer on a thin and light resin substrate in recent years, particularly as backlights for various displays, display boards such as signboards and emergency lights, and surface light emitters such as illumination light sources. Devices are drawing attention.
- a gas barrier film used for such an organic EL element for example, a gas barrier film having a layer in which a hydrocarbon compound ion is implanted into a layer containing a polysilazane compound on a substrate has been proposed (for example, a patent Reference 1).
- a gas barrier film having a silicon-containing film having a high nitrogen concentration region formed on a substrate has been proposed (see, for example, Patent Document 2).
- a gas barrier film using a polysilazane modified film has been proposed (for example, see Patent Document 3).
- the generation of dark spots cannot be sufficiently suppressed when stored in a high temperature and high humidity environment such as 85 ° C. and 85% RH for a long time.
- the gas barrier property when a thin resin substrate having a thickness of 50 ⁇ m or less is used is not sufficient.
- the present invention provides a gas barrier film having a sufficient gas barrier property on a resin substrate of 50 ⁇ m or less, and a highly reliable organic electroluminescence device using the gas barrier film. To do.
- the gas barrier film of the present invention applies energy to a coating obtained by applying and drying a resin base material having a thickness of 3 to 50 ⁇ m, a first gas barrier layer containing an inorganic compound, and a coating liquid containing polysilazane. And a region satisfying the composition range represented by SiO w N x (where 0.2 ⁇ w ⁇ 0.55, 0.66 ⁇ x ⁇ 0.75), and having a thickness of 50 to 1000 nm.
- the organic electroluminescent element of this invention is equipped with the said gas barrier film, and the organic functional layer pinched
- a gas barrier film having a sufficient gas barrier property and a highly reliable organic electroluminescence element can be provided.
- Embodiment 2 of gas barrier film Embodiment of organic electroluminescence device is not limited to the following examples. The description will be given in the following order.
- the schematic block diagram of the gas barrier film of this embodiment is shown in FIG. 1 .
- the gas barrier film shown in FIG. 1 includes a resin base material 1 and a gas barrier layer 22 formed on the resin base material 1.
- the gas barrier layer 22 includes a laminated structure in which a first gas barrier layer 22a, a second gas barrier layer 22b, and a third gas barrier layer 22c are laminated in this order from the resin substrate 1 side.
- the resin substrate 1 is a thin resin film having flexibility and a thickness of 3 to 50 ⁇ m.
- the first gas barrier layer 22a includes an inorganic compound.
- the second gas barrier layer 22b is formed by applying energy to a coating film obtained by applying and drying a coating liquid containing polysilazane.
- the second gas barrier layer 22b has a region satisfying the composition range of SiO w N x (where 0.2 ⁇ w ⁇ 0.55, 0.66 ⁇ x ⁇ 0.75), and this region. At a thickness of 50 to 1000 nm.
- the third gas barrier layer 22c is formed in contact with the second gas barrier layer 22b, and contains a metal oxide having a lower oxidation-reduction potential than silicon as a main component.
- the thin resin substrate is somewhat difficult in flatness (surface smoothness) compared to the conventional thick resin substrate, and when a transparent electrode is formed directly on the resin substrate, the thin resin substrate Since the surface irregularity pattern of this is reflected on the transparent electrode as it is, the smoothness of the transparent electrode is affected.
- a transparent electrode having high smoothness can be formed by forming the gas barrier layer 22 on the resin base material 1.
- a transparent electrode having high smoothness can be formed by including the second gas barrier layer 22b that satisfies the above composition range.
- the second gas barrier layer 22b can be formed by, for example, a wet coating method and a surface modification process. Specifically, after forming a gas barrier forming precursor layer with a polysilazane coating liquid, and smoothing the unevenness of the resin base material with this gas barrier forming precursor layer, the surface is irradiated with energy such as vacuum ultraviolet rays to modify the surface. Can be produced.
- the second gas barrier layer 22b by the above-described wet coating method and surface modification treatment, it is not necessary to expose the thin resin substrate to a high temperature environment as compared with the sputtering method or the like. Further, by performing the modification treatment from the surface of the gas barrier forming precursor layer, the modification treatment proceeds on the surface side to become a hard film. On the other hand, since the reforming process does not proceed completely on the lower layer side, the film becomes soft to some extent, and a film hardness distribution can be imparted within the gas barrier layer 22.
- the second gas barrier layer 22b has a region satisfying the composition range represented by SiOwNx (hereinafter, also simply referred to as region (b)), thereby exhibiting gas barrier properties.
- the second gas barrier layer 22b is formed by applying energy to a coating film obtained by applying and drying a coating liquid containing polysilazane, unlike the case where the second gas barrier layer 22b is formed by a vapor deposition method. For this reason, it is possible to form a layer with very few defects and almost no foreign matters such as particles mixed during film formation.
- the region (b) of the second gas barrier layer 22b is not completely stable against oxidation, and may be gradually oxidized in a high-temperature and high-humidity environment to lower the gas barrier property.
- the second gas barrier layer 22b is spot-oxidized by the water vapor, and a portion having a reduced gas barrier property is formed. It is considered that a dark spot is generated in the organic EL element when water vapor enters from a portion where the gas barrier property is lowered.
- the third gas barrier layer 22c is formed in contact with the second gas barrier layer 22b.
- the third gas barrier layer 22c contains a metal oxide having a lower oxidation-reduction potential than silicon as a main component.
- the gas barrier property of the third gas barrier layer 22c itself is not so high, and it is considered that there is no gas barrier property that contributes to the reduction of dark spots of the organic EL element.
- the third gas barrier layer 22c contains a metal oxide having a low redox potential as a main component, it is oxidized prior to the region (b) of the second gas barrier layer 22b in a high temperature and high humidity environment. . For this reason, by forming the third gas barrier layer 22c in contact with the second gas barrier layer 22b, the effect of suppressing oxidation of the surface of the second gas barrier layer 22b in a high temperature and high humidity environment is exhibited, and the spot gas barrier property is reduced. It is thought that it becomes difficult to occur.
- the gas barrier film having the gas barrier layer 22 composed of the first gas barrier layer 22a, the second gas barrier layer 22b, and the third gas barrier layer 22c is durable in a high temperature and high humidity environment such as 85 ° C. and 85% RH. Even when a thin resin substrate 1 having a thickness of 50 ⁇ m or less is used, sufficient gas barrier properties can be obtained.
- the above mechanisms are estimated.
- the above-mentioned mechanism is speculation and the expression of the barrier property of the gas barrier film is not limited to the above-described mechanism.
- the resin base material 1 constituting the gas barrier film is a flexible resin film that can be bent and is a thin resin having a thickness in the range of 3 to 50 ⁇ m.
- the resin base material 1 will not be specifically limited if it is a resin material which can hold
- polyesters such as polyethylene terephthalate (abbreviation: PET) and polyethylene naphthalate (abbreviation: PEN), polyethylene, polypropylene, cellophane, cellulose diacetate, cellulose triacetate (abbreviation: TAC), and cellulose acetate butyrate.
- PET polyethylene terephthalate
- PEN polyethylene naphthalate
- TAC cellulose triacetate
- TAC cellulose acetate butyrate
- CAP cellulose acetate propionate
- PC polycarbonate
- PES polyethersulfone
- PES Polyphenylene sulfide, polysulfones, polyether imide, polyether ketone imide, polyamide, fluororesin, nylon, polymethyl methacrylate, acrylic and polyarylates, Arton (trade name, manufactured by JSR) and Appel (trade name, Mitsui Chemicals) And the like, and the like.
- films such as polyethylene terephthalate (abbreviation: PET), polybutylene terephthalate, polyethylene naphthalate (abbreviation: PEN), polycarbonate (abbreviation: PC) are possible in terms of cost and availability. It is preferably used as a flexible resin.
- PET polyethylene terephthalate
- PEN polyethylene naphthalate
- PC polycarbonate
- the thickness of the resin substrate 1 is in the range of 3 to 50 ⁇ m, preferably in the range of 3 to 35 ⁇ m, more preferably in the range of 3 to 30 ⁇ m, and particularly preferably in the range of 10 to 30 ⁇ m. Within range.
- the resin base material 1 is preferably made of a material having heat resistance. Specifically, a resin having a linear expansion coefficient of 15 ppm / K or more and 100 ppm / K or less and a glass transition temperature (Tg) of 100 ° C. or more and 300 ° C. or less is used.
- Tg glass transition temperature
- the resin base material 1 satisfies the necessary conditions as a laminated film for electronic parts and displays. That is, when using a gas barrier film for these applications, the gas barrier film may be exposed to a process at 150 ° C. or higher.
- the substrate dimensions are not stable when the gas barrier film is passed through the temperature process as described above, and thermal expansion and contraction occur.
- the shut-off performance is deteriorated or inconvenience of being unable to withstand the heat process is likely to occur. If it is less than 15 ppm / K, the film may break like glass and the flexibility may deteriorate.
- thermoplastic resin that can be used as the resin substrate 1 include, for example, polyethylene terephthalate (PET: 70 ° C.), polyethylene naphthalate (PEN: 120 ° C.), polycarbonate (PC: 140 ° C.), and fat.
- Cyclic polyolefin for example, ZEONOR (registered trademark) 1600: 160 ° C.
- Neoprim registered trademark
- the resin substrate 1 is preferably transparent.
- Transparent means that the light transmittance is usually 80% or more, preferably 85% or more, and more preferably 90% or more.
- the light transmittance is calculated by measuring the total light transmittance and the amount of scattered light using the method described in JIS K7105: 1981, that is, using an integrating sphere light transmittance measuring device, and subtracting the diffuse transmittance from the total light transmittance. can do.
- the resin substrate 1 is transparent and each layer including the transparent electrode formed on the resin substrate 1 is also a layer having high light transmittance, so that light extraction from the resin substrate 1 side can be performed. It becomes possible.
- This resin substrate 1 can also be suitably used as a sealing member (transparent substrate) for organic EL elements.
- the resin base material 1 may be an unstretched film or a stretched film.
- the resin substrate 1 can be manufactured by a conventionally known general film forming method.
- an unstretched resin base material 1 that is substantially amorphous and not oriented can be manufactured by melting a resin as a material, and extruding it into an annular die or a T-die with an extruder and quenching.
- the resin transport direction (vertical axis direction, MD direction) can be applied to the unstretched resin by a known method such as uniaxial stretching, tenter-type sequential biaxial stretching, tenter-type simultaneous biaxial stretching, tubular simultaneous biaxial stretching, etc.
- stretching resin base material can be manufactured by extending
- the draw ratio in this case can be appropriately selected according to the resin as the raw material of the resin base material 1, but is preferably in the range of 2 to 10 times in the vertical axis direction and the horizontal axis direction.
- the resin substrate 1 may be subjected to a hydrophilic treatment such as corona treatment on the surface of the substrate before forming the precursor polysilazane layer or the like. .
- the thickness of the resin base material 1 is 3 to 50 ⁇ m, in the gas barrier film manufacturing method, the resin base material 1 is likely to be deformed or broken during the manufacturing process, and its handling is difficult.
- the thickness of the transparent substrate is thin and the rigidity is insufficient, misalignment and wrinkles are generated, and it is difficult to form an accurate and uniform layer.
- a support film is used when producing a flexible gas barrier film.
- the resin material applicable as the support film include various resin films that can be used as the resin base material 1 described above.
- the thickness of the support film is not particularly limited, but is preferably 50 to 300 ⁇ m in view of mechanical strength, handleability, and the like. The thickness of the support film can be measured using a micrometer.
- a method of applying a support film to the resin base material 1 a method of forming an adhesive layer between the resin base material 1 and the support film and press-contacting with a nip roller or the like, or a resin base material 1 and a support
- the method include a method in which a film is laminated and then charged with a potential difference between the two films laminated under vacuum to be in close contact with each other.
- This method of charging and adhering is a method of electrostatically adhering both films by charging both films with opposite charges, and after manufacturing various electronic devices on the gas barrier film. Removes the support film from the gas barrier film by performing a charge removal process in the charge removal process.
- the gas barrier film has a first gas barrier layer 22 a containing an inorganic compound on the resin substrate 1.
- the first gas barrier layer 22a may be a single layer or a laminated structure of two or more layers.
- the first gas barrier layers 22a may have the same composition or different compositions.
- the first gas barrier layer 22a contains an inorganic compound.
- the inorganic compound contained in the first gas barrier layer 22a is not particularly limited, but for example, silicon or a metal oxide, metal nitride, metal carbide, metal oxynitride or metal oxycarbide having a higher redox potential than silicon or silicon. Is mentioned. Of these, oxides, nitrides, carbides, oxynitrides or oxycarbides containing one or more metals selected from Si, In, Sn, Zn, Cu, and Ce are preferably used in terms of gas barrier performance. Can do. Specific examples of suitable inorganic compounds include silicon oxide, silicon nitride, silicon oxynitride, silicon carbide, and silicon oxycarbide. You may contain another element as a secondary component.
- content of the inorganic compound contained in the 1st gas barrier layer 22a is not specifically limited, It is preferable that it is 50 mass% or more with respect to the total mass of the 1st gas barrier layer 22a, and it is more preferable that it is 80 mass% or more. Further, it is more preferably 95% by mass or more, particularly preferably 98% by mass or more, and most preferably 100% by mass (that is, the first gas barrier layer 22a is an inorganic compound).
- the thickness of the first gas barrier layer 22a (total thickness in the case of a laminated structure of two or more layers) is not particularly limited, but is preferably 5 to 1000 nm, and more preferably 20 to 500 nm. If it is this range, the advantage of coexistence of productivity and gas barrier property will be acquired.
- the thickness of the first gas barrier layer 22a can be measured by TEM observation.
- the first gas barrier layer 22a As a method for forming the first gas barrier layer 22a, a method of applying energy to a coating film obtained by applying and drying a coating liquid containing polysilazane (wet coating method and surface modification treatment), or a gas phase formation method.
- a membrane method is mentioned.
- it is preferably formed by a vapor deposition method that is not easily oxidized by humidity and can stably exhibit gas barrier properties even in a high-temperature and high-humidity environment.
- the first gas barrier layer 22a formed by applying energy to a coating film obtained by applying and drying a coating liquid containing polysilazane so as to be in contact with the resin base material 1 having no gas barrier property is a resin base material.
- the composition is such that the resin base material 1 side in the thickness direction is oxidized by the influence of water vapor or oxygen permeating from the one side, that is, a composition such as SiO 2.0 to 2.4 .
- the surface side of the layer to which energy is applied has a SiON composition in which N is about 0.6 or less and O is about 0.6 or more with respect to Si. This region has a high gas barrier property and the second gas barrier.
- the first gas barrier layer 22a has a clear interface between the composition on the resin substrate 1 side and the composition on the surface side. Furthermore, the region (b) in the second gas barrier layer 22b is not formed in the first gas barrier layer 22a due to moisture diffusion from the resin base material 1 or the like.
- Vapor deposition method examples of the vapor deposition method that is a preferable method for forming the first gas barrier layer 22a include physical vapor deposition (PVD) and chemical vapor deposition (CVD). Hereinafter, the vapor deposition method will be described.
- PVD physical vapor deposition
- CVD chemical vapor deposition
- the physical vapor deposition method is a method of depositing a target material, for example, a thin film such as a carbon film, on the surface of the material in a gas phase by a physical method. Examples thereof include a DC sputtering method, an RF sputtering method, an ion beam sputtering method, and a magnetron sputtering method, a vacuum deposition method, and an ion plating method.
- the chemical vapor deposition method is a method of depositing a film by supplying a source gas containing a target thin film component onto a substrate and performing a chemical reaction on the surface of the substrate or in the gas phase. It is. In addition, there is also a method of generating plasma or the like for the purpose of activating a chemical reaction.
- Known CVD methods such as thermal CVD method, catalytic chemical vapor deposition method, photo CVD method, vacuum plasma CVD method, atmospheric pressure plasma CVD method, etc. Etc.
- a plasma CVD method such as a vacuum plasma CVD method or an atmospheric pressure plasma CVD method from the viewpoint of film forming speed and processing area.
- silicon oxide is generated.
- highly active charged particles and active radicals exist in the plasma space at a high density, so that multistage chemical reactions are accelerated at high speed in the plasma space, and the elements present in the plasma space are thermodynamic. This is because it is converted into an extremely stable compound in a very short time.
- FIG. 2 and 3 are schematic configuration diagrams of an example of a film forming apparatus.
- a film forming apparatus 101 shown in FIG. 3 is basically configured by connecting two film forming apparatuses 100 shown in FIG.
- the case where the first gas barrier layer 22a is formed will be described using the film forming apparatus 101 shown in FIG. 3 as an example.
- the description regarding the film forming apparatus 101 illustrated in FIG. 3 is also referred to as appropriate for the description regarding the film forming apparatus 100 illustrated in FIG.
- the film forming apparatus 101 includes a delivery roll 10, transport rolls 11, 12a, 12b, 13a, 13b, and 14, a first film forming roll 15a, a second film forming roll 16a, and a third film forming film.
- the vacuum pumps 40a and 40b and the control unit 41 are included.
- Delivery roll 10 transport rolls 11, 12a, 12b, 13a, 13b, 14, first film forming roll 15a, second film forming roll 16a, third film forming roll 15b and fourth film forming roll 16b, and winding roll 17 is accommodated in the vacuum chamber 30.
- the delivery roll 10 feeds the base material 1 a installed in a state of being wound in advance toward the transport roll 11.
- the delivery roll 10 is a cylindrical roll extending in a direction perpendicular to the paper surface, and is rotated counterclockwise by a drive motor (not shown) (see the arrow in FIG. 3), whereby the substrate 1a is transported.
- the transport rolls 11, 12 a, 12 b, 13 a, 13 b, 14 are cylindrical rolls configured to be rotatable around a rotation axis substantially parallel to the feed roll 10.
- the transport roll 11 is a roll for transporting the base material 1a from the feed roll 10 to the first film forming roll 15a while applying an appropriate tension to the base material 1a.
- the conveying rolls 12a and 13a convey the base material 1b from the first film forming roll 15a to the second film forming roll 16a while applying appropriate tension to the base material 1b formed by the first film forming roll 15a. It is a roll for.
- the conveyance rolls 12b and 13b convey the base material 1e from the third film formation roll 15b to the fourth film formation roll 16b while applying an appropriate tension to the base material 1e formed by the third film formation roll 15b. It is a roll for. Further, the transporting roll 14 transports the base material 1c from the fourth film forming roll 16b to the take-up roll 17 while applying an appropriate tension to the base material 1c formed by the fourth film forming roll 16b. It is a roll.
- the first film forming roll 15a and the second film forming roll 16a are a pair of film forming rolls having a rotation axis substantially parallel to the delivery roll 10 and facing each other with a predetermined distance therebetween.
- the third film-forming roll 15b and the fourth film-forming roll 16b are a pair of film-forming rolls having a rotation axis substantially parallel to the delivery roll 10 and facing each other with a predetermined distance therebetween.
- the second film forming roll 16a forms the base material 1b, and conveys the base material 1d to the third film forming roll 15b while applying an appropriate tension to the formed base material 1d.
- the 4th film-forming roll 16b forms the base material 1e, and conveys the base material 1c to the conveyance roll 14, providing appropriate tension to the formed base material 1c.
- the distance between the first film forming roll 15a and the second film forming roll 16a is a distance connecting the point A and the point B, and the third film forming roll 15b and the fourth film forming roll.
- the separation distance from 16b is a distance connecting point D and point E.
- the first film-forming roll 15a, the second film-forming roll 16a, the third film-forming roll 15b, and the fourth film-forming roll 16b are discharge electrodes formed of a conductive material.
- the film forming roll 16a, the third film forming roll 15b, and the fourth film forming roll 16b are insulated from each other. Note that the materials and configurations of the first film-forming roll 15a, the second film-forming roll 16a, the third film-forming roll 15b, and the fourth film-forming roll 16b may be appropriately selected so as to achieve a desired function as an electrode. it can.
- first film forming roll 15a, the second film forming roll 16a, the third film forming roll 15b, and the fourth film forming roll 16b may be individually temperature controlled.
- the temperatures of the first film-forming roll 15a, the second film-forming roll 16a, the third film-forming roll 15b, and the fourth film-forming roll 16b are not particularly limited, but are, for example, ⁇ 30 to 100 ° C. If the glass transition temperature of the substrate 1a is exceeded and the temperature is set too high, the substrate may be deformed by heat.
- Magnetic field generators 20a, 21a, 20b, and 21b are installed inside the first film forming roll 15a, the second film forming roll 16a, the third film forming roll 15b, and the fourth film forming roll 16b, respectively.
- a high frequency voltage for generating plasma is applied to the first film forming roll 15a and the second film forming roll 16a by a plasma generating power source 19a.
- a high frequency voltage for plasma generation is applied to the third film formation roll 15b and the fourth film formation roll 16b by a plasma generation power source 19b.
