JP2001167875A - Absorbent holding structure of organic electroluminescent element - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an adsorbent holding structure of an organic electroluminescent EL element for holding the adsorbent by using a means hardly producing a volatile matter or water. SOLUTION: In the organic EL device including a transparent substrate 3, organic EL laminated film 4, and an enveloping member 5 made from magnetic substance, an adsorbent holding body 1 is fixed to inner wall of the enveloping member 5 by magnetic force. The adsorbent holding body 1 includes a metallic porous body, and a first and a second filters for covering the metallic porous body. The adsorbent is held at holes of the metallic porous body. The metallic porous body, and the first and the second filters are made from nickel and attracted in thickness direction of the adsorbent holding body 1 by magnetic force. The adsorbent holding body may be formed in a form such that the attracted metallic porous body covers mold of the adsorbent, the adsorbent and permanent magnet being held by magnetic container, or magnetic powder mixed and molded with the adsorbent is attracted.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] 1. Field of the Invention [0002] The present invention relates to an adsorbent holding structure in an organic electroluminescence (EL) device.

[0002]

2. Description of the Related Art Moisture and oxygen (hereinafter referred to as "moisture etc.")
Also called. ) May be disposed. Usually it is preferable to arrange so that the adsorbent is not scattered,
(1) A method in which a compound having an adsorption function is solidified into a pellet or the like to form a molded body, and the molded body is fixed to the inner wall of the organic EL element. (2) The compound is fixed in a bag having air permeability. Methods and the like are known (Japanese Unexamined Patent Publication No. 9-148).
066). In addition, a filter made of Teflon or the like may be arranged on the lower surface of the molded body in order to prevent the adsorbent from scattering from the molded body. These molded articles, air-permeable bags and filters are usually fixed to the organic EL device using an adhesive or a pressure-sensitive adhesive (hereinafter also referred to as “adhesive or the like”).

[0003]

However, when an adhesive or the like is used to hold the adsorbent in the organic EL device, a low molecular weight compound volatilized from the adhesive or the like (hereinafter, also referred to as a "volatile compound"). ) Or moisture adsorbed on the bag or filter may adversely affect the organic EL thin film and cause dark spots or the like.

An object of the present invention is to provide an adsorbent holding structure for an organic EL device, in which an adsorbent is held by means that hardly generates volatile compounds and moisture.

[0005]

According to a first aspect of the present invention, there is provided an adsorbent holding structure comprising a transparent substrate, an organic EL laminated film formed on the surface of the transparent substrate, and a magnetic material integrated with the transparent substrate. A sealing member for sealing the organic EL laminated film, wherein the inner wall of the sealing member includes an adsorbent holding member that includes a member made of a magnetic material and holds an adsorbent. It is characterized by being fixed by magnetic force.

It is preferable that the adsorbent holding member includes a “magnetized member” made of a magnetized magnetic material. For example, an adsorbent holding body in which an adsorbent is held in pores of the porous metal body using a porous metal body as a magnetized member can be used. Further, a porous metal sheet may be used as the magnetized member, and the adsorbent holding body may hold the adsorbent in a container made of the porous metal sheet. Further, a bulk metal member such as a bar magnet or a plate-like magnet may be used as the magnetized member, and the adsorbent and the magnetized member may be held by a container made of a magnetic material. A magnetized magnetic powder formed by mixing with an adsorbent may be used as a magnetized member.

Hereinafter, the present invention will be described in detail. In this specification, “magnetic material” refers to a so-called ferromagnetic material, and typical examples thereof include metal oxides such as Fe, Ni, Co, permalloy, magnetic stainless steel or alloys thereof, and ferrite. No. The term "magnetized member" means a magnetic material (hard magnetic material) having a high coercive force that has undergone the magnetization process and has exhibited the characteristics of a permanent magnet. They say "magnetize." A member made of a magnetic material is called a magnetic member.