- An electric field is generated in the film forming section Sa between the first film forming roll 15a and the second film forming roll 16a, or in the film forming section Sb between the third film forming roll 15b and the fourth film forming roll 16b.
- the discharge plasma of the film forming gas formed and supplied from the gas supply pipe 18a or the gas supply pipe 18b is generated.
- the voltage applied by the plasma generating power source 19a and the voltage applied by the plasma generating power source 19b may be the same or different.
- the power source frequency of the plasma generation power source 19a or the plasma generation power source 19b can be arbitrarily set.
- the apparatus of this configuration is, for example, 60 to 100 kHz, and the applied power is 1 m for the effective film formation width of 1 m. For example, it is 1 to 10 kW.
- the take-up roll 17 has a rotation axis substantially parallel to the feed roll 10, and accommodates the base material 1c in the form of a take-up roll.
- the take-up roll 17 takes up the substrate 1c by rotating counterclockwise by a drive motor (not shown) (see the arrow in FIG. 3).
- a drive motor not shown
- the first gas barrier layer is transported in the forward direction and the reverse direction and the film forming unit Sa or the film forming unit Sb is reciprocated.
- the formation (film formation) step of 22a can be repeated a plurality of times.
- the base material 1a fed from the feed roll 10 is transported between the feed roll 10 and the take-up roll 17 by the transport rolls 11, 12a, 12b, 13a, 13b, 14, the first film forming roll 15a, and the second composition roll. While being wound around the film roll 16a, the third film forming roll 15b, and the fourth film forming roll 16b, it is conveyed by the rotation of each of these rolls while maintaining an appropriate tension.
- the conveyance direction of base material 1a, 1b, 1c, 1d, 1e is shown by the arrow.
- the conveyance speed (line speed) of the base materials 1a, 1b, 1c, 1d, and 1e (for example, the conveyance speed at the points C and F in FIG.
- the conveyance speed is adjusted by controlling the rotation speeds of the drive motors of the delivery roll 10 and the take-up roll 17 by the control unit 41. When the conveyance speed is decreased, the thickness of the formed region is increased.
- the transport direction of the substrates 1a, 1b, 1c, 1d, and 1e is opposite to the direction indicated by the arrow in FIG. 3 (hereinafter referred to as the forward direction) (hereinafter referred to as the reverse direction). It is also possible to carry out the film-forming process of the gas barrier film. Specifically, the control unit 41 rotates the rotation direction of the drive motors of the feed roll 10 and the take-up roll 17 in the direction opposite to that described above in a state where the substrate 1c is taken up by the take-up roll 17. Control to do.
- the base material 1c fed from the take-up roll 17 is transferred between the feed roll 10 and the take-up roll 17 with the transport rolls 11, 12a, 12b, 13a, 13b, 14 and the first component. While being wound around the film roll 15a, the second film forming roll 16a, the third film forming roll 15b, and the fourth film forming roll 16b, it is conveyed in the reverse direction by the rotation of each of these rolls while maintaining an appropriate tension. .
- the gas supply pipes 18 a and 18 b supply a film forming gas such as a plasma CVD source gas into the vacuum chamber 30.
- the gas supply pipe 18a has a tubular shape extending in the same direction as the rotation axis of the first film forming roll 15a and the second film forming roll 16a above the film forming section Sa, and is provided at a plurality of locations.
- a film forming gas is supplied to the film forming section Sa from the opened opening.
- the gas supply pipe 18b has a tubular shape extending in the same direction as the rotation axes of the third film forming roll 15b and the fourth film forming roll 16b above the film forming part Sb, and is provided at a plurality of locations.
- a film forming gas is supplied from the provided opening to the film forming unit Sb.
- the film forming gas supplied from the gas supply pipe 18a and the film forming gas supplied from the gas supply pipe 18b may be the same or different. Further, the supply gas pressure supplied from these gas supply pipes may be the same or different.
- a silicon compound can be used as the source gas.
- the silicon compound include hexamethyldisiloxane (HMDSO), 1,1,3,3-tetramethyldisiloxane, vinyltrimethylsilane, methyltrimethylsilane, hexamethyldisilane, methylsilane, dimethylsilane, trimethylsilane, and diethylsilane.
- the compounds described in paragraph [0075] of JP-A-2008-056967 can also be used.
- these silicon compounds it is preferable to use HMDSO in forming the first gas barrier layer 22a from the viewpoint of easy handling of the compound and high gas barrier properties of the obtained gas barrier film.
- the source gas may contain monosilane in addition to the silicon compound.
- a reactive gas may be used in addition to the source gas.
- a gas that reacts with the raw material gas to become a silicon compound such as oxide or nitride is selected.
- a reactive gas for forming an oxide as a thin film for example, oxygen gas or ozone gas can be used. In addition, you may use these reaction gas in combination of 2 or more type.
- a carrier gas may be further used to supply the source gas into the vacuum chamber 30.
- a discharge gas may be further used to generate plasma.
- a carrier gas and the discharge gas for example, a rare gas such as argon, hydrogen, or nitrogen is used.
- the magnetic field generators 20a and 21a are members that form a magnetic field in the film forming unit Sa between the first film forming roll 15a and the second film forming roll 16a.
- the magnetic field generators 20b and 21b are third members. It is a member that forms a magnetic field in the film forming section Sb between the film forming roll 15b and the fourth film forming roll 16b.
- These magnetic field generators 20a, 20b, 21a, and 21b do not follow the rotation of the first film-forming roll 15a, the second film-forming roll 16a, the third film-forming roll 15b, and the fourth film-forming roll 16b.
- the vacuum chamber 30 includes a delivery roll 10, transport rolls 11, 12a, 12b, 13a, 13b, and 14, a first film forming roll 15a, a second film forming roll 16a, a third film forming roll 15b, and a fourth film forming roll 16b. And the winding roll 17 is sealed and the state decompressed is maintained.
- the pressure (vacuum degree) in the vacuum chamber 30 can be appropriately adjusted according to the type of the raw material gas.
- the pressure of the film forming part S or Sb is preferably 0.1 to 50 Pa.
- the vacuum pumps 40a and 40b are communicably connected to the control unit 41 and appropriately adjust the pressure in the vacuum chamber 30 in accordance with instructions from the control unit 41.
- the control unit 41 controls each component of the film forming apparatus 101.
- the control unit 41 is connected to the drive motors of the feed roll 10 and the take-up roll 17 and adjusts the conveyance speed of the substrate 1a by controlling the number of rotations of these drive motors. Moreover, the conveyance direction of the base material 1a is changed by controlling the rotation direction of the drive motor.
- the control unit 41 is connected to a film-forming gas supply mechanism (not shown) so as to be communicable, and controls the supply amount of each component gas of the film-forming gas.
- the control unit 41 is communicably connected to the plasma generation power sources 19a and 19b, and controls the output voltages and output frequencies of the plasma generation power sources 19a and 19b. Further, the control unit 41 is communicably connected to the vacuum pumps 40a and 40b, and controls the vacuum pumps 40a and 40b so as to maintain the inside of the vacuum chamber 30 in a predetermined reduced pressure atmosphere.
- the control unit 41 includes a CPU (Central Processing Unit), HDD (Hard Disk Drive), RAM (Random Access Memory), and ROM (Read Only Memory).
- the HDD stores a software program describing a procedure for controlling each component of the film forming apparatus 101 and realizing a method for producing a gas barrier film.
- the software program is loaded into the RAM and sequentially executed by the CPU.
- the ROM stores various data and parameters used when the CPU executes the software program.
- the second gas barrier layer 22b is formed by applying energy to a coating film obtained by applying and drying a coating liquid containing polysilazane.
- the second gas barrier layer 22b may be a single layer or a laminated structure of two or more layers.
- the second gas barrier layers 22b may have the same composition or different compositions.
- the thickness of the second gas barrier layer 22b (the total thickness in the case of a laminated structure of two or more layers) is preferably 10 to 1000 nm, and more preferably 50 to 600 nm. If it is this range, the balance of gas barrier property and durability becomes favorable and is preferable.
- the thickness of the second gas barrier layer 22b can be measured by TEM observation.
- the gas barrier properties of the second gas barrier layer 22b are expressed by applying energy. Unlike the case where the second gas barrier layer 22b is formed by the vapor phase film formation method, the foreign substance such as particles is not mixed at the time of film formation, so that the gas barrier layer has very few defects.
- the second gas barrier layer 22b includes a region satisfying a composition range represented by SiO w N x (where 0.2 ⁇ w ⁇ 0.55, 0.66 ⁇ x ⁇ 0.75). (B) having a thickness of 50 to 1000 nm.
- the region (b) has a gas barrier property, but also functions as a so-called desiccant that captures water vapor by reacting with water vapor that has gradually entered.
- the thickness of the region (b) in the second gas barrier layer 22b is 50 to 1000 nm.
- the thickness of the region (b) is less than 50 nm, since the total amount of the compound that reacts with water vapor as a desiccant is reduced, the amount of water vapor that can be captured is limited, and the desiccant function is lost within the service life required for the device. There is a possibility that the gas barrier property is lowered.
- the thickness exceeds 1000 nm for example, when the region (b) is formed by the modification by application of energy, the modification is insufficient and the gas barrier property may be lowered, and the cost is increased.
- the thickness of the region (b) is preferably 100 to 300 nm. Within this range, the effect of maintaining good gas barrier properties and the effect of reducing costs are further improved during the service life required for the device.
- the region (b) is formed by applying energy to a coating film obtained by applying and drying a coating liquid containing polysilazane. If the region (b) is present in the second gas barrier layer 22b, the region (b) may be present as one continuous region, or may be present as two or more regions. Good. When there are two or more regions, the sum of the thicknesses of all the regions (total thickness) only needs to be in the above range.
- the composition ratio of silicon, oxygen, and nitrogen in the region (b) and the thickness of the region (b) can be adjusted by an arbitrary method.
- the thickness of the coating solution containing polysilazane the degree of drying after coating, the amount of energy to be applied (for example, when applying energy by applying vacuum ultraviolet light, illuminance, plasma density, irradiation time, etc.), energy application What is necessary is just to adjust the atmosphere (especially oxygen concentration) of time.
- the amount of energy to be applied is reduced, oxygen can be reduced in the composition ratio of the region.
- the second gas barrier layer 22b having the region (b) having the above composition and thickness may be formed by alternately performing coating film formation and energy application a plurality of times.
- the second gas barrier layer 22b including the region (b) is formed by applying energy to a coating film obtained by applying and drying a coating liquid containing polysilazane.
- the formation conditions (of the polysilazane used) The type, the solvent used in the coating solution, the concentration of the coating solution, the type of catalyst, the application conditions of energy, etc.) are the same as described below.
- the region (b) is not formed in the first gas barrier layer 22a directly formed on the resin base material 1, and even if the first gas barrier layer 22a and the second gas barrier layer 22b are formed. Even if formed under the same conditions, the first gas barrier layer 22a and the second gas barrier layer 22b are clearly different layers.
- Polysilazane is a polymer having a silicon-nitrogen bond, such as SiO 2 , Si 3 N 4 having a bond such as Si—N, Si—H, or N—H, and ceramics such as both intermediate solid solutions SiO x N y. It is a precursor inorganic polymer. Specifically, the polysilazane preferably has the following structure.
- R 1 , R 2 and R 3 are each independently a hydrogen atom, a substituted or unsubstituted alkyl group, aryl group, vinyl group or (trialkoxysilyl) alkyl group. .
- R 1 , R 2 and R 3 may be the same or different.
- examples of the alkyl group include linear, branched or cyclic alkyl groups having 1 to 8 carbon atoms.
- the aryl group include aryl groups having 6 to 30 carbon atoms.
- non-condensed hydrocarbon groups such as a phenyl group, a biphenyl group, and a terphenyl group; a pentarenyl group, an indenyl group, a naphthyl group, an azulenyl group, a heptaenyl group, a biphenylenyl group, a fluorenyl group, an acenaphthylenyl group, and a preadenyl group
- Condensed polycyclic hydrocarbon groups such as acenaphthenyl group, phenalenyl group, phenanthryl group, anthryl group, fluoranthenyl group, acephenanthrenyl group, aceantrirenyl group, triphenylenyl group, pyrenyl group, chrysenyl group, naphthacenyl group, etc.
- the (trialkoxysilyl) alkyl group includes an alkyl group having 1 to 8 carbon atoms having a silyl group substituted with an alkoxy group having 1 to 8 carbon atoms. More specific examples include 3- (triethoxysilyl) propyl group and 3- (trimethoxysilyl) propyl group.
- the substituent optionally present in R 1 to R 3 is not particularly limited, and examples thereof include an alkyl group, a halogen atom, a hydroxyl group (—OH), a mercapto group (—SH), a cyano group (—CN), There are a sulfo group (—SO 3 H), a carboxyl group (—COOH), a nitro group (—NO 2 ) and the like. Note that the optionally present substituent is not the same as R 1 to R 3 to be substituted. For example, when R 1 to R 3 are alkyl groups, they are not further substituted with an alkyl group.
- R 1 , R 2 and R 3 are preferably a hydrogen atom, a methyl group, an ethyl group, a propyl group, an isopropyl group, a butyl group, an isobutyl group, a tert-butyl group, a phenyl group, a vinyl group, 3 -(Triethoxysilyl) propyl group or 3- (trimethoxysilylpropyl) group.
- n is an integer
- the polysilazane having the structure represented by the general formula (I) is determined to have a number average molecular weight of 150 to 150,000 g / mol. preferable.
- one of preferred embodiments is perhydropolysilazane in which all of R 1 , R 2 and R 3 are hydrogen atoms.
- polysilazane has a structure represented by the following general formula (II).
- R 1 ′ , R 2 ′ , R 3 ′ , R 4 ′ , R 5 ′ and R 6 ′ each independently represent a hydrogen atom, a substituted or unsubstituted alkyl group, An aryl group, a vinyl group or a (trialkoxysilyl) alkyl group.
- R 1 ′ , R 2 ′ , R 3 ′ , R 4 ′ , R 5 ′ and R 6 ′ may be the same or different.
- the substituted or unsubstituted alkyl group, aryl group, vinyl group or (trialkoxysilyl) alkyl group in the above is the same as the definition of the general formula (I), and thus the description is omitted.
- n ′ and p are integers, and the polysilazane having the structure represented by the general formula (II) is determined to have a number average molecular weight of 150 to 150,000 g / mol. It is preferred that Note that n ′ and p may be the same or different.
- R 1 ′ , R 3 ′ and R 6 ′ each represent a hydrogen atom, and R 2 ′ , R 4 ′ and R 5 ′ each represent a methyl group;
- R 1 ' , R 3' and R 6 ' each represents a hydrogen atom, R 2' and R 4 ' each represents a methyl group, and R 5' represents a vinyl group;
- R 1 ' , R 3' and R 4 A compound in which ' and R 6' each represent a hydrogen atom and R 2 ' and R 5' each represents a methyl group is preferred.
- polysilazane has a structure represented by the following general formula (III).
- R 1 ′′ , R 2 ′′ , R 3 ′′ , R 4 ′′ , R 5 ′′ , R 6 ′′ , R 7 ′′ , R 8 ′′ and R 9 ′′ are each independently A hydrogen atom, a substituted or unsubstituted alkyl group, aryl group, vinyl group or (trialkoxysilyl) alkyl group, wherein R 1 ′′ , R 2 ′′ , R 3 ′′ , R 4 ′′ , R 5 ′′ , R 6 ′′ , R 7 ′′ , R 8 ′′ and R 9 ′′ may be the same or different.
- the substituted or unsubstituted alkyl group, aryl group, vinyl group or (trialkoxysilyl) alkyl group in the above is the same as the definition of the general formula (I), and thus the description is omitted.
- n ′′, p ′′ and q are integers, and the polysilazane having the structure represented by the general formula (III) has a number average molecular weight of 150 to 150,000 g / mol. It is preferable to be determined as follows. Note that n ′′, p ′′ and q may be the same or different.
- R 1 ′′ , R 3 ′′ and R 6 ′′ each represent a hydrogen atom
- R 2 ′′ , R 4 ′′ , R 5 ′′ and R 8 ′′ each represent a methyl group.
- R 9 ′′ represents a (triethoxysilyl) propyl group
- R 7 ′′ represents an alkyl group or a hydrogen atom.
- the organopolysilazane in which a part of hydrogen atoms bonded to Si is substituted with an alkyl group or the like has improved adhesion to the first gas barrier layer 22a, which is the base, by having an alkyl group such as a methyl group.
- the ceramic film made of hard and brittle polysilazane can be toughened, and there is an advantage that the occurrence of cracks can be suppressed even when the (average) film thickness is increased. For this reason, these perhydropolysilazane and organopolysilazane may be appropriately selected according to the application, and may be used in combination.
- Perhydropolysilazane is presumed to have a linear structure and a ring structure centered on 6- and 8-membered rings. Its molecular weight is approximately 600 to 2000 (polystyrene conversion) in terms of number average molecular weight (Mn), and there are liquid or solid substances, and the state varies depending on the molecular weight.
- Polysilazane is commercially available in a solution state dissolved in an organic solvent, and the commercially available product can be used as it is as a coating solution for forming the second gas barrier layer 22b.
- Examples of commercially available polysilazane solutions include NN120-10, NN120-20, NAX120-20, NN110, NN310, NN320, NL110A, NL120A, NL120-20, NL150A, NP110, NP140, and SP140 manufactured by AZ Electronic Materials Co., Ltd. Is mentioned.
- polysilazane examples include, but are not limited to, for example, silicon alkoxide-added polysilazane obtained by reacting the above polysilazane with silicon alkoxide (Japanese Patent Laid-Open No.
- glycidol addition obtained by reacting glycidol Polysilazane (JP-A-6-122852), alcohol-added polysilazane obtained by reacting an alcohol (JP-A-6-240208), metal carboxylate-added polysilazane obtained by reacting a metal carboxylate 6-299118), acetylacetonate complex-added polysilazane obtained by reacting a metal-containing acetylacetonate complex (JP-A-6-306329), metal fine particle-added polysilazane obtained by adding metal fine particles (specialty) Kaihei 7- Publication), etc.
- No. 96986 include polysilazane ceramic at low temperatures.
- the content of polysilazane in the second gas barrier layer 22b before application of energy is 100% by mass when the total mass of the second gas barrier layer 22b is 100% by mass.
- the content of polysilazane in the layer is preferably 10% by mass or more and 99% by mass or less, and 40% by mass or more and 95% by mass or less. Is more preferably 70% by mass or more and 95% by mass or less.
- the solvent for preparing the coating solution for forming the second gas barrier layer 22b is not particularly limited as long as it can dissolve polysilazane, but water and reactive groups (for example, hydroxyl group, easily reacting with polysilazane).
- an organic solvent which does not contain an amine group and is inert to polysilazane is preferable, and an aprotic organic solvent is more preferable.
- the solvent includes an aprotic solvent; for example, carbon such as aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons such as pentane, hexane, cyclohexane, toluene, xylene, solvesso, and turben.
- an aprotic solvent for example, carbon such as aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons such as pentane, hexane, cyclohexane, toluene, xylene, solvesso, and turben.
- Hydrogen solvents Halogen hydrocarbon solvents such as methylene chloride and trichloroethane; Esters such as ethyl acetate and butyl acetate; Ketones such as acetone and methyl ethyl ketone; Aliphatic ethers such as dibutyl ether, dioxane and tetrahydrofuran; Alicyclic ethers and the like Ethers: Examples include tetrahydrofuran, dibutyl ether, mono- and polyalkylene glycol dialkyl ethers (diglymes), and the like.
- the solvent is selected according to purposes such as the solubility of polysilazane and the evaporation rate of the solvent, and may be used alone or in the form of a mixture of two or more.
- the concentration of polysilazane in the coating solution for forming the second gas barrier layer 22b is not particularly limited and varies depending on the film thickness of the layer and the pot life of the coating solution, but is preferably 1 to 80% by mass, more preferably 5 to 50% by mass. %, More preferably 10 to 40% by mass.
- the coating liquid for forming the second gas barrier layer 22b contains a catalyst in order to promote reforming.
- the catalyst is preferably a basic catalyst, and in particular, N, N-diethylethanolamine, N, N-dimethylethanolamine, triethanolamine, triethylamine, 3-morpholinopropylamine, N, N, N ′, N′— Amine catalysts such as tetramethyl-1,3-diaminopropane, N, N, N ′, N′-tetramethyl-1,6-diaminohexane, Pt compounds such as Pt acetylacetonate, and Pd compounds such as propionic acid Pd And metal catalysts such as Rh compounds such as Rh acetylacetonate and N-heterocyclic compounds.
- the concentration of the catalyst added at this time is preferably in the range of 0.1 to 10% by mass, more preferably 0.5 to 7% by mass, based on the silicon compound. By setting the addition amount of the catalyst within this range, it is possible to avoid excessive silanol formation due to rapid progress of the reaction, decrease in film density, increase in film defects, and the like.
- the following additives can be used as necessary.