[0008] As the above-mentioned "transparent substrate", a substrate made of a material having such a degree of transparency that characters and figures due to light emission of the organic EL laminate are not impaired can be used. In addition, it is preferable that the organic EL element has strength enough to maintain the shape of the surface layer of the organic EL element and has such hardness that the surface is not easily damaged. Such substrates include, besides glass, polyethylene terephthalate,
Those made of polyethersulfone, polycarbonate and the like can also be used. The transparent substrate may be colorless and transparent, or may be colored and transparent with an appropriate color tone.

An "organic EL laminated film" is formed by laminating an anode, an organic EL film and a cathode on this transparent substrate. The organic EL film disposed between the two electrodes includes at least a light emitting layer, and may have a hole transport layer and / or an electron transport layer in addition to the light emitting layer. It may have an injection layer. Various known materials can be used for the materials constituting the anode, the cathode, and the organic EL film. The method of forming each of these layers includes a vacuum deposition method, a spin coating method, a casting method, a sputtering method,
What is necessary is just to select suitably from methods, such as LB method.

The above-mentioned "sealing member" has a joining surface which is joined to the transparent substrate at the periphery thereof, and the other parts include the sealing member, the adsorbent holder attached thereto and the organic EL laminate. It is preferable that the shape is such that a space is formed to the extent that no contact occurs. The sealing member is made of a magnetic material, for example, a hard magnetic material such as a magnet alloy (magnet steel), ferrite and samarium cobalt, Fe, Ni, Co,
Soft magnetic materials such as permalloy and magnetic stainless steel can be used. This magnetic material may or may not be magnetized depending on the combination with the configuration of the adsorbent holder described below, and is preferably not magnetized from the viewpoint of handleability. Normally, it is preferable that the sealing member is made of only a magnetic material. However, for example, a sealing member or the like having a central portion made of a magnetic material and a peripheral portion made of a non-magnetic material is also used as the sealing member in the present invention. be able to. Further, a magnetic material may be laminated on the inner surface (sealing space side) or the outer surface of the sealing member made of a non-magnetic material.

The sealing member and the substrate are integrated, for example, by bonding the bonding surface and the substrate with a sealing resin. As the sealing resin, a thermosetting resin or a photosetting resin made of an epoxy resin, an acrylate resin, or the like can be used. Among them, it is preferable to use a photocurable resin that is cured by ultraviolet light (UV) or the like because of its high curing speed. In addition, in order to suppress a decrease in luminance or the like, it is more preferable to use a sealing resin that forms a cured body through which moisture or the like hardly permeates. In order to sufficiently suppress the invasion of moisture and the like, it is advantageous that the thickness of the resin layer on the bonding surface is thinner, and it is preferable that the thickness be smaller as long as the bondability is not impaired.

The "adsorbent" used in the present invention is not particularly limited.
That can absorb and remove moisture, etc.
I just need. As an adsorbent for removing water, (1)
Na _TwoO, K_TwoAn alkali metal oxide such as O, BaO,
Alkaline earth metal oxides such as CaO and SrO, (2) M
gCl_Two, CaCl_TwoMetal halides such as (3) Al
Potassium and alkaline earth metals and their metals
Alloy, (4) activated alumina, silica gel, zeolite, etc.
One or more selected from general adsorbents
Can be used. Of these, moisture is physically adsorbed
Moisture is more chemically adsorbed than common adsorbents
Alkali metal oxides and / or alkalis that are stably retained
An earth metal oxide or the like is preferably used. Adsorbent form
The shape is not particularly limited, such as powder, granule, pellet and the like
can do. If powder or granular
This is preferable because the wearing area increases. On the other hand, pellet
The advantage of good handling of the adsorbent
Can be

"Adsorbent Holder" for Holding the Adsorbent
Includes a member made of a magnetic material, and is fixed to an inner wall of a sealing member made of a magnetic material by a magnetic force. Examples of the method of “fixing by magnetic force” include (a) an adsorbent holding member having a magnetized magnetic member (magnetized member) and a non-magnetized magnetic member serving as a sealing member. (B) a method using a magnetized member but not a magnetized member as an adsorbent holder, and using a magnetized member as a sealing member, (c) an adsorbent holder and sealing A method in which both of the members are composed of magnetized members, (d)
A method in which both the adsorbent holding body and the sealing member include a magnetic member but do not include a magnetized member, and a magnetized member such as a bar magnet or a plate magnet is attached to the outer wall of the sealing member. No. Of these, like (a) or (c),
It is preferable that at least the adsorbent holder has a magnetized member, and the method (a) is most preferable because of easy production.

As the adsorbent holder having the magnetized member, there can be mentioned, as in the third invention, one in which an adsorbent is held in pores of a magnetized porous metal body. The above "porous metal body" has a large number of pores, and many of them communicate with each other. The preferred porosity is 60 to 98 vol%.
And more preferably 70 to 95% by volume. If the porosity is too low, sufficient adsorption performance may not be exhibited, and if the porosity is too high, handling during production becomes difficult. The average pore diameter of the pores is usually about 50 to 500 μm, and preferably 200 to 400 μm. As the material of the porous metal body, a hard magnetic material having a high coercive force (for example, a magnet alloy, ferrite, samarium cobalt, or the like) is used. In order to hold the adsorbent in the pores of the porous metal body, for example, powder of the adsorbent may be sprayed on the porous metal body. The average particle size of the adsorbent powder is preferably about 1 to 500 μm (more preferably 10 to 150 μm). According to this method, the adsorbent can be held in a form having a large surface area. The magnetization of the porous metal body may be performed before or after holding the adsorbent, but from the viewpoint of easy handling, it is preferable to magnetize after holding the adsorbent.

In the adsorbent holding body of the third invention, in order to prevent the adsorbent powder from dropping and scattering from the pores of the porous metal body and to facilitate handling of the adsorbent holding body,
Normally, the porous metal body is covered with a filter that has gas permeability and does not leak the adsorbent powder. This filter is
It is preferable to cover at least the lower surface of the porous metal body, more preferably to cover the lower surface and side surfaces, and it is more preferable to cover almost the entire surface. As the material of the filter, a magnetic alloy (magnet steel), a hard magnetic material such as ferrite and samarium cobalt, or a porous metal made of a soft magnetic material such as Fe, Ni, Co, permalloy and magnetic stainless steel is preferably used. The metal porous body is moderately (for example, porosity of 20% by volume or less, more preferably 10% by volume
It is particularly preferred to use a compressed porous metal compact (below). In the adsorbent holding body covered with the filter made of porous metal, the magnetization of the porous metal body may be performed at any stage before or after the covering with the filter, but from the viewpoint of easy handling, after the covering with the filter. It is preferable to magnetize. In addition, it is preferable to use a filter made of a hard magnetic material and to magnetize the filter in the same direction as the porous metal body, since the fixing to the sealing member by the magnetic force is ensured.

The adsorbent holder used in the present invention may be one in which the adsorbent is held by a container made of a magnetized porous metal sheet as in the fourth invention. As the porous metal sheet, a sheet made of a hard magnetic material such as a magnet alloy (magnet steel), ferrite, and samarium cobalt, having air permeability and not leaking the adsorbent may be used.
A metal film, the above-described porous metal compact, or the like can be used. The shape of the container may be any of a bowl shape, a bag shape, and the like as long as it can hold the adsorbent.However, the container is securely fixed to the sealing member by a magnetic force, and it is easy to prevent scattering of the adsorbent. And a bag shape is preferred.