- cellulose ethers, cellulose esters for example, ethyl cellulose, nitrocellulose, cellulose acetate, cellulose acetobutyrate, etc.
- natural resins for example, rubber, rosin resin, etc., synthetic resins
- Aminoplasts especially urea resins, melamine formaldehyde resins, alkyd resins, acrylic resins, polyesters or modified polyesters, epoxides, polyisocyanates or blocked polyisocyanates, polysiloxanes, and the like.
- Method of applying the coating solution for forming the second gas barrier layer As a method of applying the coating liquid for forming the second gas barrier layer 22b, a conventionally known appropriate wet coating method can be employed. Specific examples include spin coating method, roll coating method, flow coating method, ink jet method, spray coating method, printing method, dip coating method, casting film forming method, bar coating method, die coating method, gravure printing method and the like. It is done.
- the coating thickness can be appropriately set according to the preferred thickness and purpose.
- the thickness of the coating liquid (coating film) after drying is preferably 40 nm or more and 1000 nm or less, more preferably 100 nm or more. 300 nm or less.
- the coating film After applying the coating solution, it is preferable to dry the coating film.
- the organic solvent contained in the coating film can be removed. At this time, all of the organic solvent contained in the coating film may be dried or may be partially left. Even when a part of the organic solvent is left, a suitable second gas barrier layer 22b can be obtained. The remaining solvent is removed later.
- the drying temperature of the coating film varies depending on the substrate to be applied, but is preferably 50 to 200 ° C.
- the drying temperature is preferably set to 150 ° C. or less in consideration of deformation of the substrate due to heat.
- the temperature is set by using a hot plate, oven, furnace or the like.
- the drying time is preferably set to a short time. For example, when the drying temperature is 150 ° C., the drying time is preferably set within 30 minutes.
- the drying atmosphere may be any condition such as an air atmosphere, a nitrogen atmosphere, an argon atmosphere, a vacuum atmosphere, or a reduced pressure atmosphere with a controlled oxygen concentration.
- the coating film obtained by applying the coating solution for forming the second gas barrier layer 22b may include a step of removing moisture before application of energy or during application of energy.
- a form of dehumidification while maintaining a low humidity environment is preferable. Since humidity in a low-humidity environment varies depending on temperature, a preferable form is shown for the relationship between temperature and humidity by defining the dew point temperature.
- the preferable dew point temperature is 4 ° C. or lower (temperature 25 ° C./humidity 25%), the more preferable dew point temperature is ⁇ 5 ° C. or lower (temperature 25 ° C./humidity 10%), and the time to be maintained is that of the second gas barrier layer 22b.
- the dew point temperature is ⁇ 5 ° C. or less and the maintaining time is 1 minute or more.
- the lower limit of the dew point temperature is not particularly limited, but is usually ⁇ 50 ° C. or higher, and preferably ⁇ 40 ° C. or higher. From the viewpoint of promoting the dehydration reaction of the second gas barrier layer 22b converted to silanol by removing water before or during the reforming process.
- the coating film formed as described above to perform a conversion reaction of polysilazane to silicon oxide, silicon oxynitride or the like, and the second gas barrier layer 22b is an inorganic material that exhibits gas barrier properties. Modification to a thin film is performed.
- the conversion reaction of polysilazane to silicon oxide or silicon oxynitride can be applied by appropriately selecting a known method.
- Specific examples of the modification treatment include plasma treatment, ultraviolet irradiation treatment, and heat treatment.
- modification by heat treatment formation of a silicon oxide film or a silicon oxynitride layer by a substitution reaction of a silicon compound requires a high temperature of 450 ° C. or higher, so it is difficult to adapt to a flexible substrate such as plastic. . For this reason, it is preferable to perform the heat treatment in combination with other reforming treatments.
- a plasma treatment capable of a conversion reaction at a lower temperature or a conversion reaction by an ultraviolet irradiation treatment is preferable.
- plasma treatment and ultraviolet irradiation treatment which are preferable modification treatment methods, will be described.
- the plasma treatment that can be used as the modification treatment a known method can be used, and an atmospheric pressure plasma treatment or the like can be preferably used.
- the atmospheric pressure plasma CVD method which performs plasma CVD processing near atmospheric pressure, does not need to be reduced in pressure and is more productive than the plasma CVD method under vacuum.
- the film speed is high, and further, under a high pressure condition under atmospheric pressure as compared with the conditions of a normal CVD method, the gas mean free process is very short, so that a very homogeneous film can be obtained.
- nitrogen gas or a gas containing Group 18 atoms of the long-period periodic table specifically helium, neon, argon, krypton, xenon, radon, or the like is used.
- nitrogen, helium, and argon are preferably used, and nitrogen is particularly preferable because of low cost.
- UV irradiation treatment As one of the modification treatment methods, treatment by ultraviolet irradiation is preferable. Ozone and active oxygen atoms generated by ultraviolet rays (synonymous with ultraviolet light) have high oxidation ability, and can form silicon oxide films or silicon oxynitride films with high density and insulation at low temperatures. It is.
- the base material is heated, and O 2 and H 2 O contributing to ceramicization (silica conversion), an ultraviolet absorber, and polysilazane itself are excited and activated.
- the conversion to ceramics is promoted, and the obtained second gas barrier layer 22b becomes denser. Irradiation with ultraviolet rays is effective at any time after the formation of the coating film.
- ultraviolet rays refer to electromagnetic waves having a wavelength of 10 to 400 nm, but in the case of ultraviolet irradiation treatment other than vacuum ultraviolet ray (10 to 200 nm) treatment described later, preferably ultraviolet rays of 210 to 375 nm are used.
- the irradiation intensity and the irradiation time are set within the range where the base material carrying the irradiated second gas barrier layer 22b is not damaged.
- a plastic film for example, a 2 kW (80 W / cm ⁇ 25 cm) lamp is used, and the strength of the base material surface is 20 to 300 mW / cm 2 , preferably 50 to 200 mW / cm.
- the distance between the base material and the ultraviolet irradiation lamp is set so as to be 2, and irradiation can be performed for 0.1 seconds to 10 minutes.
- the substrate temperature during ultraviolet irradiation treatment is 150 ° C. or more
- the properties of the substrate are impaired, such as deformation of the substrate or deterioration of its strength.
- a modification treatment at a higher temperature is possible.
- the substrate temperature at the time of ultraviolet irradiation there is no general upper limit for the substrate temperature at the time of ultraviolet irradiation, and it can be appropriately set by those skilled in the art depending on the type of substrate.
- UV ray generating means examples include metal halide lamps, high pressure mercury lamps, low pressure mercury lamps, xenon arc lamps, carbon arc lamps, and excimer lamps (single wavelengths of 172 nm, 222 nm, and 308 nm, for example, USHIO INC. Manufactured by M.D. Com Co., Ltd.), UV light laser, and the like, but are not particularly limited.
- the UV light from the generation source is reflected by the reflector and then applied to the second gas barrier layer 22b. It is preferable to apply.
- UV irradiation can be applied to both batch processing and continuous processing, and can be appropriately selected depending on the shape of the substrate used.
- the laminate having the second gas barrier layer 22b on the surface can be processed in an ultraviolet baking furnace equipped with the above-described ultraviolet ray generation source.
- the ultraviolet baking furnace itself is generally known.
- an ultraviolet baking furnace manufactured by I-Graphics Co., Ltd. can be used.
- the laminated body which has the 2nd gas barrier layer 22b on the surface is a long film shape, it irradiates with an ultraviolet-ray continuously in the drying zone provided with the above ultraviolet-ray generation sources, conveying this. Can be made into ceramics.
- the time required for ultraviolet irradiation is generally 0.1 seconds to 10 minutes, preferably 0.5 seconds to 3 minutes, depending on the substrate used and the composition and concentration of the second gas barrier layer 22b.
- the most preferable modification treatment method is treatment by excimer irradiation with vacuum ultraviolet rays (excimer irradiation treatment).
- the treatment by the vacuum ultraviolet irradiation uses light energy of 100 to 200 nm, preferably light energy of a wavelength of 100 to 180 nm, which is larger than the interatomic bonding force in the polysilazane compound, and bonds atoms with only photons called photon processes.
- This is a method of forming a silicon oxide film at a relatively low temperature (about 200 ° C. or lower) by causing an oxidation reaction with active oxygen or ozone to proceed while cutting directly by action.
- the radiation source can be any light source that generates light with a wavelength of 100-180 nm, but is preferably an excimer radiator having a maximum emission at about 172 nm (eg, Xe excimer lamp), a low-pressure mercury vapor having an emission line at about 185 nm. Lamps, and medium and high pressure mercury vapor lamps with wavelength components of 230 nm or less, and excimer lamps with maximum emission at about 222 nm.
- an excimer radiator having a maximum emission at about 172 nm (eg, Xe excimer lamp), a low-pressure mercury vapor having an emission line at about 185 nm.
- the Xe excimer lamp emits ultraviolet light having a short wavelength of 172 nm at a single wavelength, and thus has excellent luminous efficiency. Since this light has a large oxygen absorption coefficient, it can generate radical oxygen atom species and ozone at a high concentration with a very small amount of oxygen. Moreover, it is known that the energy of light having a short wavelength of 172 nm has a high ability to dissociate organic bonds. Due to the high energy possessed by the active oxygen, ozone and ultraviolet radiation, the polysilazane coating can be modified in a short time.
- ⁇ Excimer lamps have high light generation efficiency and can be lit with low power.
- light having a long wavelength that causes a temperature increase due to light is not emitted, and energy is irradiated in the ultraviolet region, that is, in a short wavelength, so that the increase in the surface temperature of the target object is suppressed.
- it is suitable for flexible film materials such as PET, which are likely to be affected by heat.
- Oxygen is necessary for the reaction at the time of ultraviolet irradiation, but since vacuum ultraviolet rays are absorbed by oxygen, the efficiency in the ultraviolet irradiation process is likely to decrease. It is preferable to carry out in a state where the water vapor concentration is low. That is, the oxygen concentration at the time of irradiation with vacuum ultraviolet rays is preferably 10 to 20,000 volume ppm (0.001 to 2 volume%), and preferably 50 to 10,000 volume ppm (0.005 to 1 volume%). More preferably. Also, the water vapor concentration during the conversion process is preferably in the range of 1000 to 4000 ppm by volume.
- the gas satisfying the irradiation atmosphere used at the time of irradiation with vacuum ultraviolet rays is preferably a dry inert gas, and particularly preferably dry nitrogen gas from the viewpoint of cost.
- the oxygen concentration can be adjusted by measuring the flow rate of oxygen gas and inert gas introduced into the irradiation chamber and changing the flow rate ratio.
- the illuminance of the vacuum ultraviolet ray on the coating surface received by the polysilazane coating is preferably 1 mW / cm 2 to 10 W / cm 2 , more preferably 30 mW / cm 2 to 200 mW / cm 2. and further preferably 50mW / cm 2 ⁇ 160mW / cm 2. If it is 1 mW / cm 2 or more, the reforming efficiency is improved, and if it is 10 W / cm 2 or less, ablation that can occur in the coating film and damage to the substrate can be reduced.
- the amount of irradiation energy (irradiation amount) of vacuum ultraviolet rays on the coating surface is preferably 100 mJ / cm 2 to 50 J / cm 2 , more preferably 200 mJ / cm 2 to 20 J / cm 2 , and 500 mJ / cm 2. More preferably, it is 2 to 10 J / cm 2 . If it is 100 mJ / cm 2 or more, modification is sufficient, and if it is 50 J / cm 2 or less, generation of cracks due to excessive modification and thermal deformation of the substrate can be suppressed.
- the vacuum ultraviolet ray to be used may be generated by plasma formed of a gas containing at least one of CO, CO 2 and CH 4 .
- the gas containing at least one of CO, CO 2 and CH 4 hereinafter also referred to as carbon-containing gas
- the carbon-containing gas may be used alone, but the rare gas or H 2 is used as the main gas. It is preferable to add a small amount of the contained gas.
- a plasma generation method capacitively coupled plasma or the like can be given.
- the composition distribution and thickness in the thickness direction of the region (b) can be obtained by measurement by a method using XPS (photoelectron spectroscopy) analysis as described below.
- the etching rate of the region (b) varies depending on the composition. For this reason, the thickness per layer is determined once based on the etching rate in terms of SiO 2 as a reference, and the layer interface is specified in the layered region based on the cross-sectional TEM image of the measurement sample. Ask for. While comparing this with the composition distribution in the thickness direction obtained from the XPS analysis, each layer in the composition distribution in the thickness direction is specified and obtained from the thickness of each region obtained from the corresponding XPS analysis and the cross-sectional TEM image. Further, a coefficient is uniformly applied to the thickness of each region obtained from the XPS analysis so that the thickness of each region matches. Thus, in the XPS analysis, correction in the thickness direction is performed.
- the etching depth per measurement point (corresponding to the following sputter ion and depth profile conditions) is 1 to 15 nm even if the apparatus and measurement conditions change.
- the resolution in the thickness direction of 1 to 10 nm can be applied without any problem.
- a gas barrier film is prepared by using the following FIB processing apparatus, and then a cross-sectional TEM observation is performed according to a conventional method. In this way, the thickness of each region can be calculated.
- An example that can be used for FIB processing and TEM observation is shown below.
- the third gas barrier layer 22c contains a metal oxide having a lower oxidation-reduction potential than silicon as a main component.
- the third gas barrier layer 22c may be a single layer or a laminated structure of two or more layers. When the third gas barrier layer 22c has a laminated structure of two or more layers, the third gas barrier layer 22c may have the same composition or a different composition.
- the thickness of the third gas barrier layer 22c (the total thickness in the case of a laminated structure of two or more layers) is not particularly limited, but is preferably 1 to 500 nm, and more preferably 5 to 200 nm. If it is this range, the advantage that sufficient gas barrier property improvement effect is acquired within the range of the film-forming tact time with high productivity is acquired.
- the third gas barrier layer 22c alone containing a metal oxide whose oxidation-reduction potential is lower than that of silicon as a main component does not have, for example, a high gas barrier property enough to reduce dark spots of an organic EL element.
- it is oxidized before the region (b) of the second gas barrier layer 22b.
- the oxidation suppression effect with respect to the surface of the 2nd gas barrier layer 22b is exhibited, and it is thought that it becomes difficult to produce spot-like gas barrier property fall. Therefore, by providing the third gas barrier layer 22c, durability of the gas barrier film in a high temperature and high humidity environment is improved.
- the phrase “comprising a metal oxide having a lower redox potential than silicon as a main component” in the third gas barrier layer 22c means that the content of the metal oxide having a lower redox potential than silicon is the third gas barrier layer 22c. It means that it is 50 mass% or more with respect to the total mass of. The content is more preferably 80% by mass or more, further preferably 95% by mass or more, particularly preferably 98% by mass or more, and 100% by mass (the third gas barrier layer 22c is made of silicon). Also, it is most preferable that only a metal oxide having a low redox potential).
- the metal having a lower redox potential than silicon include niobium, tantalum, zirconium, titanium, hafnium, magnesium, yttrium, aluminum, and the like. These metals may be used alone or in combination of two or more. Among these, at least one metal selected from the group consisting of niobium, tantalum, zirconium, and titanium is preferable. That is, it is preferable that the third gas barrier layer 22c contains, as a main component, an oxide of at least one metal selected from the group consisting of niobium, tantalum, zirconium, and titanium.
- Table 1 shows the standard redox potentials of major metals.
- the third gas barrier layer 22c more preferably contains an oxide of at least one of niobium and tantalum as a main component from the viewpoint that an oxidation suppressing effect on the surface of the second gas barrier layer 22b is easily exhibited.
- the third gas barrier layer 22c may contain another compound as long as it contains a metal oxide having a lower oxidation-reduction potential than silicon as a main component. Examples of other compounds include hafnium, magnesium, yttrium, and aluminum. These other compounds can be used alone or in combination of two or more.
- the method for forming the third gas barrier layer 22c is not particularly limited, and examples thereof include physical vapor deposition (PVD) methods such as sputtering, vapor deposition, and ion plating, and plasma CVD (plasma-enhanced chemical vapor deposition, PECVD). And chemical vapor deposition such as ALD (Atomic Layer Deposition).
- PVD physical vapor deposition
- PECVD plasma CVD
- ALD Atomic Layer Deposition
- Films formed by sputtering include conventional techniques such as DC (direct current) sputtering, RF (high frequency) sputtering, a combination of these magnetron sputtering, and dual magnetron (DMS) sputtering using an intermediate frequency range. These can be used alone or in combination of two or more.
- a reactive sputtering method using a transition mode that is intermediate between the metal mode and the oxide mode can also be used. By controlling the sputtering phenomenon so as to be in the transition region, a metal oxide film can be formed at a high film formation speed, which is preferable.
- a metal having a lower redox potential than silicon is used as a target, and oxygen is introduced into the process gas to oxidize a metal having a lower redox potential than silicon.
- a thin film of an object can be formed.
- RF radio frequency
- a metal oxide target having a lower oxidation-reduction potential than silicon can be used.
- an inert gas such as He, Ne, Ar, Kr, or Xe, or at least one process gas selected from oxygen, nitrogen, carbon dioxide, and carbon monoxide can be used.
- Examples of film formation conditions in the sputtering method include applied power, discharge current, discharge voltage, time, and the like, which can be appropriately selected according to the sputtering apparatus, film material, film thickness, and the like.
- a sputtering method using a metal oxide having a lower oxidation-reduction potential than silicon as a target is preferable because it has a higher film formation rate and higher productivity.
- the gas barrier film may include other layers in addition to the above-described barrier layer.
- layers having various functions such as an anchor coat layer and a smooth layer can be provided.
- An anchor coat layer may be formed on the surface of the resin substrate 1 on the side where the gas barrier layer 22 is formed for the purpose of improving the adhesion with the gas barrier layer 22.
- the thickness of the anchor coat layer is not particularly limited, but is preferably about 0.5 to 10 ⁇ m.
- polyester resins As anchor coating agents used in the anchor coat layer, polyester resins, isocyanate resins, urethane resins, acrylic resins, ethylene vinyl alcohol resins, vinyl modified resins, epoxy resins, modified styrene resins, modified silicone resins, alkyl titanates, etc. are used alone. Or in combination of two or more.
- the above-mentioned anchor coating agent is coated on the support by a known method such as roll coating, gravure coating, knife coating, dip coating, spray coating, etc., and anchor coating is performed by drying and removing the solvent, diluent, etc. be able to.
- the application amount of the anchor coating agent is preferably about 0.1 to 5.0 g / m 2 (dry state).
- the anchor coat layer can be formed by a vapor phase method such as physical vapor deposition or chemical vapor deposition.
- a vapor phase method such as physical vapor deposition or chemical vapor deposition.
- an inorganic film mainly composed of silicon oxide can be formed for the purpose of improving adhesion and the like.
- an anchor coat layer as described in Japanese Patent Application Laid-Open No. 2004-314626, when an inorganic thin film is formed thereon by a vapor phase method, the gas generated from the substrate side is blocked to some extent.
- an anchor coat layer can be formed for the purpose of controlling the composition of the inorganic thin film.
- a smooth layer In a gas barrier film, you may have a smooth layer between the resin base material 1 and the 1st gas barrier layer 22a.
- a smooth layer is provided in order to planarize the rough surface of the resin base material 1 in which a protrusion etc. exist.
- the thickness of the smooth layer is preferably in the range of 1 to 10 ⁇ m, more preferably in the range of 2 to 7 ⁇ m, from the viewpoint of improving the heat resistance of the film and facilitating the balance adjustment of the optical properties of the film. Is preferred.
- the smooth layer is basically produced by curing a photosensitive material or a thermosetting material.
- the photosensitive material include a resin composition containing an acrylate compound having a radical reactive unsaturated compound, a resin composition containing an acrylate compound and a mercapto compound having a thiol group, epoxy acrylate, urethane acrylate, polyester acrylate, Examples thereof include resin compositions in which polyfunctional acrylate monomers such as polyether acrylate, polyethylene glycol acrylate, and glycerol methacrylate are dissolved.
- OPSTAR registered trademark
- thermosetting materials include TutProm Series (Organic Polysilazane) manufactured by Clariant, SP COAT heat-resistant clear paint manufactured by Ceramic Co., Ltd., Nanohybrid Silicone manufactured by Adeka, and Unidic manufactured by DIC.
- the method for forming the smooth layer is not particularly limited, but is preferably formed by a wet coating method such as a spin coating method, a spray method, a blade coating method, a dip method, or a dry coating method such as an evaporation method.
- a wet coating method such as a spin coating method, a spray method, a blade coating method, a dip method, or a dry coating method such as an evaporation method.
- additives such as an antioxidant, an ultraviolet absorber, and a plasticizer can be added to the above-described photosensitive resin as necessary.
- an appropriate resin or additive may be used in order to improve the film formability and prevent the generation of pinholes in the film.