Another configuration of the adsorbent holder used in the present invention is, as in the fifth invention, one that holds a bulk magnetized member and an adsorbent in a container made of a magnetic material. . As the bulk magnetized member, a bar magnet or a plate magnet made of a ferrite magnet, a samarium cobalt magnet, or the like can be used. As the material of the container, a porous metal sheet is preferably used, and its shape may be any of a bowl shape, a bag shape, and the like as long as it can hold a bulk magnetized member and an adsorbent. As the material of the porous metal sheet, any of a hard magnetic material and a soft magnetic material can be used, but a soft magnetic material is preferable because of easy processing.

In the fourth and fifth aspects of the present invention, the adsorbent held in the container may be in the form of a powder, or may be formed by compression or the like. It is preferable to use a molded article from the viewpoints of workability in storing the adsorbent in the container, prevention of scattering of the adsorbent, and easy handling of the adsorbent holder. On the other hand, in the case of powder, there is an advantage that the adsorption performance is excellent. The powdery adsorbent may be held in pores of the non-magnetized porous metal body. The magnetization of the container may be performed before storing the adsorbent, or may be performed after storing the adsorbent. Further, in order to prevent scattering of the adsorbent and facilitate handling of the adsorbent holder, at least the lower surface of the adsorbent holder is preferably covered with a container, and the lower surface and side surfaces are covered. It is more preferable that almost the entire circumference is covered.

As still another configuration of the adsorbent holder used in the present invention, there is provided an adsorbent holder having a magnetized member obtained by magnetizing a magnetic powder formed by mixing with an adsorbent as in the sixth invention. Can be A mixture of a magnetic powder made of a hard magnetic material such as a magnet alloy (magnet steel), ferrite, and samarium cobalt and an adsorbent powder is formed by compression or the like, and then the magnetic powder in the formed body is magnetized to be adsorbed. The agent holder can be fixed to the sealing member by magnetic force. In order to prevent the adsorbent powder and the magnetic powder generated due to the damage of the molded body from adversely affecting the element, the molded body is usually permeable with a filter that does not leak the adsorbent and the magnetic powder. It is preferable to cover the periphery. As a material of the filter, a metal porous body is preferably used,
Either a hard magnetic material or a soft magnetic material can be used as the material, but a soft magnetic material is preferable because of easy processing.

The magnetization of the magnetic material may be performed by a conventionally known method, such as placing the magnetic material in a strong magnetic field that is generated electrically. The direction of magnetization is not particularly limited, but is preferably a direction in which the lines of magnetic force of the magnetized member are substantially perpendicular to the surface on which the adsorbent holder is fixed.

[0021]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described more specifically by way of examples. Example 1 (1) Configuration of Adsorbent Holder As shown in FIG. 2, the adsorbent holder 1 is substantially disc-shaped with a diameter of 30 mm and a thickness of 1.5 mm, and is magnetized in the thickness direction of the disc. Have been. Note that the arrow H in FIG. 2 indicates the direction of the line of magnetic force. The adsorbent holder 1 is a nickel porous body having a thickness of 2.5 mm (trade name “FO” manufactured by Katayama Special Industrial Co., Ltd.).
RMEX500 ", porosity 97 vol%, average pore diameter about 20
0 μm) and a plate-shaped first filter portion 11 made of a porous metal compact formed by pressing the nickel porous body and covering one surface of the metal porous body 10.
And a bowl-shaped second filter portion 12 that covers the other surface of the porous metal body 10. In the pores of the metal porous body 10, BaO powder 0.15 as an adsorbent 2 having an average particle size of 100 μm was used.
g is retained. Further, the porous metal compact is compressed to such an extent that the adsorbent 2 does not leak, and its porosity is about 9% by volume.

The adsorbent holder 1 is made of, for example, a plate-shaped porous metal compact by compressing the nickel porous body to a thickness of 0.3 mm. The compression body is laminated on the upper and lower sides of the body 10, and the laminated body is formed by punching with a punch or the like, and the molded article is placed in a magnetic field and magnetized in the thickness direction of the adsorbent holding body 1. be able to. The obtained adsorbent holding body 1 did not leak the adsorbent 2 to the outside even if vibration was applied in any direction, and was excellent in handleability.