- the smoothness of the smooth layer is a value expressed by the surface roughness defined by JIS B 0601: 2001, and the 10-point average roughness Rz is preferably 10 nm or more and 30 nm or less. If it is this range, even if it is a case where a barrier layer is apply
- Embodiment of Organic Electroluminescence Device> an embodiment of an organic electroluminescence element (organic EL element) using the gas barrier film described above will be described.
- the organic EL element of the present embodiment has a configuration in which electrodes (anode and cathode) and a light emitting unit are provided on the above gas barrier film.
- the gas barrier film of the organic EL element is the same as the above-described embodiment of the gas barrier film. For this reason, detailed description of the gas barrier film is omitted in the description of the organic EL element.
- FIG. 4 the schematic block diagram (sectional drawing) of the organic EL element of this embodiment is shown.
- a gas barrier film 21, a first electrode 23, a light emitting unit 26 having an organic functional layer, and a second electrode 25 are laminated in this order.
- a sealing layer 27 and a sealing member 28 are provided on the second electrode 25.
- the organic EL element has a so-called bottom emission type configuration in which light from the light emitting unit 26 is extracted from the gas barrier film 21 side.
- the gas barrier film 21 includes the resin base material 1, and the first gas barrier layer 22a, the second gas barrier layer 22b, and the third gas barrier layer 22c provided on the resin base material 1.
- An electrode consists of the 1st electrode 23 and the 2nd electrode 25, and comprises the cathode or anode of an organic EL element, respectively.
- the organic functional layer has a light emitting layer containing at least an organic material, and may further include another layer between the light emitting layer and the electrode.
- anode / light emitting layer / cathode (2) Anode / light emitting layer / electron transport layer / cathode (3) Anode / hole transport layer / light emitting layer / cathode (4) Anode / hole transport layer / light emitting layer / electron Transport layer / cathode (5) anode / hole transport layer / light emitting layer / electron transport layer / electron injection layer / cathode (6) anode / hole injection layer / hole transport layer / light emitting layer / electron transport layer / cathode ( 7) Anode / hole injection layer / hole transport layer / (electron blocking layer /) luminescent layer / (hole blocking layer /) electron transport layer / electron injection layer / cathode Among
- the layer excluding the anode and the cathode is an organic functional layer.
- a unit (unit) mainly composed of an organic functional layer including at least the light emitting layer is a light emitting unit, and the light emitting unit is sandwiched between an anode and a cathode to constitute an organic EL element as a whole.
- the light emitting layer is formed of a single layer or a plurality of layers.
- a non-light emitting intermediate connector layer may be provided between the light emitting layers.
- a hole blocking layer (hole blocking layer), an electron injection layer (cathode buffer layer), or the like may be provided between the light emitting layer and the cathode, and between the light emitting layer and the anode.
- An electron blocking layer (electron barrier layer), a hole injection layer (anode buffer layer), or the like may be provided.
- the electron transport layer is a layer having a function of transporting electrons.
- the electron transport layer includes an electron injection layer and a hole blocking layer in a broad sense.
- the electron transport layer may be composed of a plurality of layers.
- the hole transport layer is a layer having a function of transporting holes.
- the hole transport layer includes a hole injection layer and an electron blocking layer in a broad sense.
- the hole transport layer may be composed of a plurality of layers.
- the organic EL element may be an element having a so-called tandem structure in which a plurality of light emitting units 26 including at least one light emitting layer are stacked.
- Examples of typical element configurations of the tandem structure include the following configurations. Anode / first light emitting unit / intermediate connector layer / second light emitting unit / intermediate connector layer / third light emitting unit / cathode
- the first light emitting unit, the second light emitting unit, and the third light emitting unit may all be the same or different. Further, the two light emitting units may be the same, and the remaining one may be different.
- the plurality of light emitting units 26 may be directly stacked or may be stacked via an intermediate connector layer.
- the intermediate connector layer is also commonly referred to as an intermediate electrode, intermediate conductive layer, charge generation layer, electron extraction layer, connection layer, or intermediate insulating layer. Electrons are transferred to the anode side adjacent layer and holes are connected to the cathode side adjacent layer.
- a known material structure can be used as long as the layer has a function of supplying. Examples of materials used for the intermediate connector layer include ITO (indium tin oxide), IZO (indium zinc oxide), ZnO 2 , TiN, ZrN, HfN, TiO x , VO x , CuI, InN, and GaN.
- Examples of a preferable configuration in the light emitting unit 26 include, but are not limited to, a configuration in which the anode and the cathode are removed from the configuration described in the representative element configuration.
- Specific examples of the tandem organic EL element include, for example, US Pat. No. 6,337,492, US Pat. No. 7,420,203, US Pat. No. 7,473,923, US Pat. No. 6,872,472, US Pat. No. 6,107,734. Specification, US Pat. No.
- the present invention is not limited to these.
- the light-emitting layer used in the organic EL element is a layer that provides a field in which electrons and holes injected from an electrode or an adjacent layer are recombined to emit light via excitons.
- the light emitting portion may be within the layer of the light emitting layer or may be the interface between the light emitting layer and the adjacent layer.
- the total sum of the thicknesses of the light emitting layers is not particularly limited, and is determined from the viewpoints of the uniformity of the film to be formed, the voltage required at the time of light emission, and the stability of the emitted color with respect to the driving current.
- the total thickness of the light emitting layers is preferably adjusted in the range of 2 nm to 5 ⁇ m, more preferably adjusted in the range of 2 to 500 nm, and further preferably adjusted in the range of 5 to 200 nm.
- the thickness of each light emitting layer is preferably adjusted within the range of 2 nm to 1 ⁇ m, more preferably adjusted within the range of 2 to 200 nm, and further preferably adjusted within the range of 3 to 150 nm.
- the light emitting layer preferably contains a light emitting dopant (a light emitting dopant compound, a dopant compound, also simply referred to as a dopant) and a host compound (a matrix material, a light emitting host compound, also simply referred to as a host).
- a light emitting dopant a light emitting dopant compound, a dopant compound, also simply referred to as a dopant
- a host compound a matrix material, a light emitting host compound, also simply referred to as a host.
- Luminescent dopant As the light-emitting dopant used in the light-emitting layer, a fluorescent light-emitting dopant (also referred to as a fluorescent dopant or a fluorescent compound) and a phosphorescent dopant (also referred to as a phosphorescent dopant or a phosphorescent compound) are preferably used. Of these, at least one light emitting layer preferably contains a phosphorescent dopant.
- the concentration of the light emitting dopant in the light emitting layer can be arbitrarily determined based on the specific dopant used and the requirements of the device.
- the concentration of the light emitting dopant may be contained at a uniform concentration in the film thickness direction of the light emitting layer, or may have an arbitrary concentration distribution.
- the light emitting layer may contain a plurality of types of light emitting dopants. For example, a combination of dopants having different structures, or a combination of a fluorescent luminescent dopant and a phosphorescent luminescent dopant may be used. Thereby, arbitrary luminescent colors can be obtained.
- the color emitted by the organic EL element is shown in Fig. 4.16 on page 108 of the "New Color Science Handbook” (edited by the Japan Society for Color Science, University of Tokyo Press, 1985).
- the spectral radiance meter CS-2000 Konica Minolta Co., Ltd. It is determined by the color when the result measured in ()) is applied to the CIE chromaticity coordinates.
- the light emitting layer of one layer or a plurality of layers contains a plurality of light emitting dopants having different light emission colors and emits white light.
- the combination of light-emitting dopants that exhibit white but examples include a combination of blue and orange, a combination of blue, green, and red.
- the phosphorescent dopant is a compound in which light emission from an excited triplet is observed.
- the phosphorescent dopant is a compound that emits phosphorescence at room temperature (25 ° C.), and has a phosphorescence quantum yield of 0 at 25 ° C. .01 or more compounds.
- a preferable phosphorescence quantum yield is 0.1 or more.
- the phosphorescent quantum yield can be measured by the method described in Spectroscopic II, page 398 (1992 edition, Maruzen) of the Fourth Edition Experimental Chemistry Course 7.
- the phosphorescence quantum yield in a solution can be measured using various solvents.
- the phosphorescence emitting dopant used for the light emitting layer should just achieve the said phosphorescence quantum yield (0.01 or more) in any solvent.
- an excited state of the host compound is generated by recombination of carriers on the host compound to which carriers are transported.
- a phosphorescent dopant By transferring this energy to a phosphorescent dopant, it is an energy transfer type in which light emission from the phosphorescent dopant is obtained.
- the other is a carrier trap type in which a phosphorescent dopant becomes a carrier trap, carrier recombination occurs on the phosphorescent dopant, and light emission from the phosphorescent dopant is obtained.
- it is a condition that the excited state energy of the phosphorescent dopant is lower than the excited state energy of the host compound.
- the phosphorescent dopant can be appropriately selected from known materials used for the light emitting layer of the organic EL element. Specific examples of known phosphorescent dopants include compounds described in the following documents.
- a preferable phosphorescent dopant is an organometallic complex having Ir as a central metal. More preferably, a complex containing at least one coordination mode of metal-carbon bond, metal-nitrogen bond, metal-oxygen bond, and metal-sulfur bond is preferable.
- the electron transport layer used for the organic EL element is made of a material having a function of transporting electrons, and has a function of transmitting electrons injected from the cathode to the light emitting layer.
- An electron transport material may be used independently and may be used in combination of multiple types.
- the total thickness of the electron transport layer is not particularly limited, but is usually in the range of 2 nm to 5 ⁇ m, more preferably in the range of 2 to 500 nm, and still more preferably in the range of 5 to 200 nm.
- the organic EL element when the light generated in the light emitting layer is extracted from the electrode, the light extracted directly from the light emitting layer and the light extracted after being reflected by the electrode from which the light is extracted and the electrode located at the counter electrode are: It is known to cause interference. When light is reflected by the cathode, this interference effect can be efficiently utilized by appropriately adjusting the total film thickness of the electron transport layer between several nanometers and several micrometers. On the other hand, since the voltage is likely to increase when the thickness of the electron transport layer is increased, the electron mobility of the electron transport layer is preferably 10 ⁇ 5 cm 2 / Vs or more, particularly when the thickness is large. .
- the material used for the electron transport layer may have either an electron injecting or transporting property or a hole blocking property. Any one can be selected and used.
- Examples include nitrogen-containing aromatic heterocyclic derivatives, aromatic hydrocarbon ring derivatives, dibenzofuran derivatives, dibenzothiophene derivatives, silole derivatives, and the like.
- nitrogen-containing aromatic heterocyclic derivatives examples include carbazole derivatives, azacarbazole derivatives (one or more carbon atoms constituting the carbazole ring are substituted with nitrogen atoms), pyridine derivatives, pyrimidine derivatives, pyrazine derivatives, pyridazine derivatives, triazine derivatives.
- aromatic hydrocarbon ring derivative examples include naphthalene derivatives, anthracene derivatives, triphenylene and the like.
- a metal complex having a quinolinol skeleton or a dibenzoquinolinol skeleton as a ligand such as tris (8-quinolinol) aluminum (Alq 3 ), tris (5,7-dichloro-8-quinolinol) aluminum, tris (5,7 -Dibromo-8-quinolinol) aluminum, tris (2-methyl-8-quinolinol) aluminum, tris (5-methyl-8-quinolinol) aluminum, bis (8-quinolinol) zinc (Znq), etc., and their metals
- a metal complex in which the central metal of the complex is replaced with In, Mg, Cu, Ca, Sn, Ga, or Pb can also be used as the electron transport material.
- metal-free or metal phthalocyanine, or those having the terminal substituted with an alkyl group or a sulfonic acid group can be preferably used as the electron transporting material.
- the distyrylpyrazine derivative exemplified as the material for the light emitting layer can also be used as an electron transport material, and an inorganic semiconductor such as n-type-Si, n-type-SiC, etc. as in the case of the hole injection layer and the hole transport layer. Can also be used as an electron transporting material.
- a polymer material in which these materials are introduced into a polymer chain or these materials are used as a polymer main chain can also be used.
- a doping material may be doped into the electron transport layer as a guest material to form an electron transport layer having a high n property (electron rich).
- the doping material include metal compounds such as metal complexes and metal halides, and other n-type dopants.
- Specific examples of the electron transport layer having such a structure include, for example, JP-A-4-297076, JP-A-10-270172, JP-A-2000-196140, 2001-102175, J. Appl. Phys., 95, 5773 (2004) and the like.
- preferable electron transport materials used in the organic EL device include, but are not limited to, compounds described in the following documents.
- More preferable electron transport materials include pyridine derivatives, pyrimidine derivatives, pyrazine derivatives, triazine derivatives, dibenzofuran derivatives, dibenzothiophene derivatives, carbazole derivatives, azacarbazole derivatives, and benzimidazole derivatives.
- the hole blocking layer is a layer having a function of an electron transport layer in a broad sense. Preferably, it is made of a material having a function of transporting electrons and a small ability to transport holes. By blocking holes while transporting electrons, the recombination probability of electrons and holes can be improved. Moreover, the structure of the above-mentioned electron carrying layer can be used as a hole-blocking layer as needed.
- the hole blocking layer provided in the organic EL element is preferably provided adjacent to the cathode side of the light emitting layer.
- the thickness of the hole blocking layer is preferably in the range of 3 to 100 nm, more preferably in the range of 5 to 30 nm.
- the material used for the hole blocking layer the material used for the above-described electron transport layer is preferably used, and the material used as the above-described host compound is also preferably used for the hole blocking layer.
- the electron injection layer (also referred to as “cathode buffer layer”) is a layer provided between the cathode and the light emitting layer in order to lower the driving voltage and improve the light emission luminance.
- An example of an electron injection layer can be found in the second chapter, Chapter 2, “Electrode Materials” (pages 123-166) of “Organic EL devices and their industrialization front line (issued by NTT Corporation on November 30, 1998)”. Are listed.
- the electron injection layer is provided as necessary, and is provided between the cathode and the light emitting layer or between the cathode and the electron transport layer as described above.
- the electron injection layer is preferably a very thin film, and the film thickness is preferably in the range of 0.1 to 5 nm, although it depends on the material.
- the constituent material may be a non-uniform film that exists intermittently.
- JP-A-6-325871, JP-A-9-17574, and JP-A-10-74586 Specific examples of materials preferably used for the electron injection layer include metals typified by strontium and aluminum, alkali metal compounds typified by lithium fluoride, sodium fluoride, and potassium fluoride, magnesium fluoride, and fluoride. Examples thereof include alkaline earth metal compounds typified by calcium, metal oxides typified by aluminum oxide, metal complexes typified by lithium 8-hydroxyquinolate (Liq), and the like.
- the material used for said electron injection layer may be used independently, and may be used in combination of multiple types.
- the hole transport layer is made of a material having a function of transporting holes.
- the hole transport layer is a layer having a function of transmitting holes injected from the anode to the light emitting layer.
- the total thickness of the hole transport layer is not particularly limited, but is usually not in the range of 5 nm to 5 ⁇ m, more preferably in the range of 2 to 500 nm, and further preferably in the range of 5 to 200 nm. Within range.
- the material used for the hole transport layer (hereinafter referred to as a hole transport material) only needs to have either a hole injecting or transporting property or an electron blocking property.
- a hole transport material an arbitrary material can be selected and used from conventionally known compounds.
- the hole transport material may be used alone or in combination of two or more.
- Hole transport materials include, for example, porphyrin derivatives, phthalocyanine derivatives, oxazole derivatives, oxadiazole derivatives, triazole derivatives, imidazole derivatives, pyrazoline derivatives, pyrazolone derivatives, phenylenediamine derivatives, hydrazone derivatives, stilbene derivatives, polyarylalkane derivatives, tria.
- Reelamine derivatives carbazole derivatives, indolocarbazole derivatives, isoindole derivatives, acene derivatives such as anthracene and naphthalene, fluorene derivatives, fluorenone derivatives, polyvinyl carbazole, polymer materials with aromatic amines introduced into the main chain or side chain, or Oligomer, polysilane, conductive polymer or oligomer (eg, PEDOT: PSS, aniline copolymer, polyaniline, polythiophene, etc.) And the like.
- PEDOT PEDOT: PSS, aniline copolymer, polyaniline, polythiophene, etc.
- triarylamine derivative examples include a benzidine type typified by ⁇ -NPD, a starburst type typified by MTDATA, and a compound having fluorene or anthracene in the triarylamine linking core part.
- hexaazatriphenylene derivatives described in JP-T-2003-519432 and JP-A-2006-135145 can also be used as the hole transport material.
- a hole transport layer having a high p property doped with impurities can also be used.
- the configurations described in JP-A-4-297076, JP-A-2000-196140, 2001-102175, J. Appl. Phys., 95, 5773 (2004), etc. It can also be applied to the transport layer.
- Inorganic compounds such as -Si and p-type -SiC can also be used. Further, ortho-metalated organometallic complexes having Ir or Pt as a central metal as typified by Ir (ppy) 3 are also preferably used.
- the above-mentioned materials can be used, and triarylamine derivatives, carbazole derivatives, indolocarbazole derivatives, azatriphenylene derivatives, organometallic complexes, and aromatic amines in the main chain or side chain.
- the introduced polymer material or oligomer is preferably used.
- the hole transport material used for the organic EL element include, but are not limited to, the compounds described in the following documents in addition to the documents listed above. Appl. Phys. Lett. 69, 2160 (1996), J. Lumin. 72-74, 985 (1997), Appl. Phys. Lett. 78, 673 (2001), Appl. Phys. Lett. 90, 183503 (2007) ), Appl. Phys. Lett. 90, 183503 (2007), Appl. Phys. Lett. 51, 913 (1987), Synth. Met. 87, 171 (1997), Synth. Met. 91, 209 (1997), Synth. Met.
- the electron blocking layer is a layer having a function of a hole transport layer in a broad sense. Preferably, it is made of a material having a function of transporting holes and a small ability to transport electrons.
- the electron blocking layer can improve the probability of recombination of electrons and holes by blocking electrons while transporting holes.
- the structure of the above-described hole transport layer can be used as an electron blocking layer of an organic EL element as necessary.
- the electron blocking layer provided in the organic EL element is preferably provided adjacent to the anode side of the light emitting layer.
- the thickness of the electron blocking layer is preferably in the range of 3 to 100 nm, and more preferably in the range of 5 to 30 nm.
- the materials used for the electron blocking layer can be preferably used.
- the material used as the above-mentioned host compound can also be preferably used as the electron blocking layer.
- the hole injection layer (also referred to as “anode buffer layer”) is a layer provided between the anode and the light emitting layer in order to lower the driving voltage and improve the light emission luminance.
- An example of the hole injection layer is “Organic EL device and its industrialization front line (November 30, 1998, issued by NTT)”, Chapter 2, Chapter 2, “Electrode material” (pages 123-166). It is described in.
- the hole injection layer is provided as necessary, and is provided between the anode and the light emitting layer or between the anode and the hole transport layer as described above.
- Examples of the material used for the hole injection layer include the materials used for the hole transport layer described above. Among them, phthalocyanine derivatives typified by copper phthalocyanine, hexaazatriphenylene derivatives as described in JP-T-2003-519432 and JP-A 2006-135145, metal oxides typified by vanadium oxide, amorphous carbon, polyaniline ( Preferred are conductive polymers such as emeraldine) and polythiophene, orthometalated complexes represented by tris (2-phenylpyridine) iridium complex, and triarylamine derivatives.
- the materials used for the hole injection layer described above may be used alone or in combination of two or more.
- the organic functional layer constituting the organic EL element may further contain other additives.
- other additives include halogen elements and halogenated compounds such as bromine, iodine and chlorine, alkali metals and alkaline earth metals such as Pd, Ca, and Na, transition metal compounds, complexes, and salts.
- the content of the additive can be arbitrarily determined, but is preferably 1000 ppm or less, more preferably 500 ppm or less, and further preferably 50 ppm or less with respect to the total mass% of the contained layer. . However, it is not within this range depending on the purpose of improving the transportability of electrons and holes or the purpose of favoring the exciton energy transfer.
- a method for forming an organic functional layer (hole injection layer, hole transport layer, light emitting layer, hole blocking layer, electron transport layer, electron injection layer, etc.) of the organic EL element will be described.
- the method for forming the organic functional layer is not particularly limited, and can be formed by a conventionally known method such as a vacuum deposition method or a wet method (wet process).
- Examples of the wet method include a spin coating method, a casting method, an ink jet method, a printing method, a die coating method, a blade coating method, a roll coating method, a spray coating method, a curtain coating method, and an LB method (Langmuir-Blodgett method).
- a method having high suitability for a roll-to-roll method such as a die coating method, a roll coating method, an ink jet method, or a spray coating method is preferable.
- liquid medium for dissolving or dispersing the organic functional layer material in the wet method examples include ketones such as methyl ethyl ketone and cyclohexanone, fatty acid esters such as ethyl acetate, halogenated hydrocarbons such as dichlorobenzene, toluene, and xylene.