(2) Structure of Organic EL Element As shown in FIG. 1, a transparent substrate 3 made of soda-lime glass having a length of 75 mm × width 150 mm × thickness 1.1 mm is provided with an anode 41 made of ITO and an organic EL element. A film 42 and a cathode 43 made of an aluminum alloy are sequentially laminated to form an organic
The L laminated film 4 is formed. The organic EL film 42 includes, in order from the cathode 43 side, an electron injection layer made of LiF, an electron transport layer made of an aluminum quinolium complex, a light emitting layer doped with quinacridone using an aluminum quinolium complex as a host,
A hole transport layer made of TPTE (a tetramer of triphenylamine) and a hole injection layer made of a copper phthalocyanine complex are laminated (both are not shown). On the other hand, the sealing member 5 is made of magnetic stainless steel (soft magnetic material) having a thickness of 0.4 mm, and is press-formed into a dish having a concave portion 51 corresponding to the adsorbent holder 1 at the center. After the adsorbent holding body 1 obtained above is heated at 350 ° C. for 30 minutes to remove moisture and the like, the adsorbent holding body 1 is arranged in the concave portion 51,
It is held on the inner wall of the sealing member 5 by magnetic force. Thereafter, the peripheral portion of the sealing member 5 is joined to the transparent substrate 3 using an acrylic ultraviolet curing adhesive 6, whereby an organic EL element in which the organic EL laminated film 4 is hermetically sealed is obtained.

(Example 2) As shown in FIG. 3, the adsorbent holder 1 is composed of an adsorbent pellet 21 having a diameter of 35 mm and a thickness of 1 mm obtained by compression-molding 5 g of BaO powder having an average particle diameter of 100 μm. And a porous metal sheet 13 covering the entire surface of the adsorbent pellet 21. This porous metal sheet 13 is made of the porous metal compact used in Example 1,
By being placed in a magnetic field after covering the adsorbent pellet 21, the adsorbent holder 1 is magnetized in the thickness direction.
As in the first embodiment, the adsorbent holding body 1 can be held on the inner wall of the sealing member 5 made of a magnetic material by magnetic force.

(Embodiment 3) As shown in FIG. 4, the adsorption holder 1 includes a metal porous body 10 made of the nickel porous body used in Embodiment 1, and the adsorbent 2 And 0.15 g of BaO powder having an average particle size of 100 μm. On the upper surface of the porous metal body 10, a plate-like magnet 14 as a bulk metal member is arranged. The plate-shaped magnet 14 is made of a samarium-cobalt material, and has a shape of a prism of 15 mm × 15 mm × 0.5 mm. The metal porous body 10 and the plate-like magnet 14 are formed by pressing the nickel porous body to form the first filter unit 11.
And a second filter unit 12. In the present embodiment, none of the porous metal body 10, the first filter section 11, and the second filter section 12 are magnetized. Since the adsorbent holder 1 has the plate-shaped magnet 14 as a magnetized member, it can be held on the inner wall of the sealing member 5 by magnetic force, as in the first embodiment.

Example 4 As shown in FIG. 5, 3 g of BaO powder having an average particle size of 100 μm was compression-molded together with the plate magnet 14 used in Example 3 to obtain the plate magnet 1.
The adsorbent pellet 21 in which No. 4 was embedded almost in the center was formed. Next, the lower surface and the side surfaces of the adsorbent pellets 21 are covered with the porous metal sheet 13 made of the porous metal compact used in Example 1, and the upper end is caulked.
A container (not magnetized) made of the porous metal sheet 13 and holding the adsorbent pellets 21 and the plate-like magnets 14 was formed. This adsorbent holder 1 is similar to the first embodiment,
It can be held on the inner wall of the sealing member 5 by magnetic force.