- Aromatic hydrocarbons such as mesitylene and cyclohexylbenzene, aliphatic hydrocarbons such as cyclohexane, decalin and dodecane, and organic solvents such as DMF and DMSO can be used.
- it can disperse
- the vapor deposition conditions vary depending on the type of compound used, but generally a boat heating temperature of 50 to 450 ° C. and a degree of vacuum of 10 ⁇ 6 to 10 ⁇ 2 Pa. Desirably, the deposition rate is 0.01 to 50 nm / second, the substrate temperature is ⁇ 50 to 300 ° C., the film thickness is 0.1 nm to 5 ⁇ m, and preferably 5 to 200 nm.
- the organic EL element is preferably formed from the organic functional layer to the cathode consistently by a single evacuation, but it may be taken out halfway and subjected to different film forming methods. In that case, it is preferable to perform the work in a dry inert gas atmosphere. Different formation methods may be applied for each layer.
- an electrode material made of a metal, an alloy, an electrically conductive compound, and a mixture thereof having a high work function (4 eV or more, preferably 4.3 V or more) is used.
- an electrode substance include metals such as Au and Ag, alloys thereof, and conductive transparent materials such as CuI, indium tin oxide (ITO), SnO 2 , and ZnO.
- conductive transparent materials such as CuI, indium tin oxide (ITO), SnO 2 , and ZnO.
- an amorphous material such as IDIXO (In 2 O 3 —ZnO) capable of forming a transparent conductive film may be used.
- a thin film is formed from these electrode materials by a method such as vapor deposition or sputtering, and a pattern having a desired shape is formed by a photolithography method.
- a pattern accuracy is not required so much (about 100 ⁇ m or more)
- the pattern may be formed through a mask having a desired shape when the electrode material is formed by vapor deposition or sputtering.
- a wet film forming method such as a printing method or a coating method can also be used.
- the transmittance be greater than 10%.
- the sheet resistance as the first electrode 23 is several hundred ⁇ / sq. The following is preferred.
- the thickness of the first electrode 23 is usually selected in the range of 10 nm to 1 ⁇ m, preferably 10 to 200 nm, although it depends on the material.
- the first electrode 23 is a layer composed mainly of silver, and is preferably composed of silver or an alloy mainly composed of silver.
- a method for forming the first electrode 23 a method using a wet process such as a coating method, an inkjet method, a coating method, a dip method, a vapor deposition method (resistance heating, EB method, etc.), a sputtering method, a CVD method, or the like. And a method using the dry process.
- the vapor deposition method is preferably applied.
- the alloy mainly composed of silver (Ag) constituting the first electrode 23 is silver magnesium (AgMg), silver copper (AgCu), silver palladium (AgPd), silver palladium copper (AgPdCu), silver indium (AgIn). ) And the like.
- the first electrode 23 as described above may have a configuration in which silver or an alloy layer mainly composed of silver is divided into a plurality of layers as necessary.
- the first electrode 23 preferably has a thickness of 20 nm or less and a thickness in the range of 4 to 15 nm.
- a thickness of 15 nm or less is preferable because the absorption component and reflection component of the layer are kept low and the light transmittance of the transparent barrier film is maintained. Further, when the thickness is 4 nm or more, the conductivity of the layer is also ensured.
- the first electrode 23 When a layer composed mainly of silver is formed as the first electrode 23, another conductive layer containing Pd or the like, or an organic layer such as a nitrogen compound or a sulfur compound is placed under the first electrode 23. It may be formed as a formation.
- the base layer By forming the base layer, it is possible to improve the film formation of a layer composed mainly of silver, to reduce the resistivity of the first electrode 23, and to improve the light transmittance of the first electrode 23. it can.
- Electrode material made of a metal (referred to as an electron injecting metal), an alloy, an electrically conductive compound, and a mixture thereof having a small work function (4 eV or less) is used.
- electrode materials include sodium, sodium-potassium alloy, magnesium, lithium, magnesium / copper mixture, magnesium / silver mixture, magnesium / aluminum mixture, magnesium / indium mixture, aluminum / aluminum oxide (Al 2 O 3 ) Mixtures, indium, lithium / aluminum mixtures, aluminum, rare earth metals and the like.
- a mixture of an electron injecting metal and a second metal having a work function value larger and more stable than that of the electron injecting metal for example, magnesium / Silver mixtures, magnesium / aluminum mixtures, magnesium / indium mixtures, aluminum / aluminum oxide (Al 2 O 3 ) mixtures, lithium / aluminum mixtures, aluminum and the like are preferred.
- the second electrode 25 can be manufactured by using the above electrode material by a method such as vapor deposition or sputtering.
- the sheet resistance of the second electrode 25 is several hundred ⁇ / sq. The following is preferred.
- the thickness of the second electrode 25 is usually selected in the range of 10 nm to 5 ⁇ m, preferably in the range of 50 to 200 nm.
- a conductive transparent material mentioned in the description of the first electrode is formed thereon, thereby forming a transparent or translucent first electrode.
- Two electrodes 25 can be produced. By applying this, an element in which both the first electrode 23 and the second electrode 25 are transmissive can be manufactured.
- the sealing member 28 is provided on one surface of the gas barrier film 21 on which the gas barrier layer 22 is formed via the sealing layer 27 that covers the first electrode 23, the light emitting unit 26, and the second electrode 25. Solid bonding is achieved by bonding. Solid sealing of the organic EL element is performed by dispersing and applying an uncured resin material at a plurality of locations on the bonding surface of the sealing member 28 or the gas barrier film 21, and sealing member through these resin materials. After pressing 28 and the gas barrier film 21 against each other, the resin material is cured to be integrated.
- the sealing layer 27 is provided in a state of covering at least the light emitting unit 26, and is provided in a state of exposing terminal portions (not shown) of the first electrode 23 and the second electrode 25. Further, an electrode may be provided on the sealing member 28 so that the terminal portions of the first electrode 23 and the second electrode 25 of the organic EL element are electrically connected to the electrode.
- the sealing layer 27 is made of a resin material (resin sealing layer) for joining the gas barrier film 21 and the sealing member 28.
- resin material resin sealing layer
- an inorganic material inorganic sealing layer
- the resin sealing layer is used for fixing the sealing member 28 to the gas barrier film 21 side. Further, it is used as a sealing agent for sealing the first electrode 23, the light emitting unit 26 and the second electrode 25 sandwiched between the sealing member 28 and the gas barrier film 21.
- sealing member 28 In order to join the sealing member 28 to the gas barrier film 21, it is preferable to bond the sealing member 28 using an arbitrary curable resin sealing layer.
- a suitable adhesive can be appropriately selected for the resin sealing layer from the viewpoint of improving the adhesion with the adjacent sealing member 28, gas barrier film 21, and the like.
- thermosetting resin for example, a resin mainly composed of a compound having an ethylenic double bond at the molecular end or side chain and a thermal polymerization initiator can be used. More specifically, a thermosetting resin made of an epoxy resin, an acrylic resin, or the like can be used. Moreover, according to the bonding apparatus and hardening processing apparatus which are used by the manufacturing process of an organic EL element, you may use fusion type thermosetting resin.
- photo-radically polymerizable resins mainly composed of various (meth) acrylates such as polyester (meth) acrylate, polyether (meth) acrylate, epoxy (meth) acrylate, polyurethane (meth) acrylate, epoxy, vinyl ether, etc.
- photo-radically polymerizable resins mainly composed of various (meth) acrylates such as polyester (meth) acrylate, polyether (meth) acrylate, epoxy (meth) acrylate, polyurethane (meth) acrylate, epoxy, vinyl ether, etc.
- examples thereof include a cationic photopolymerizable resin mainly composed of a resin and a thiol / ene addition type resin.
- an epoxy resin-based photo-cationic polymerizable resin having a low shrinkage of the cured product, a small outgas, and excellent long-term reliability is preferable.
- a resin sealing layer a chemical curing type (two-component mixed) resin can be used. Hot melt polyamide, polyester, and polyolefin can also be used. Moreover, a cationic curing type ultraviolet curing epoxy resin can be used.
- the organic material which comprises an organic EL element may deteriorate with heat processing. For this reason, it is preferable to use a resin material that can be adhesively cured from room temperature to 80 ° C.
- the inorganic sealing layer is formed on the gas barrier film 21 having the gas barrier layer 22 so as to cover a portion other than the first electrode 23, the light emitting unit 26, and the second electrode 25.
- the inorganic sealing layer is a member that seals the first electrode 23, the light emitting unit 26, and the second electrode 25 together with the resin sealing layer. For this reason, it is preferable to use the material which has a function which suppresses penetration
- the inorganic sealing layer is configured to be in direct contact with the first electrode 23, the light emitting unit 26, and the second electrode 25, the material has excellent bonding properties with the first electrode 23, the light emitting unit 26, and the second electrode 25. Is preferably used.
- the inorganic sealing layer is preferably formed of a compound such as an inorganic oxide, an inorganic nitride, or an inorganic carbide having high sealing properties. Specifically, it is formed of SiO x , Al 2 O 3 , In 2 O 3 , TiO x , ITO (tin / indium oxide), AlN, Si 3 N 4 , SiO x N, TiO x N, SiC, or the like. be able to.
- the inorganic sealing layer can be formed by a known method such as a sol-gel method, a vapor deposition method, CVD, ALD (Atomic Layer Deposition), PVD, or a sputtering method.
- the inorganic sealing layer is mainly composed of silicon oxide and silicon oxide by selecting conditions such as organometallic compound, decomposition gas, decomposition temperature, input power, etc., which are raw materials (also referred to as raw materials) in the atmospheric pressure plasma method.
- the composition of inorganic oxides, or mixtures of inorganic carbides, inorganic nitrides, inorganic sulfides, and inorganic halides, such as inorganic oxynitrides and inorganic oxide halides, can be made separately. .
- silicon oxide is generated.
- silazane or the like is used as a raw material compound, silicon oxynitride is generated. This is because highly active charged particles and active radicals exist in the plasma space at a high density, so that multistage chemical reactions are accelerated very rapidly in the plasma space, and the elements in the plasma space are thermodynamically This is because it is converted into a very stable compound in a very short time.
- the raw material for forming such an inorganic sealing layer is a silicon compound
- it may be in a gas, liquid, or solid state at normal temperature and pressure.
- gas it can be introduced into the discharge space as it is, but in the case of liquid or solid, it is used after being vaporized by means such as heating, bubbling, decompression or ultrasonic irradiation.
- the solvent may be diluted with a solvent, and an organic solvent such as methanol, ethanol, n-hexane or a mixed solvent thereof may be used as the solvent.
- these dilution solvents are decomposed
- silicon compounds include silane, tetramethoxysilane, tetraethoxysilane, tetra n-propoxysilane, tetraisopropoxysilane, tetra n-butoxysilane, tetrat-butoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, Diethyldimethoxysilane, diphenyldimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, phenyltriethoxysilane, (3,3,3-trifluoropropyl) trimethoxysilane, hexamethyldisiloxane, bis (dimethylamino) dimethylsilane Bis (dimethylamino) methylvinylsilane, bis (ethylamino) dimethylsilane, N, O-bis (trimethylsilyl) acetamide
- a decomposition gas for decomposing these silicon-containing source gases to obtain an inorganic sealing layer hydrogen gas, methane gas, acetylene gas, carbon monoxide gas, carbon dioxide gas, nitrogen gas, ammonia gas, suboxide
- examples thereof include nitrogen gas, nitrogen oxide gas, nitrogen dioxide gas, oxygen gas, water vapor, fluorine gas, hydrogen fluoride, trifluoroalcohol, trifluorotoluene, hydrogen sulfide, sulfur dioxide, carbon disulfide, and chlorine gas.
- An inorganic sealing layer containing silicon oxide, nitride, carbide or the like can be obtained by appropriately selecting the source gas containing silicon and the decomposition gas.
- a discharge gas that tends to be in a plasma state is mainly mixed with these reactive gases, and the gas is sent to a plasma discharge generator.
- a discharge gas nitrogen gas and / or 18th group atom of the periodic table, specifically, helium, neon, argon, krypton, xenon, radon, etc. are used. Among these, nitrogen, helium, and argon are preferably used.
- the film is formed by mixing the discharge gas and the reactive gas and supplying them as a thin film forming (mixed) gas to an atmospheric pressure plasma discharge generator (plasma generator).
- plasma generator atmospheric pressure plasma discharge generator
- the ratio of the discharge gas and the reactive gas varies depending on the properties of the film to be obtained, the reactive gas is supplied with the ratio of the discharge gas being 50% or more with respect to the entire mixed gas.
- the sealing member 28 covers the organic EL element, and a plate-like (film-like) sealing member 28 is fixed to the gas barrier film 21 side by a sealing layer 27.
- the plate-like (film-like) sealing member 28 include a glass substrate and a polymer substrate, and these substrate materials may be used in the form of a thin film.
- the glass substrate include soda-lime glass, barium / strontium-containing glass, lead glass, aluminosilicate glass, borosilicate glass, barium borosilicate glass, and quartz.
- the polymer substrate include polycarbonate, acrylic, polyethylene terephthalate, polyether sulfide, and polysulfone.
- sealing member 28 it is preferable to use a metal foil on which a resin film is laminated (polymer film).
- a metal foil laminated with a resin film cannot be used as a substrate on the light extraction side, but is a low-cost and low moisture-permeable sealing material. For this reason, it is suitable as the sealing member 28 not intended to extract light.
- the metal foil refers to a metal foil or film formed by rolling or the like, unlike a metal thin film formed by sputtering or vapor deposition, or a conductive film formed from a fluid electrode material such as a conductive paste. .
- metal foil there is no limitation in particular in the kind of metal, for example, copper (Cu) foil, aluminum (Al) foil, gold (Au) foil, brass foil, nickel (Ni) foil, titanium (Ti) foil, copper alloy Examples thereof include foil, stainless steel foil, tin (Sn) foil, and high nickel alloy foil.
- a particularly preferable metal foil is an Al foil.
- the thickness of the metal foil is preferably in the range of 6 to 50 ⁇ m. When the thickness is in the range of 6 to 50 ⁇ m, it is possible to prevent the generation of pinholes during use depending on the material used for the metal foil, and to obtain the required gas barrier properties (moisture permeability, oxygen permeability).
- the resin film it is possible to use various materials described in “New development of functional packaging materials: cutting-edge technology and future trends” (Toray Research Center, Inc.).
- polyethylene resin, polypropylene resin, polyethylene terephthalate resin, polyamide resin, ethylene-vinyl alcohol copolymer resin, ethylene-vinyl acetate copolymer resin, acrylonitrile-butadiene copolymer resin, cellophane resin, vinylon Resin, vinylidene chloride resin and the like can be used.
- a resin such as a polypropylene resin and a nylon resin may be stretched and further coated with a vinylidene chloride resin.
- the polyethylene resin may be either low density or high density.
- the sealing member 28 has an oxygen permeability measured by a method according to JIS-K-7126-1987 of 1 ⁇ 10 ⁇ 3 ml / (m 2 ⁇ 24 h ⁇ atm) or less, and conforms to JIS-K-7129-1992.
- the water vapor permeability (25 ⁇ 0.5 ° C., relative humidity (90 ⁇ 2)% RH) measured by a compliant method is preferably 1 ⁇ 10 ⁇ 3 g / (m 2 ⁇ 24 h) or less.
- the above-described substrate material may be processed into a concave plate shape and used as the sealing member 28.
- the above-described substrate member is subjected to processing such as sand blasting or chemical etching to form a concave shape.
- the present invention is not limited to this, and a metal material may be used.
- the metal material include one or more metals or alloys selected from the group consisting of stainless steel, iron, copper, aluminum, magnesium, nickel, zinc, chromium, titanium, molybdenum, silicon, germanium, and tantalum.
- the organic EL element can be applied to electronic devices such as a display device, a display, and various light emission sources.
- light-emitting light sources include lighting devices such as home lighting and interior lighting, backlights for clocks and liquid crystals, signboard advertisements, traffic lights, optical storage media and other light sources, light sources for electrophotographic copying machines, and light sources for optical communication processors. Examples include, but are not limited to, a light source of an optical sensor. In particular, it can be effectively used as a backlight of a liquid crystal display device and an illumination light source.
- patterning may be performed by a metal mask, an inkjet printing method, or the like at the time of film formation as necessary. In the case of patterning, only the electrode may be patterned, the electrode and the light emitting layer may be patterned, or the entire element layer may be patterned. In manufacturing the element, a conventionally known method can be used.
- Example 101 Under the following conditions, a first gas barrier layer, a second gas barrier layer, and a third gas barrier layer were formed on one surface of the resin base material, and a gas barrier film of Sample 101 was produced.
- a resin base material As a resin base material, a polyethylene terephthalate film (manufactured by Teijin DuPont Films, Teijin Tetron Film G2P2, hereinafter abbreviated as PET) with easy adhesion processing on both surfaces was used. Further, the surface of the resin substrate was subjected to corona treatment using a corona discharge device AGI-080 (manufactured by Kasuga Denki Co., Ltd.). During the corona treatment, the gap between the discharge electrode of the corona discharge device and the surface of the film was set to 1 mm, and the treatment output was 600 mW / cm 2 , and a corona discharge was performed for 10 seconds.
- AGI-080 manufactured by Kasuga Denki Co., Ltd.
- the first gas barrier layer is formed by connecting two apparatuses having a film forming section composed of opposing film forming rolls described in Japanese Patent No. 4268195, and has a roll-to-roller having a first film forming section and a second film forming section. It was produced by a plasma CVD method (PECVD) using a roll type CVD film forming apparatus (see FIG. 3). Using this apparatus, a first gas barrier layer having a thickness of 200 nm was formed on a resin base material under the following conditions.
- PECVD plasma CVD method
- the first gas barrier layer has an effective film formation width of 1000 mm and a conveyance speed of 7.0 m / min.
- the supply amount of each source gas (HMDSO) and the supply of oxygen gas in the first film formation unit and the second film formation unit were the following conditions.
- the film thickness was adjusted by the number of times of film formation (number of apparatus passes).
- the second pass conveys the resin base material in the direction of rewinding, but even when the pass direction is different, the first film forming unit passes through the first film forming unit and then passes through.
- the film forming unit was a second film forming unit.
- the thickness was determined by cross-sectional TEM observation. As other conditions, the power supply frequency was 84 kHz, and the film forming roll temperatures were all 30 ° C.
- the film forming conditions of the first film forming unit and the second film forming unit are shown below.
- ⁇ First film forming unit Conveying speed: 7.0 m / min ⁇
- a second gas barrier layer was formed on the first gas barrier layer.
- the second gas barrier layer was formed by applying a coating liquid containing polysilazane shown below to form a coating film, and then modifying the coating film by vacuum ultraviolet irradiation.
- a dibutyl ether solution containing 20% by mass of perhydropolysilazane (PHPS, manufactured by AZ Electronic Materials Co., Ltd., NN120-20) and an amine catalyst (N, N, N ′, N′-tetramethyl-1,6) -Dihydrohexane (TMDAH))-containing perhydropolysilazane 20% by mass dibutyl ether solution manufactured by AZ Electronic Materials Co., Ltd., NAX120-20
- PHPS perhydropolysilazane
- TMDAH amine catalyst
- the resin base material on which the first gas barrier layer was formed was prepared by cutting it into a sheet shape.
- the coating film was formed on the surface of the already formed first gas barrier layer.
- the coating solution was applied by spin coating so that the dry film thickness was 470 nm, and dried at 80 ° C. for 2 minutes.
- vacuum ultraviolet irradiation treatment was performed on the dried coating film using an Xe excimer lamp having a wavelength of 172 nm under the conditions of an oxygen concentration of 1.0 (volume%) and an irradiation energy of 3.0 (J / cm 2 ).
- a second gas barrier layer having the entire thickness of 470 nm was formed in the region (b).
- composition distribution in the thickness direction of the region (b) included in the second gas barrier layer was determined by measurement using the following XPS analysis method.
- -XPS analysis conditions-Equipment QUANTERASXM manufactured by ULVAC-PHI ⁇
- X-ray source Monochromatic Al-K ⁇ Measurement area: Si2p, C1s, N1s, O1s ⁇
- Sputtering ion Ar (2 keV)
- Depth profile repeats measurement after sputtering for a certain time. In one measurement, the sputtering time was adjusted so that the thickness was about 2.8 nm in terms of SiO 2 .
- Quantification The background was determined by the Shirley method, and quantified using the relative sensitivity coefficient method from the obtained peak area. For data processing, MultiPak manufactured by ULVAC-PHI was used.
- a third gas barrier layer was formed on the second gas barrier layer.
- the third gas barrier layer was formed under the following conditions using a magnetron sputtering apparatus. ⁇ Film formation conditions ⁇ Target: Oxygen deficient niobium pentoxide target ⁇ Sputter power supply power: DC 5 W / cm 2 Process gas: Ar, O 2 (O 2 partial pressure 15%) ⁇ Gas pressure: 0.3Pa ⁇ Film thickness: 100 nm
- Sample 102 A gas barrier film of Sample 102 was produced in the same manner as Sample 101, except that the thickness of the second gas barrier layer was 750 nm (the entire region was region (b)).
- Sample 103 A gas barrier film of Sample 103 was produced in the same manner as Sample 101 except that the thickness of the second gas barrier layer was changed to 60 nm (the entire region was region (b)).
- Sample 104 A gas barrier film of Sample 104 was produced in the same manner as Sample 101 except that the film formation conditions of the third gas barrier layer were changed to the following conditions.
- ⁇ Film formation conditions ⁇ Target: Tantalum target ⁇
- Sample 105 A gas barrier film of Sample 105 was produced in the same manner as Sample 101 except that the film formation conditions of the third gas barrier layer were changed to the following conditions.
- ⁇ Film formation conditions ⁇ Target: Oxygen deficient titanium oxide target ⁇
- Sputter power supply power DC 5 W / cm 2 Process gas: Ar, O 2 (O 2 partial pressure 3%) ⁇ Gas pressure: 0.3Pa ⁇ Film thickness: 100 nm
- Sample 106 A gas barrier film of Sample 106 was produced in the same manner as Sample 101 except that the film formation conditions for the third gas barrier layer were changed to the following conditions.
- ⁇ Film formation conditions ⁇ Target: Zirconium target ⁇ Sputter power supply power: DC 5 W / cm 2 Process gas: Ar, O 2 (O 2 partial pressure 20%) ⁇ Gas pressure: 0.3Pa ⁇ Film thickness: 100 nm
- Example 107 Except that the first gas barrier layer was formed by applying energy to the coating obtained by applying and drying the polysilazane-containing liquid under the same conditions as the second gas barrier layer of Sample 101, and the dry film thickness was 250 nm, A gas barrier film of Sample 107 was produced by the same method as Sample 101. That is, in the gas barrier film of sample 107, both the first gas barrier layer and the second gas barrier layer are layers formed by applying energy to a coating film obtained by applying and drying a polysilazane-containing liquid, and containing polysilazane. It is the structure by which the layer formed by applying energy to the coating film obtained by apply
- Sample 108 A gas barrier film of Sample 108 was produced by the same method as Sample 101, except that the first gas barrier layer was formed using a magnetron sputtering apparatus under the following film formation conditions.
- -Film formation conditions Polycrystalline SiO 2 ⁇ Sputter power supply power: DC 5 W / cm 2 Process gas: Ar, O 2 (O 2 partial pressure 20%) ⁇ Gas pressure: 0.3Pa ⁇ Film thickness: 250nm
- sample 109 A gas barrier film of Sample 109 was produced in the same manner as Sample 101 except that the third gas barrier layer was not produced. Therefore, the gas barrier film of the sample 109 is composed of a resin base material, a first gas barrier film, and a second gas barrier layer.
- Sample 110 A gas barrier film of Sample 110 was produced in the same manner as Sample 101 except that the thickness of the second gas barrier layer was 35 nm.
- Sample 111 A gas barrier film of Sample 111 was produced in the same manner as Sample 101 except that the thickness of the second gas barrier layer was 1100 nm (the entire region was region (b)).
- Sample 112 A gas barrier film of Sample 112 was produced in the same manner as Sample 111 except that the third gas barrier layer was formed under the following film formation conditions.
- -Film formation conditions Polycrystalline SiO 2 ⁇ Sputter power supply power: DC 5 W / cm 2 Process gas: Ar, O 2 (O 2 partial pressure 20%) ⁇ Gas pressure: 0.3Pa ⁇ Film thickness: 100 nm
- Table 2 shows the structures of the gas barrier films of the samples 101 to 112 and the evaluation results.
- the samples 101 to 108 in which the first to third gas barrier layers satisfy the definition of the above-described embodiment have excellent results of the continuous bending test.
- the results of a continuous bending test of a sample containing Nb or Ta oxide as the third gas barrier layer are excellent.
- the result of the continuous bending test is deteriorated.
- the sample 109 that does not have the third gas barrier layer and the sample 112 in which the third gas barrier layer does not contain a metal oxide having a lower oxidation-reduction potential than silicon as a main component have poor results of the continuous bending test.
- an adhesive made of a heat-resistant acrylic resin having a thickness of 20 ⁇ m is provided on the back side of the gas barrier film of sample 101 (the surface opposite to the surface on which the organic EL element is formed).
- a 75 ⁇ m-thick PET film was bonded as a support film through the layers, and pressure-bonded with a nip roll to prepare a gas barrier film with a support film.
- the support film including the adhesive layer was equipped in the manufacturing process of the organic EL element, and was peeled off after the organic EL element was produced.
- the heating boat containing the compound 118 was energized and heated, and the deposition rate was 0.1 nm / second to 0.2 nm / second.
- the underlayer of the first electrode was provided with a thickness of 10 nm.
- the base material formed up to the base layer was transferred to the second vacuum chamber while being vacuumed, and after the pressure in the second vacuum chamber was reduced to 4 ⁇ 10 ⁇ 4 Pa, the heating boat containing silver was energized and heated.
- a first electrode (anode) made of silver having a thickness of 8 nm was formed at a deposition rate of 0.1 nm / second to 0.2 nm / second.
- first electrode (Formation of first electrode; Samples 201, 204 to 209, 211)
- Ar 20 sccm Ar 20 sccm
- sputtering pressure 0.5 Pa
- room temperature Ar 20 sccm
- target side power 150 W formation rate 1.4 nm / s
- ITO film thickness The first electrode (anode) was formed by facing sputtering under the condition of 15 nm.
- the target-substrate distance was 90 mm.
- compound A-3 blue light-emitting dopant
- compound A-1 green light-emitting dopant
- compound A-2 red light-emitting dopant
- compound H-1 host compound
- the vapor deposition rate was varied depending on the location so that the concentration was 35% to 5% by mass linearly, and the concentrations of Compound A-1 and Compound A-2 were each 0.2% by mass without depending on the film thickness.
- compound H-1 was co-deposited to a thickness of 70 nm by changing the deposition rate from 64.6% to 94.6% by mass.
- a light emitting layer was formed.
- the compound ET-1 was deposited to a thickness of 30 nm to form an electron transport layer, and further potassium fluoride (KF) was formed to a thickness of 2 nm. Furthermore, aluminum 110nm was vapor-deposited and the 2nd electrode (cathode) was formed.
- KF potassium fluoride
- the compound 118, compound HT-1, compounds A-1 to A-3, compound H-1 and S compound ET-1 are the compounds shown below.
- the sample was placed in a decompression device, and pressed against the superposed resin substrate and the sealing member at 90 ° C. under a decompression condition of 0.1 MPa, and held for 5 minutes. Subsequently, the sample was returned to an atmospheric pressure environment and further heated at 120 ° C. for 30 minutes to cure the adhesive.
- the sealing step is performed under atmospheric pressure and in a nitrogen atmosphere with a water content of 1 ppm or less, in accordance with JIS B 9920: 2002.
- the measured cleanliness is class 100, the dew point temperature is ⁇ 80 ° C. or less, and the oxygen concentration is 0. It was performed at an atmospheric pressure of 8 ppm or less.
- the description regarding formation of the lead-out wiring etc. from the 1st electrode and the 2nd electrode is omitted.
- Each organic EL element sample was stored for 500 hours in an environment of 85 ° C. and 85% RH in a state where the organic EL element forming surface was wound around a plastic roller having a curvature of 6 mm ⁇ . Thereafter, a current of 1 mA / cm 2 was applied to each organic EL element removed from the roller to emit light. Next, a part of the light emitting portion of the organic EL element was enlarged and photographed with a 100 ⁇ optical microscope (MS-804 manufactured by Moritex Co., Ltd., lens MP-ZE25-200). Next, the photographed image was cut out in a 2 mm square, and the presence or absence of dark spots was observed for each image. From the observation results, the ratio of the dark spot generation area to the light emission area was determined, and the dark spot resistance was evaluated according to the following criteria.
- Table 3 shows the configurations of the organic EL elements of the samples 201 to 211 and the evaluation results.
- Samples 201 to 206 in which the first to third gas barrier layers satisfy the provisions of the above-described embodiment gave good results in both the continuous folding test and the folding storage stability test.
- Sample 202 and Sample 203, in which Nb oxide was used as the third gas barrier layer and the base layer and the thin Ag layer were provided as the anode showed particularly good results in both the continuous folding test and the folding storage stability test.
- the metal oxide having a low oxidation-reduction potential constituting the third gas barrier layer is oxidized before the region (b) of the second gas barrier layer, and the deterioration of the gas barrier property of the second gas barrier layer is suppressed. It is presumed that the durability of the gas barrier film in a high temperature and high humidity environment has been improved.
- the sample 207 not having the third gas barrier layer and the sample 211 in which the third gas barrier layer is an oxide of silicon and does not contain a metal oxide having a lower oxidation-reduction potential than silicon are a continuous bending test.
- bad results were obtained in both the bending storage stability tests. Since these sample 207 and sample 211 do not have the third gas barrier layer containing a metal oxide having a low oxidation-reduction potential as a main component, the spot gas barrier in the region (b) of the second gas barrier layer described above. It is presumed that the durability of the gas barrier film in a high-temperature and high-humidity environment is low because the deterioration of the property cannot be suppressed.
- Samples 208 to 210 in which the thickness of the region (b) of the second gas barrier layer is outside the range of 50 to 1000 nm are compared with the samples 201 and 202 having the same configuration except for the second gas barrier layer. Both folding and shelf life tests have deteriorated. This is presumably because the region (b) of the second gas barrier layer is insufficient in thickness, or the region (b) is not sufficiently modified by the thickness.
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Abstract
Description
また、本発明の有機エレクトロルミネッセンス素子は、上記ガスバリア性フィルムと、第1電極と第2電極とに挟持された有機機能層とを備える。
なお、説明は以下の順序で行う。
1.ガスバリア性フィルムの実施形態
2.有機エレクトロルミネッセンス素子の実施形態
以下、ガスバリア性フィルムの具体的な実施形態について説明する。
図1に本実施形態のガスバリア性フィルムの概略構成図を示す。図1に示すガスバリア性フィルムは、樹脂基材1と、この樹脂基材1上に形成されたガスバリア層22とから構成されている。このガスバリア層22は、樹脂基材1側から、第1ガスバリア層22a、第2ガスバリア層22b、及び、第3ガスバリア層22cがこの順に積層された積層構造を含んで構成されている。
ガスバリア性フィルムを構成する樹脂基材1は、可撓性を有する折り曲げ可能な可撓性樹脂フィルムで、その厚さが3~50μmの範囲内にある薄膜の樹脂である。樹脂基材1は、後述する各構成層を保持することができる樹脂材料であれば、特に限定されない。
サポートフィルムの厚さは、特に制限されないものの、機械的強度、取扱性等を考慮すると、50~300μmが好ましい。なお、サポートフィルムの厚さは、マイクロメータを使用して測定することが可能である。
ガスバリア性フィルムは、樹脂基材1上に、無機化合物を含む第1ガスバリア層22aを有する。第1ガスバリア層22aを備えることにより、樹脂基材1側から浸入する水蒸気を遮断することができ、高温高湿環境での耐久性が向上したガスバリア性フィルムとなる。第1ガスバリア層22aは、単層でもよく、2層以上の積層構造であってもよい。第1ガスバリア層22aが2層以上の積層構造である場合、各第1ガスバリア層22aは同じ組成であってもよいし異なる組成であってもよい。
第1ガスバリア層22aの形成方法の一つである、ポリシラザンを含有する塗布液を塗布及び乾燥して得られる塗膜にエネルギーを印加して形成する方法において、エネルギーの印加の条件以外の形成条件(用いられるポリシラザンの種類、塗布液に用いられる溶媒、塗布液濃度、触媒の種類等)は、後述する第2ガスバリア層22bの項で詳細に説明するため、ここでは説明を省略する。エネルギーを印加する方法としては、転化反応が可能なプラズマ処理や紫外線照射処理による転化反応が好ましく、真空紫外線を照射することがより好ましい。