Example 5 As shown in FIG. 6, 3 g of BaO powder having an average particle diameter of 100 μm and 3 g of ferrite powder having an average particle diameter of 150 μm were mixed and compression-molded to contain a magnetic powder 15. Adsorbent pellets 21 were obtained. This adsorbent pellet 21 is wrapped with a porous metal sheet 13 made of permalloy (Ni78.5, Fe21.5), which is a soft magnetic material.
The magnetic powder 15 was magnetized in the thickness direction to obtain the adsorbent holder 1. The adsorbent holder 1 can be held on the inner wall of the sealing member 5 by magnetic force, as in the first embodiment.

[0028]

According to the adsorbent holding structure of the present invention, since the adsorbent holding body is fixed by magnetic force, there is no need to worry about generation of volatile compounds unlike the conventional technique of fixing using an adhesive or the like. In addition, when a defect occurs in another portion of the organic EL element during manufacturing or the like, the adsorbent holder can be easily removed from the organic EL element and reused.
A metal porous body, a porous metal sheet, or the like used for holding the adsorbent and preventing scattering thereof is preferable because it does not easily adsorb moisture unlike a Teflon filter or the like. In addition, since the adsorbent holder can be made of only a material having higher heat resistance than a Teflon filter or the like, the adsorbent holder is heated before being attached to the element, so that the adsorbed moisture and the like can be surely removed. The heating can be performed at high temperature in a short time.

[Brief description of the drawings]

FIG. 1 is a longitudinal sectional view showing an adsorbent holding structure in an organic EL device of Example 1.

FIG. 2 is a longitudinal sectional view showing an adsorbent holding body used in the adsorbent holding structure of Example 1.

FIG. 3 is a longitudinal sectional view showing an adsorbent holding body used in the adsorbent holding structure of Example 2.

FIG. 4 is a longitudinal sectional view showing an adsorbent holding body used in the adsorbent holding structure of Example 3.

FIG. 5 is a longitudinal sectional view showing an adsorbent holding body used in the adsorbent holding structure of Example 4.

FIG. 6 is a longitudinal sectional view showing an adsorbent holding body used in the adsorbent holding structure of Example 5.

[Explanation of symbols]

1; adsorbent support, 10; metal porous body, 11; first filter section, 12; second filter section, 13; porous metal sheet, 14; plate magnet, 15; magnetic powder, 2; 2
1; adsorbent pellet; 3; transparent substrate; 4; organic EL laminated film; 5; sealing member.

 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 3K007 AB00 AB13 AB18 BB00 BB01 BB02 BB05 CA01 CA05 CB01 DA00 DB03 EB00 FA01 FA02 FA03

Claims (6)

[Claims] 1. A transparent substrate, an organic EL laminated film formed on a surface of the transparent substrate, a sealing member made of a magnetic material and integrated with the transparent substrate to seal the organic EL laminated film, An organic EL element comprising: an adsorbent holder that includes a member made of a magnetic material and holds an adsorbent is fixed by magnetic force to an inner wall of the sealing member. Adsorbent holding structure. 2. The adsorbent holding structure for an organic EL device according to claim 1, wherein the adsorbent holding body includes a magnetized member. 3. The organic EL element holding structure according to claim 2, wherein the magnetized member is a porous metal body, and the adsorbent is held in pores of the porous metal body. 4. The adsorbent holding structure for an organic EL device according to claim 2, wherein the magnetized member is a porous metal sheet, and the adsorbent is held by a container made of the porous metal sheet. 5. The magnetized member is a bulk metal member, and the adsorbent holder holds the adsorbent and the magnetized member in a container made of a magnetic material. 3. The adsorbent holding structure of the organic EL device according to claim 1. 6. The adsorbent holding structure for an organic EL device according to claim 2, wherein the magnetized member is obtained by magnetizing a magnetic powder formed by mixing with the adsorbent.