第1ガスバリア層22aの好ましい形成方法である気相成膜法としては、物理気相成長法(PVD法)又は化学気相成長法(CVD法)が挙げられる。以下、気相成膜法について説明する。
第2ガスバリア層22bは、ポリシラザンを含有する塗布液を塗布及び乾燥して得られる塗膜にエネルギーを印加して形成される。第2ガスバリア層22bは、単層でもよいし2層以上の積層構造であってもよい。第2ガスバリア層22bが2層以上の積層構造である場合、各第2ガスバリア層22bは同じ組成であってもよいし異なる組成であってもよい。
領域(b)の厚さは、好ましくは100~300nmである。この範囲であれば、デバイスとして求められる耐用年数の間、良好なガスバリア性を維持できる効果や、コストを削減できる効果がさらに向上する。
また、上記一般式(I)において、nは、整数であり、一般式(I)で表される構造を有するポリシラザンが150~150,000g/モルの数平均分子量を有するように定められることが好ましい。
上記一般式(I)で表される構造を有する化合物において、好ましい態様の一つは、R1、R2及びR3のすべてが水素原子であるパーヒドロポリシラザンである。
第2ガスバリア層22b形成用塗布液を調製するための溶剤としては、ポリシラザンを溶解できるものであれば特に制限されないが、ポリシラザンと容易に反応してしまう水及び反応性基(例えば、ヒドロキシル基、あるいはアミン基等)を含まず、ポリシラザンに対して不活性の有機溶剤が好ましく、非プロトン性の有機溶剤がより好ましい。具体的には、溶剤としては、非プロトン性溶剤;例えば、ペンタン、ヘキサン、シクロヘキサン、トルエン、キシレン、ソルベッソ、ターベン等の、脂肪族炭化水素、脂環式炭化水素、芳香族炭化水素等の炭化水素溶媒;塩化メチレン、トリクロロエタン等のハロゲン炭化水素溶媒;酢酸エチル、酢酸ブチル等のエステル類;アセトン、メチルエチルケトン等のケトン類;ジブチルエーテル、ジオキサン、テトラヒドロフラン等の脂肪族エーテル、脂環式エーテル等のエーテル類:例えば、テトラヒドロフラン、ジブチルエーテル、モノ-及びポリアルキレングリコールジアルキルエーテル(ジグライム類)等を挙げることができる。上記溶剤は、ポリシラザンの溶解度や溶剤の蒸発速度等の目的にあわせて選択され、単独で使用されても又は2種以上の混合物の形態で使用されてもよい。
第2ガスバリア層22b形成用塗布液を塗布する方法としては、従来公知の適切な湿式塗布方法が採用され得る。具体例としては、スピンコート法、ロールコート法、フローコート法、インクジェット法、スプレーコート法、プリント法、ディップコート法、流延成膜法、バーコート法、ダイコート法、グラビア印刷法等が挙げられる。
続いて、上記のようにして形成された塗膜に対して、エネルギーを印加し、ポリシラザンの酸化ケイ素又は酸窒化ケイ素等への転化反応を行い、第2ガスバリア層22bがガスバリア性を発現する無機薄膜への改質を行う。
改質処理として用いることのできるプラズマ処理は、公知の方法を用いることができるが、好ましくは大気圧プラズマ処理等をあげることができる。大気圧近傍でのプラズマCVD処理を行う大気圧プラズマCVD法は、真空下のプラズマCVD法に比べ、減圧にする必要がなく生産性が高いだけでなく、プラズマ密度が高密度であるために成膜速度が速く、さらには通常のCVD法の条件に比較して、大気圧下という高圧力条件では、ガスの平均自由工程が非常に短いため、極めて均質の膜が得られる。
改質処理の方法の1つとして、紫外線照射による処理が好ましい。紫外線(紫外光と同義)によって生成されるオゾンや活性酸素原子は高い酸化能力を有しており、低温で高い緻密性と絶縁性を有する酸化ケイ素膜又は酸窒化ケイ素膜を形成することが可能である。
最も好ましい改質処理方法は、真空紫外線照射による処理(エキシマ照射処理)である。真空紫外線照射による処理は、ポリシラザン化合物内の原子間結合力より大きい100~200nmの光エネルギーを用い、好ましくは100~180nmの波長の光エネルギーを用い、原子の結合を光量子プロセスと呼ばれる光子のみの作用により、直接切断しながら活性酸素やオゾンによる酸化反応を進行させることで、比較的低温(約200℃以下)で、酸化ケイ素膜の形成を行う方法である。なお、エキシマ照射処理を行う際は、上述したように熱処理を併用することが好ましい。
また、波長の短い172nmの光のエネルギーは、有機物の結合を解離させる能力が高いことが知られている。この活性酸素やオゾンと紫外線放射が持つ高いエネルギーによって、短時間でポリシラザン塗膜の改質を実現できる。
領域(b)のエッチングレートは組成によって異なる。このため、基準としてSiO2換算のエッチングレートを元にして一旦求めておき、測定試料の断面TEM画像をもとに、積層して形成した領域で層の界面を特定して一層当たりの厚さを求める。これをXPS分析から求めた厚さ方向の組成分布と比較しながら、厚さ方向の組成分布における各層を特定し、それぞれに対応するXPS分析から求めた各領域の厚さと、断面TEM画像から求めた各領域の厚さが一致するように、XPS分析から求めた各領域の厚さに対して一律に係数をかける。このように、XPS分析では、厚さ方向の補正を行う。
・装置:アルバックファイ製QUANTERASXM
・X線源:単色化Al-Kα
・測定領域:Si2p、C1s、N1s、O1s
・スパッタイオン:Ar(2keV)
・デプスプロファイル:一定時間スパッタ後、測定を繰り返す。1回の測定は、SiO2換算で、約2.8nmの厚さ分となるようにスパッタ時間を調整する。
・定量:バックグラウンドをShirley法で求め、得られたピーク面積から相対感度係数法を用いて定量した。データ処理は、アルバックファイ社製のMultiPakを用いる。
また、各試料の断面をTEMで撮影し、積層構成の各膜厚を求める。上記で求めた膜厚方向の組成分布のプロファイルをTEM画像から求めた実膜厚データを用いて補正し、領域の膜厚方向の組成分布を得る。これを元に、領域(b)の厚さを求める。
・装置:SII製SMI2050
・加工イオン:(Ga 30kV)
・試料厚み:100nm~200nm
・装置:日本電子株式会社製JEM2000FX(加速電圧:200kV)
第3ガスバリア層22cは、ケイ素よりも酸化還元電位の低い金属の酸化物を主成分として含む。第3ガスバリア層22cは、単層でもよいし2層以上の積層構造であってもよい。該第3ガスバリア層22cが2層以上の積層構造である場合、第3ガスバリア層22cは同じ組成であってもよいし異なる組成であってもよい。
中でも、成膜レートがより高く、より高い生産性を有することから、ケイ素よりも酸化還元電位の低い金属の酸化物をターゲットとして用いるスパッタ法が好ましい。
ガスバリア性フィルムは、上述のバリア層以外にも他の層を備えていてもよい。例えば、アンカーコート層や平滑層等の種々の機能を有する層を設けることができる。
樹脂基材1のガスバリア層22を形成する側の表面には、ガスバリア層22との密着性の向上を目的として、アンカーコート層を形成してもよい。アンカーコート層の厚さは、特に制限されないが、0.5~10μm程度が好ましい。
ガスバリア性フィルムにおいては、樹脂基材1と第1ガスバリア層22aとの間に、平滑層を有してもよい。平滑層は突起等が存在する樹脂基材1の粗面を平坦化するために設けられる。平滑層の厚さとしては、フィルムの耐熱性を向上させ、フィルムの光学特性のバランス調整を容易にする観点から、1~10μmの範囲が好ましく、さらに好ましくは、2μm~7μmの範囲にすることが好ましい。
感光性材料としては、例えば、ラジカル反応性不飽和化合物を有するアクリレート化合物を含有する樹脂組成物、アクリレート化合物とチオール基を有するメルカプト化合物を含有する樹脂組成物、エポキシアクリレート、ウレタンアクリレート、ポリエステルアクリレート、ポリエーテルアクリレート、ポリエチレングリコールアクリレート、グリセロールメタクリレート等の多官能アクリレートモノマーを溶解させた樹脂組成物等が挙げられる。具体的には、JSR株式会社製のUV硬化型有機/無機ハイブリッドハードコート材 OPSTAR(登録商標)シリーズを用いることができる。また、上記のような樹脂組成物の任意の混合物を使用することも可能であり、光重合性不飽和結合を分子内に1個以上有する反応性のモノマーを含有している感光性樹脂であれば特に制限はない。
熱硬化性材料として具体的には、クラリアント社製のトゥットプロムシリーズ(有機ポリシラザン)、セラミックコート株式会社製のSP COAT耐熱クリアー塗料、株式会社アデカ製のナノハイブリッドシリコーン、DIC株式会社製のユニディック(登録商標)V-8000シリーズ、EPICLON(登録商標) EXA-4710(超高耐熱性エポキシ樹脂)、信越化学工業株式会社製の各種シリコン樹脂、日東紡株式会社製の無機・有機ナノコンポジット材料SSGコート、アクリルポリオールとイソシアネートプレポリマーとからなる熱硬化性ウレタン樹脂、フェノール樹脂、尿素メラミン樹脂、エポキシ樹脂、不飽和ポリエステル樹脂、シリコン樹脂等が挙げられる。この中でも特に耐熱性を有するエポキシ樹脂ベースの材料であることが好ましい。
次に、上述のガスバリア性フィルムを用いた有機エレクトロルミネッセンス素子(有機EL素子)の実施形態について説明する。本実施形態の有機EL素子は、上述のガスバリア性フィルム上に、電極(陽極、陰極)及び発光ユニットが設けられた構成である。有機EL素子のガスバリア性フィルムは、上述のガスバリア性フィルムの実施形態と同様である。このため、有機EL素子の説明では、ガスバリア性フィルムの詳細な説明は省略する。
図4に、本実施形態の有機EL素子の概略構成図(断面図)を示す。
図4に示すように、有機EL素子は、ガスバリア性フィルム21、第1電極23、有機機能層を有する発光ユニット26及び第2電極25が、この順に積層されている。また、第2電極25上に、封止層27及び封止部材28が設けられている。有機EL素子は、発光ユニット26からの光を、ガスバリア性フィルム21側から取り出す、いわゆるボトムエミッション型の構成である。
(1)陽極/発光層/陰極
(2)陽極/発光層/電子輸送層/陰極
(3)陽極/正孔輸送層/発光層/陰極
(4)陽極/正孔輸送層/発光層/電子輸送層/陰極
(5)陽極/正孔輸送層/発光層/電子輸送層/電子注入層/陰極
(6)陽極/正孔注入層/正孔輸送層/発光層/電子輸送層/陰極
(7)陽極/正孔注入層/正孔輸送層/(電子阻止層/)発光層/(正孔阻止層/)電子輸送層/電子注入層/陰極
上記の中で(7)の構成が好ましく用いられるが、これに限定されない。
上記の代表的な素子構成において、陽極と陰極を除く層が有機機能層である。これらの少なくとも発光層を含む有機機能層を主体とするユニット(単位)が発光ユニットであり、この発光ユニットが陽極と陰極の間に挟持され、全体として有機EL素子を構成する。
また、必要に応じて、発光層と陰極との間に正孔阻止層(正孔障壁層)や電子注入層(陰極バッファー層)等を設けてもよく、また、発光層と陽極との間に電子阻止層(電子障壁層)や正孔注入層(陽極バッファー層)等を設けてもよい。
電子輸送層は、電子を輸送する機能を有する層である。電子輸送層には、広い意味で電子注入層、及び、正孔阻止層も含まれる。また、電子輸送層は、複数層で構成されていてもよい。
正孔輸送層は、正孔を輸送する機能を有する層である。正孔輸送層には、広い意味で正孔注入層、及び、電子阻止層も含まれる。また、正孔輸送層は、複数層で構成されていてもよい。
有機EL素子は、少なくとも1層の発光層を含む発光ユニット26を複数積層した、いわゆるタンデム構造の素子であってもよい。タンデム構造の代表的な素子構成としては、例えば、以下の構成を挙げることができる。
陽極/第1発光ユニット/中間コネクタ層/第2発光ユニット/中間コネクタ層/第3発光ユニット/陰極
複数の発光ユニット26は直接積層されていても、中間コネクタ層を介して積層されていてもよい。
タンデム型有機EL素子の具体例としては、例えば、米国特許第6337492号明細書、米国特許第7420203号明細書、米国特許第7473923号明細書、米国特許第6872472号明細書、米国特許第6107734号明細書、米国特許第6337492号明細書、国際公開第2005/009087号パンフレット、特開2006-228712号公報、特開2006-24791号公報、特開2006-49393号公報、特開2006-49394号公報、特開2006-49396号公報、特開2011-96679号公報、特開2005-340187号公報、特許第4711424号公報、特許第3496681号公報、特許第3884564号公報、特許第4213169号公報、特開2010-192719号公報、特開2009-076929号公報、特開2008-078414号公報、特開2007-059848号公報、特開2003-272860号公報、特開2003-045676号公報、国際公開第2005/094130号パンフレット等に記載の素子構成や構成材料等が挙げられるが、これらに限定されない。
有機EL素子に用いる発光層は、電極又は隣接層から注入される電子と正孔とが再結合し、励起子を経由して発光する場を提供する層である。発光層において、発光する部分は発光層の層内であっても、発光層と隣接層との界面であってもよい。
発光層の厚さの総和は、例えば、2nm~5μmの範囲内に調整することが好ましく、より好ましくは2~500nmの範囲内に調整され、さらに好ましくは5~200nmの範囲内に調整される。
また、発光層の個々の膜厚としては、2nm~1μmの範囲内に調整することが好ましく、より好ましくは2~200nmの範囲内に調整され、さらに好ましくは3~150nmの範囲内に調整される。
発光層に用いられる発光ドーパントとしては、蛍光発光性ドーパント(蛍光ドーパント、蛍光性化合物ともいう)、及び、リン光発光性ドーパント(リン光ドーパント、リン光性化合物ともいう)が好ましく用いられる。これらのうち、少なくとも1層の発光層がリン光発光ドーパントを含有することが好ましい。
有機EL素子における白色としては、2度視野角正面輝度を前述の方法により測定した際に、1000cd/m2でのCIE1931表色系における色度がx=0.39±0.09、y=0.38±0.08の領域内にあることが好ましい。
リン光発光性ドーパントは、励起三重項からの発光が観測される化合物であり、具体的には、室温(25℃)にてリン光発光する化合物であり、25℃においてリン光量子収率が0.01以上の化合物である。発光層に用いるリン光発光性ドーパントにおいて、好ましいリン光量子収率は、0.1以上である。
一つは、キャリアが輸送されるホスト化合物上で、キャリアの再結合によるホスト化合物の励起状態が生成される。このエネルギーをリン光発光性ドーパントに移動させることで、リン光発光性ドーパントからの発光を得るというエネルギー移動型である。もう一つは、リン光発光性ドーパントがキャリアトラップとなり、リン光発光性ドーパント上でキャリアの再結合が起こり、リン光発光性ドーパントからの発光が得られるというキャリアトラップ型である。いずれの場合においても、リン光発光性ドーパントの励起状態のエネルギーは、ホスト化合物の励起状態のエネルギーよりも低いことが条件となる。
公知のリン光発光性ドーパントの具体例としては、以下の文献に記載されている化合物等が挙げられる。
有機EL素子に用いる電子輸送層とは、電子を輸送する機能を有する材料からなり、陰極より注入された電子を発光層に伝達する機能を有する。
電子輸送材料は、単独で用いてもよく、また複数種を併用して用いてもよい。
電子輸送層の総厚については、特に制限はないが、通常は2nm~5μmの範囲内であり、より好ましくは2~500nmの範囲内であり、さらに好ましくは5~200nmの範囲内である。
一方で、電子輸送層の膜厚を厚くすると電圧が上昇しやすくなるため、特に膜厚が厚い場合においては、電子輸送層の電子移動度は10-5cm2/Vs以上であることが好ましい。
芳香族炭化水素環誘導体としては、ナフタレン誘導体、アントラセン誘導体、トリフェニレン等が挙げられる。
また、発光層の材料として例示したジスチリルピラジン誘導体も、電子輸送材料として用いることができるし、正孔注入層、正孔輸送層と同様にn型-Si、n型-SiC等の無機半導体も電子輸送材料として用いることができる。
また、これらの材料を高分子鎖に導入した、又は、これらの材料を高分子の主鎖とした高分子材料を用いることもできる。
ドープ材としては、金属錯体及びハロゲン化金属等の金属化合物や、その他のn型ドーパントが挙げられる。
このような構成の電子輸送層の具体例としては、例えば、特開平4-297076号公報、同10-270172号公報、特開2000-196140号公報、同2001-102175号公報、J.Appl.Phys.,95,5773(2004)等の文献に記載されたものが挙げられる。
米国特許第6528187号、米国特許第7230107号、米国特許出願公開第2005/0025993号明細書、米国特許出願公開第2004/0036077号明細書、米国特許出願公開第2009/0115316号明細書、米国特許出願公開第2009/0101870号明細書、米国特許出願公開第2009/0179554号明細書、国際公開第2003/060956号、国際公開第2008/132085号、Appl. Phys. Lett. 75, 4 (1999)、Appl. Phys. Lett. 79, 449 (2001)、Appl. Phys. Lett. 81, 162 (2002)、Appl. Phys. Lett. 81, 162 (2002)、Appl. Phys. Lett. 79, 156 (2001)、米国特許第7964293号、、国際公開第2004/080975号、国際公開第2004/063159号、国際公開第2005/085387号、国際公開第2006/067931号、国際公開第2007/086552号、国際公開第2008/114690号、国際公開第2009/069442号、国際公開第2009/066779号、国際公開第2009/054253号、国際公開第2011/086935号、国際公開第2010/150593号、国際公開第2010/047707号、EP2311826号、特開2010-251675号公報、特開2009-209133号公報、特開2009-124114号公報、特開2008-277810号公報、特開2006-156445号公報、特開2005-340122号公報、特開2003-45662号公報、特開2003-31367号公報、特開2003-282270号公報、国際公開第2012/115034号等
正孔阻止層は、広い意味では電子輸送層の機能を有する層である。好ましくは、電子を輸送する機能を有しつつ、正孔を輸送する能力が小さい材料からなる。電子を輸送しつつ正孔を阻止することで、電子と正孔の再結合確率を向上させることができる。
また、上述の電子輸送層の構成を、必要に応じて正孔阻止層として用いることができる。
有機EL素子に設ける正孔阻止層は、発光層の陰極側に隣接して設けられることが好ましい。
正孔阻止層に用いられる材料としては、上述の電子輸送層に用いられる材料が好ましく用いられ、また、上述のホスト化合物として用いられる材料も正孔阻止層に好ましく用いられる。
電子注入層(「陰極バッファー層」ともいう)は、駆動電圧低下や発光輝度向上のために陰極と発光層との間に設けられる層である。電子注入層の一例は、「有機EL素子とその工業化最前線(1998年11月30日エヌ・ティー・エス社発行)」の第2編第2章「電極材料」(123~166頁)に記載されている。
電子注入層は、ごく薄い膜であることが好ましく、素材にもよるがその膜厚は0.1~5nmの範囲内が好ましい。また、構成材料が、断続的に存在する不均一な膜であってもよい。
また、上記の電子注入層に用いられる材料は単独で用いてもよく、複数種を併用して用いてもよい。
正孔輸送層は、正孔を輸送する機能を有する材料からなる。正孔輸送層は、陽極より注入された正孔を発光層に伝達する機能を有する層である。
正孔輸送材料は、従来公知の化合物の中から任意のものを選択して用いることができる。正孔輸送材料は単独で用いてもよく、また複数種を併用して用いてもよい。
さらに、不純物をドープしたp性の高い正孔輸送層を用いることもできる。例えば、特開平4-297076号公報、特開2000-196140号公報、同2001-102175号公報の各公報、J.Appl.Phys.,95,5773(2004)等に記載された構成を正孔輸送層に適用することもできる。
また、特開平11-251067号公報、J.Huang et.al.著文献(Applied Physics Letters 80(2002),p.139)に記載されているような、いわゆるp型正孔輸送材料やp型-Si、p型-SiC等の無機化合物を用いることもできる。さらに、Ir(ppy)3に代表されるような中心金属にIrやPtを有するオルトメタル化有機金属錯体も好ましく用いられる。
Appl. Phys. Lett. 69, 2160 (1996)、J. Lumin. 72-74, 985 (1997)、Appl. Phys. Lett. 78, 673 (2001)、Appl. Phys. Lett. 90, 183503 (2007)、Appl. Phys. Lett. 90, 183503 (2007)、Appl. Phys. Lett. 51, 913 (1987)、Synth. Met. 87, 171 (1997)、Synth. Met. 91, 209 (1997)、Synth. Met. 111,421 (2000)、SID Symposium Digest, 37, 923 (2006)、J. Mater. Chem. 3, 319 (1993)、Adv. Mater. 6, 677 (1994)、Chem. Mater.15,3148 (2003)、米国特許出願公開第2003/0162053号明細書、米国特許出願公開第2002/0158242号明細書、米国特許出願公開第2006/0240279号明細書、米国特許出願公開第2008/0220265号明細書、米国特許第5061569号、国際公開第2007/002683号、国際公開第2009/018009号、EP650955、米国特許出願公開第2008/0124572号明細書、米国特許出願公開第2007/0278938号明細書、米国特許出願公開第2008/0106190号明細書、米国特許出願公開第2008/0018221号明細書、国際公開第2012/115034号、特表2003-519432号公報、特開2006-135145号公報、米国特許出願番号13/585981号
電子阻止層は、広い意味では正孔輸送層の機能を有する層である。好ましくは、正孔を輸送する機能を有しつつ電子を輸送する能力が小さい材料からなる。電子阻止層は、正孔を輸送しつつ電子を阻止することで、電子と正孔の再結合確率を向上させることができる。
電子阻止層に用いられる材料としては、上述の正孔輸送層に用いられる材料が好ましく用いることができる。また、上述のホスト化合物として用いられる材料も、電子阻止層として好ましく用いることができる。
正孔注入層(「陽極バッファー層」ともいう)は、駆動電圧低下や発光輝度向上のために陽極と発光層との間に設けられる層である。正孔注入層の一例は、「有機EL素子とその工業化最前線(1998年11月30日エヌ・ティー・エス社発行)」の第2編第2章「電極材料」(123~166頁)に記載されている。
正孔注入層は、必要に応じて設けられ、上述のように陽極と発光層との間、又は、陽極と正孔輸送層との間に設けられる。
正孔注入層に用いられる材料は、例えば上述の正孔輸送層に用いられる材料等が挙げられる。中でも、銅フタロシアニンに代表されるフタロシアニン誘導体、特表2003-519432や特開2006-135145等に記載されているようなヘキサアザトリフェニレン誘導体、酸化バナジウムに代表される金属酸化物、アモルファスカーボン、ポリアニリン(エメラルディン)やポリチオフェン等の導電性高分子、トリス(2-フェニルピリジン)イリジウム錯体等に代表されるオルトメタル化錯体、トリアリールアミン誘導体等が好ましい。
上述の正孔注入層に用いられる材料は、単独で用いてもよく、また複数種を併用して用いてもよい。
有機EL素子を構成する有機機能層は、さらに他の添加剤を含んでもよい。
その他添加剤としては、例えば臭素、ヨウ素及び塩素等のハロゲン元素やハロゲン化化合物、Pd、Ca、Na等のアルカリ金属やアルカリ土類金属、遷移金属の化合物や錯体、塩等が挙げられる。
ただし、電子や正孔の輸送性を向上させる目的や、励起子のエネルギー移動を有利にするための目的などによってはこの範囲内ではない。
有機EL素子の有機機能層(正孔注入層、正孔輸送層、発光層、正孔阻止層、電子輸送層、電子注入層等)の形成方法について説明する。
有機機能層の形成方法は、特に制限はなく、従来公知の例えば、真空蒸着法、湿式法(ウェットプロセス)等により形成することができる。
また、超音波、高剪断力分散やメディア分散等の分散方法により分散することができる。
また、層毎に異なる形成方法を適用してもよい。
第1電極23は、仕事関数の大きい(4eV以上、好ましくは4.3V以上)金属、合金、電気伝導性化合物、及び、これらの混合物からなる電極物質が用いられる。
このような電極物質の具体例としては、AuやAg等の金属及びこれらの合金、CuI、インジウムチンオキシド(ITO)、SnO2、ZnO等の導電性透明材料が挙げられる。
また、IDIXO(In2O3-ZnO)等の非晶質で透明導電膜を作製可能な材料を用いてもよい。
有機導電性化合物のように塗布可能な物質を用いる場合には、印刷方式、コーティング方式等の湿式成膜法を用いることもできる。
また、第1電極23としてのシート抵抗は、数百Ω/sq.以下が好ましい。
また、第1電極23の厚さは、材料にもよるが、通常10nm~1μm、好ましくは10~200nmの範囲で選ばれる。
このような第1電極23の形成方法としては、塗布法、インクジェット法、コーティング法、ディップ法等のウェットプロセスを用いる方法や、蒸着法(抵抗加熱、EB法等)、スパッタ法、CVD法等のドライプロセスを用いる方法等が挙げられる。中でも、蒸着法が好ましく適用される。
第2電極25としては、仕事関数の小さい(4eV以下)金属(電子注入性金属と称する)、合金、電気伝導性化合物、及び、これらの混合物からなる電極物質が用いられる。
このような電極物質の具体例としては、ナトリウム、ナトリウム-カリウム合金、マグネシウム、リチウム、マグネシウム/銅混合物、マグネシウム/銀混合物、マグネシウム/アルミニウム混合物、マグネシウム/インジウム混合物、アルミニウム/酸化アルミニウム(Al2O3)混合物、インジウム、リチウム/アルミニウム混合物、アルミニウム、希土類金属等が挙げられる。
有機EL素子は、ガスバリア層22が形成されたガスバリア性フィルム21の一方面上に、第1電極23、発光ユニット26及び第2電極25を覆う封止層27を介して、封止部材28が貼り合わされることにより、固体封止されている。
有機EL素子の固体封止は、封止部材28又はガスバリア性フィルム21の貼合面上に、未硬化の樹脂材料を複数箇所に分散させて塗布し、これらの樹脂材料を介して封止部材28とガスバリア性フィルム21とを互いに押圧した後、樹脂材料を硬化することで一体化して形成される。
また、樹脂材料(樹脂封止層)に加えて、無機材料(無機封止層)を用いてもよい。例えば、第1電極23、発光ユニット26及び第2電極25を無機封止層で覆った後、樹脂封止層により封止部材28とガスバリア性フィルム21とを接合する構成としてもよい。
樹脂封止層は、封止部材28をガスバリア性フィルム21側に固定するために用いられる。また、封止部材28とガスバリア性フィルム21との間に挟持された第1電極23、発光ユニット26及び第2電極25を封止するためのシール剤として用いられる。
樹脂封止層には、隣接する封止部材28やガスバリア性フィルム21等との密着性の向上の観点から、好適な接着材を適宜選択することができる。
熱硬化性樹脂としては、例えば、分子の末端又は側鎖にエチレン性二重結合を有する化合物と熱重合開始剤とを主成分とする樹脂等を用いることができる。
より具体的には、エポキシ系樹脂、アクリル系樹脂等からなる熱硬化性樹脂を使用することができる。また、有機EL素子の製造工程で用いる貼合装置及び硬化処理装置に応じて、溶融タイプの熱硬化性樹脂を使用してもよい。
例えば、ポリエステル(メタ)アクリレート、ポリエーテル(メタ)アクリレート、エポキシ(メタ)アクリレート、ポリウレタン(メタ)アクリレート等の各種(メタ)アクリレートを主成分とした光ラジカル重合性樹脂や、エポキシやビニルエーテル等の樹脂を主成分とした光カチオン重合性樹脂や、チオール・エン付加型樹脂等が挙げられる。これら光硬化性樹脂の中でも、硬化物の収縮率が低く、アウトガスも少なく、また長期信頼性に優れるエポキシ樹脂系の光カチオン重合性樹脂が好ましい。
なお、有機EL素子を構成する有機材料は、熱処理により劣化する場合がある。このため、室温から80℃までに接着硬化できる樹脂材料を使用することが好ましい。
無機封止層は、ガスバリア層22を有するガスバリア性フィルム21上において、第1電極23、発光ユニット26及び第2電極25が配置された以外の部分を覆うように形成されている。
また、無機封止層は、第1電極23、発光ユニット26及び第2電極25に直接接する構成であるため、第1電極23、発光ユニット26及び第2電極25との接合性に優れた材料を用いることが好ましい。
具体的には、SiOx、Al2O3、In2O3、TiOx、ITO(スズ・インジウム酸化物)、AlN、Si3N4、SiOxN、TiOxN、SiC等により形成することができる。
無機封止層は、ゾルゲル法、蒸着法、CVD、ALD(Atomic Layer Deposition)、PVD、スパッタリング法等の公知な手法により形成可能である。
また、溶媒によって希釈して使用してもよく、溶媒は、メタノール、エタノール、n-ヘキサン等の有機溶媒及びこれらの混合溶媒を使用できる。なお、これらの希釈溶媒は、プラズマ放電処理中において、分子状、原子状に分解されるため、影響をほとんど無視することができる。
このような放電ガスとしては、窒素ガス及び/又は周期表の第18属原子、具体的には、ヘリウム、ネオン、アルゴン、クリプトン、キセノン、ラドン等が用いられる。これらの中でも特に、窒素、ヘリウム、アルゴンが好ましく用いられる。
封止部材28は、有機EL素子を覆うものであって、板状(フィルム状)の封止部材28が封止層27によってガスバリア性フィルム21側に固定されている。
板状(フィルム状)の封止部材28としては、具体的には、ガラス基板、ポリマー基板が挙げられ、これらの基板材料をさらに薄型のフィルム状にして用いてもよい。
ガラス基板としては、特にソーダ石灰ガラス、バリウム・ストロンチウム含有ガラス、鉛ガラス、アルミノケイ酸ガラス、ホウケイ酸ガラス、バリウムホウケイ酸ガラス、石英等を挙げることができる。
また、ポリマー基板としては、ポリカーボネート、アクリル、ポリエチレンテレフタレート、ポリエーテルサルファイド、ポリサルフォン等を挙げることができる。
例えば、ポリエチレン系樹脂、ポリプロピレン系樹脂、ポリエチレンテレフタレート系樹脂、ポリアミド系樹脂、エチレン-ビニルアルコール共重合体系樹脂、エチレン-酢酸ビニル共重合体系樹脂、アクリロニトリル-ブタジエン共重合体系樹脂、セロハン系樹脂、ビニロン系樹脂、塩化ビニリデン系樹脂等を用いることができる。
ポリプロピレン系樹脂、及び、ナイロン系樹脂等の樹脂は、延伸されていてもよく、さらに塩化ビニリデン系樹脂がコートされていてもよい。また、ポリエチレン系樹脂は、低密度と高密度とのいずれを用いてもよい。
有機EL素子は、表示デバイス、ディスプレイ、各種発光光源等の電子機器に適用することができる。
発光光源としては、例えば、家庭用照明や車内照明等の照明装置、時計や液晶用バックライト、看板広告、信号機、光記憶媒体等の光源、電子写真複写機の光源、光通信処理機の光源、光センサーの光源等が挙げられるがこれに限定するものではない。特に、液晶表示装置のバックライト、照明用光源としての用途に有効に用いることができる。
以下、実施例を挙げて具体的に説明する。
試料101~112の各ガスバリア性フィルムを作製した。下記表2には試料101~112のガスバリア性フィルムにおける各層の構成を示す。
下記条件により、樹脂基材の一方の面上に、第1ガスバリア層、第2ガスバリア層、及び、第3ガスバリア層を形成し、試料101のガスバリア性フィルムを作製した。
樹脂基材として、両面に易接着加工された厚さ25μmのポリエチレンテレフタレートフィルム(帝人デュポンフィルム株式会社製、帝人テトロンフィルムG2P2、以下、PETと略記する)を用いた。また、樹脂基材の表面に、コロナ放電装置AGI-080(春日電機社製)を用いてコロナ処理を施した。コロナ処理時、コロナ放電装置の放電電極とフィルムの表面との間隙を1mmに設定し、処理出力を600mW/cm2の条件として、10秒間のコロナ放電を行った。
第1ガスバリア層は、特許第4268195号公報に記載の対向する成膜ロールからなる成膜部を有する装置を2台連接し、第1成膜部及び第2成膜部を有するロール・トゥ・ロール型CVD成膜装置(図3参照)を用いてプラズマCVD法(PECVD)により作製した。この装置を用いて、下記条件により樹脂基材上に、厚さ200nmの第1ガスバリア層を形成した。
成膜厚さは、成膜回数(装置のパス数)で調整した。1パス目に対して、2パス目は樹脂基材を巻き戻す方向に搬送しているが、パス方向が異なる場合でも、最初に通過する成膜部を第1成膜部、次に通過する成膜部を第2成膜部とした。厚さは断面TEM観察で求めた。
その他の条件として、電源周波数は84kHz、成膜ロールの温度はすべて30℃とした。
・第1成膜部
・搬送速度:7.0m/min
・原料ガス(HMDSO)供給量:150sccm
・酸素ガス供給量:500sccm
・真空度:1.5Pa
・印加電力:4.5kW
・第2成膜部
・搬送速度:7.0m/min
・原料ガス供給量:150sccm
・酸素ガス供給量:500sccm
・真空度:1.5Pa
・印加電力:4.5kW
次に、第1ガスバリア層上に、第2ガスバリア層を形成した。第2ガスバリア層は、下記に示すポリシラザンを含む塗布液を塗布して塗膜を形成した後、この塗膜に真空紫外線照射による改質を行って形成した。
・XPS分析条件
・装置:アルバックファイ製QUANTERASXM
・X線源:単色化Al-Kα
・測定領域:Si2p、C1s、N1s、O1s
・スパッタイオン:Ar(2keV)
・デプスプロファイル:一定時間スパッタ後、測定を繰り返す。1回の測定は、SiO2換算で約2.8nmの厚さ分となるようにスパッタ時間を調整した。
・定量:バックグラウンドをShirley法で求め、得られたピーク面積から相対感度係数法を用いて定量した。データ処理は、アルバックファイ社製のMultiPakを用いた。
第2ガスバリア層の膜厚は断面TEM観察で求めた。
次に、第2ガスバリア層上に、第3ガスバリア層を形成した。
第3ガスバリア層は、マグネトロンスパッタ装置を用い、下記条件で形成した。
・成膜条件
・ターゲット:酸素欠損型五酸化ニオブターゲット
・スパッタ電源パワー:DC 5W/cm2
・プロセスガス:Ar、O2(O2分圧15%)
・ガス圧:0.3Pa
・成膜厚さ:100nm
第2ガスバリア層の厚さを750nm(全域が領域(b))とした以外は、試料101と同様の方法により、試料102のガスバリア性フィルムを作製した。
第2ガスバリア層の厚さを60nm(全域が領域(b))とした以外は、試料101と同様の方法により、試料103のガスバリア性フィルムを作製した。
第3ガスバリア層の成膜条件を下記条件に変更した以外は、試料101と同様の方法により、試料104のガスバリア性フィルムを作製した。
・成膜条件
・ターゲット:タンタルターゲット
・スパッタ電源パワー:DC 5W/cm2
・プロセスガス:Ar、O2(O2分圧20%)
・ガス圧:0.3Pa
・成膜厚さ:50nm
第3ガスバリア層の成膜条件を下記条件に変更した以外は、試料101と同様の方法により、試料105のガスバリア性フィルムを作製した。
・成膜条件
・ターゲット:酸素欠損型酸化チタンターゲット
・スパッタ電源パワー:DC 5W/cm2
・プロセスガス:Ar、O2(O2分圧3%)
・ガス圧:0.3Pa
・成膜厚さ:100nm
第3ガスバリア層の成膜条件を下記条件に変更した以外は、試料101と同様の方法により、試料106のガスバリア性フィルムを作製した。
・成膜条件
・ターゲット:ジルコニウムターゲット
・スパッタ電源パワー:DC 5W/cm2
・プロセスガス:Ar、O2(O2分圧20%)
・ガス圧:0.3Pa
・成膜厚さ:100nm
第1ガスバリア層を、試料101の第2ガスバリア層と同様の条件でポリシラザン含有液を塗布及び乾燥して得られる塗膜にエネルギーを印加して形成し、乾燥膜厚を250nmとした以外は、試料101と同様の方法により、試料107のガスバリア性フィルムを作製した。
つまり、試料107のガスバリア性フィルムでは、第1ガスバリア層と第2ガスバリア層とが、共にポリシラザン含有液を塗布及び乾燥して得られる塗膜にエネルギーを印加して形成した層であり、ポリシラザン含有液を塗布及び乾燥して得られる塗膜にエネルギーを印加して形成した層が2層積層された構成である。
第1ガスバリア層を、マグネトロンスパッタ装置を用いて下記成膜条件により形成した以外は、試料101と同様の方法により、試料108のガスバリア性フィルムを作製した。
・成膜条件
・ターゲット:多結晶SiO2
・スパッタ電源パワー:DC 5W/cm2
・プロセスガス:Ar、O2(O2分圧20%)
・ガス圧:0.3Pa
・成膜厚さ:250nm
第3ガスバリア層を作製しなかった以外は、試料101と同様の方法により、試料109のガスバリア性フィルムを作製した。従って、試料109のガスバリア性フィルムは、樹脂基材、第1ガスバリア性フィルム、及び、第2ガスバリア層により構成されている。
第2ガスバリア層の厚さを35nmとした以外は、試料101と同様の方法により、試料110のガスバリア性フィルムを作製した。
第2ガスバリア層の厚さを1100nm(全域が領域(b))とした以外は、試料101と同様の方法により、試料111のガスバリア性フィルムを作製した。
第3ガスバリア層を、下記成膜条件により形成した以外は、試料111と同様の方法により、試料112のガスバリア性フィルムを作製した。
・成膜条件
・ターゲット:多結晶SiO2
・スパッタ電源パワー:DC 5W/cm2
・プロセスガス:Ar、O2(O2分圧20%)
・ガス圧:0.3Pa
・成膜厚さ:100nm
作製したガスバリア性フィルムの試料について、下記の評価を行った。
(連続折り曲げ試験)
連続折り曲げ試験は、室温下、ガスバリア性フィルムを屈曲直径6mmφの曲率で連続して1000往復折り曲げ、折り曲げた部分と、折り曲げていない部分との劣化度合いの差を5段階[(良)5>1(悪)]で評価した。
第2ガスバリア層の領域(b)の厚さが50~1000nmの範囲に入らない試料110及び試料111では、連続折り曲げ試験の結果が悪化している。特に、第3ガスバリア層を有していない試料109や、第3ガスバリア層がケイ素よりも酸化還元電位の低い金属の酸化物を主成分として含まない試料112では、連続折り曲げ試験の結果が悪い。
(ガスバリア性フィルムの準備)
試料201~211の有機EL素子の作製用に、上述の実施例1の試料101、試料104~106、及び、試料109~112のガスバリア性フィルムを準備した。
各試料のガスバリア性フィルムを、市販の真空蒸着装置の基材ホルダーに固定し、化合物118をタングステン製の抵抗加熱ボートに入れ、これら基材ホルダーと加熱ボートとを真空蒸着装置の第1真空槽内に取り付けた。また、タングステン製の抵抗加熱ボートに銀(Ag)を入れ、真空蒸着装置の第2真空槽内に取り付けた。
各試料のガスバリア性フィルム上に、FTSコーポレーション社の対向スパッタ機を用い、Ar 20sccm、スパッタ圧0.5Pa、室温下、ターゲット側電力150W、形成速度1.4nm/sで、ITO膜を層厚が15nmとなる条件で対向スパッタし第1電極(陽極)を形成した。ターゲット-基板間距離は90mmであった。
引き続き、市販の真空蒸着装置を用い、真空度1×10-4Paまで減圧した後、基材を移動させながら化合物HT-1を、蒸着速度0.1nm/秒で蒸着し、20nmの正孔輸送層(HTL)を設けた。
次に、封止部材として厚さ25μmのアルミ箔を使用し、このアルミ箔の片面に封止樹脂層として熱硬化型のシート状接着剤(エポキシ系樹脂)を厚さ20μmで貼合した封止部材を用いて、第2電極までを作製した試料に重ね合わせた。このとき、第1電極及び第2電極の引き出し電極の端部が外に出るように、封止部材の接着剤形成面と、素子の有機機能層面とを連続的に重ね合わせた。
作製した有機EL素子の試料について、下記の評価を行った。
(連続折り曲げ試験)
連続折り曲げ試験は、室温下、ガスバリア性フィルムを屈曲直径6mmφの曲率で連続して1000往復折り曲げ、折り曲げた部分と、折り曲げていない部分との劣化度合いの差を5段階[(良)5>1(悪)]で評価した。
各有機EL素子の試料を、曲率が6mmφのプラスチック製ローラーに、有機EL素子形成面が外側になるように巻き付けた状態で、85℃、85%RHの環境下で、500時間保存した。その後、ローラーからはずした各有機EL素子に、1mA/cm2の電流を印加して発光させた。次いで、100倍の光学顕微鏡(株式会社モリテックス製 MS-804、レンズMP-ZE25-200)で、有機EL素子の発光部の一部分を拡大して撮影した。次いで、撮影画像を2mm四方に切り抜き、それぞれの画像について、ダークスポット発生の有無を観察した。観察結果より、発光面積に対するダークスポットの発生面積比率を求め、下記の基準に従って、ダークスポット耐性を評価した。
4:ダークスポットの発生面積が、0.1%以上、1.0%未満である
3:ダークスポットの発生面積が、1.0%以上、3.0%未満である
2:ダークスポットの発生面積が、3.0%以上、6.0%未満である
1:ダークスポットの発生面積が、6.0%以上である
これらの試料207、試料211は、酸化還元電位の低い金属の酸化物を主成分として含む第3ガスバリア層を有していないため、上述の第2ガスバリア層の領域(b)のスポット的なガスバリア性の低下が抑制できないため、ガスバリア性フィルムの高温高湿環境での耐久性が低いと推測される。
Claims (5)
- 厚さ3~50μmの樹脂基材と、
無機化合物を含む第1ガスバリア層と、
ポリシラザンを含有する塗布液を塗布及び乾燥して得られる塗膜にエネルギーを印加して形成され、SiOwNx(ただし、0.2<w≦0.55、0.66<x≦0.75)で表される組成範囲を満たす領域を、50~1000nmの厚さで有する第2ガスバリア層と、
前記第2ガスバリア層に接して形成された、ケイ素よりも酸化還元電位の低い金属の酸化物を主成分として含む第3ガスバリア層と、を備える
ガスバリア性フィルム。 - 前記第3ガスバリア層は、ニオブ、タンタル、ジルコニウム、及びチタンからなる群より選択される少なくとも1種の金属の酸化物を主成分として含む、請求項1に記載のガスバリア性フィルム。
- 前記エネルギーの印加が、真空紫外線の照射である請求項1に記載のガスバリア性フィルム。
- ガスバリア性フィルムと、
第1電極と第2電極とに挟持された有機機能層と、を有し、
前記ガスバリア性フィルムが、
厚さ3~50μmの樹脂基材と、
無機化合物を含む第1ガスバリア層と、
ポリシラザンを含有する塗布液を塗布及び乾燥して得られる塗膜にエネルギーを印加して形成され、SiOwNx(ただし、0.2<w≦0.55、0.66<x≦0.75)で表される組成範囲を満たす領域を、50~1000nmの厚さで有する第2ガスバリア層と、
前記第2ガスバリア層に接して形成された、ケイ素よりも酸化還元電位の低い金属の酸化物を主成分として含む第3ガスバリア層と、を備える
有機エレクトロルミネッセンス素子。 - 前記第1電極が、厚さ20nm以下の銀を主成分として構成された層である請求項4に記載の有機エレクトロルミネッセンス素子。
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2016152822A1 (ja) * | 2015-03-23 | 2016-09-29 | コニカミノルタ株式会社 | 導電性フィルム及び有機エレクトロルミネッセンス素子 |
WO2018021021A1 (ja) * | 2016-07-28 | 2018-02-01 | コニカミノルタ株式会社 | ガスバリア性膜、これを用いたガスバリア性フィルム、およびこれらを用いた電子デバイス、ならびにガスバリア性膜の製造方法 |
WO2018034179A1 (ja) * | 2016-08-18 | 2018-02-22 | コニカミノルタ株式会社 | ガスバリアー性膜、その製造方法及びそれを具備した電子デバイス |
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010167777A (ja) * | 2008-12-19 | 2010-08-05 | Samsung Electronics Co Ltd | ガス遮断性薄膜、これを備えた電子素子及びその製造方法 |
WO2013002026A1 (ja) * | 2011-06-27 | 2013-01-03 | コニカミノルタホールディングス株式会社 | ガスバリア性フィルム、ガスバリア性フィルムの製造方法、および電子デバイス |
JP2013188942A (ja) * | 2012-03-14 | 2013-09-26 | Konica Minolta Inc | 水蒸気バリアーフィルムの製造方法、水蒸気バリアーフィルム及び電子機器 |
WO2013161809A1 (ja) * | 2012-04-26 | 2013-10-31 | コニカミノルタ株式会社 | ガスバリア性フィルム、およびこれを用いる電子デバイス |
JP2013233716A (ja) * | 2012-05-08 | 2013-11-21 | Mitsubishi Plastics Inc | ガスバリア性フィルム |
JP2014151571A (ja) * | 2013-02-08 | 2014-08-25 | Konica Minolta Inc | ガスバリア性フィルムおよびその製造方法、ならびに前記ガスバリア性フィルムを含む電子デバイス |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20120107607A1 (en) | 2009-07-17 | 2012-05-03 | Mitsui Chemicals, Inc. | Multilayered material and method of producing the same |
EP2554582A4 (en) | 2010-03-29 | 2014-03-05 | Lintec Corp | PRESSLING, MANUFACTURING METHOD, ELEMENT FOR AN ELECTRONIC DEVICE AND ELECTRONIC DEVICE |
US9267280B2 (en) * | 2012-02-14 | 2016-02-23 | Vireo Llc | Structural panels, cladding assemblies and components |
JP5578270B2 (ja) | 2013-12-18 | 2014-08-27 | コニカミノルタ株式会社 | ガスバリア性フィルム、その製造方法及びそのガスバリア性フィルムを用いた有機光電変換素子 |
-
2015
- 2015-08-10 JP JP2016547784A patent/JPWO2016039060A1/ja active Pending
- 2015-08-10 US US15/327,751 patent/US20170207415A1/en not_active Abandoned
- 2015-08-10 KR KR1020167035010A patent/KR20170010382A/ko not_active Application Discontinuation
- 2015-08-10 WO PCT/JP2015/072665 patent/WO2016039060A1/ja active Application Filing
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010167777A (ja) * | 2008-12-19 | 2010-08-05 | Samsung Electronics Co Ltd | ガス遮断性薄膜、これを備えた電子素子及びその製造方法 |
WO2013002026A1 (ja) * | 2011-06-27 | 2013-01-03 | コニカミノルタホールディングス株式会社 | ガスバリア性フィルム、ガスバリア性フィルムの製造方法、および電子デバイス |
JP2013188942A (ja) * | 2012-03-14 | 2013-09-26 | Konica Minolta Inc | 水蒸気バリアーフィルムの製造方法、水蒸気バリアーフィルム及び電子機器 |
WO2013161809A1 (ja) * | 2012-04-26 | 2013-10-31 | コニカミノルタ株式会社 | ガスバリア性フィルム、およびこれを用いる電子デバイス |
JP2013233716A (ja) * | 2012-05-08 | 2013-11-21 | Mitsubishi Plastics Inc | ガスバリア性フィルム |
JP2014151571A (ja) * | 2013-02-08 | 2014-08-25 | Konica Minolta Inc | ガスバリア性フィルムおよびその製造方法、ならびに前記ガスバリア性フィルムを含む電子デバイス |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2016152822A1 (ja) * | 2015-03-23 | 2016-09-29 | コニカミノルタ株式会社 | 導電性フィルム及び有機エレクトロルミネッセンス素子 |
JPWO2016152822A1 (ja) * | 2015-03-23 | 2018-01-11 | コニカミノルタ株式会社 | 導電性フィルム及び有機エレクトロルミネッセンス素子 |
WO2018021021A1 (ja) * | 2016-07-28 | 2018-02-01 | コニカミノルタ株式会社 | ガスバリア性膜、これを用いたガスバリア性フィルム、およびこれらを用いた電子デバイス、ならびにガスバリア性膜の製造方法 |
CN109477202A (zh) * | 2016-07-28 | 2019-03-15 | 柯尼卡美能达株式会社 | 气体阻隔性膜、使用它的气体阻隔性膜材和使用它们的电子设备、以及气体阻隔性膜的制造方法 |
JPWO2018021021A1 (ja) * | 2016-07-28 | 2019-05-09 | コニカミノルタ株式会社 | ガスバリア性膜、これを用いたガスバリア性フィルム、およびこれらを用いた電子デバイス、ならびにガスバリア性膜の製造方法 |
WO2018034179A1 (ja) * | 2016-08-18 | 2018-02-22 | コニカミノルタ株式会社 | ガスバリアー性膜、その製造方法及びそれを具備した電子デバイス |
JPWO2018034179A1 (ja) * | 2016-08-18 | 2019-06-13 | コニカミノルタ株式会社 | ガスバリアー性膜、その製造方法及びそれを具備した電子デバイス |
WO2018079429A1 (ja) * | 2016-10-28 | 2018-05-03 | リンテック株式会社 | 積層フィルム、電子デバイス用部材、及び電子デバイス |
JPWO2018079429A1 (ja) * | 2016-10-28 | 2019-09-19 | リンテック株式会社 | 積層フィルム、電子デバイス用部材、及び電子デバイス |
WO2020241821A1 (ja) * | 2019-05-31 | 2020-12-03 | キヤノン株式会社 | 活物質、活物質の製造方法、電極、及び電池 |
CN113906591A (zh) * | 2019-05-31 | 2022-01-07 | 佳能株式会社 | 活性材料、活性材料的制造方法、电极和电池 |
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