WO2003080235A1 - Flexible film-type desiccant body for enclosed electronic device and production method of the same - Google Patents
Flexible film-type desiccant body for enclosed electronic device and production method of the same Download PDFInfo
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- WO2003080235A1 WO2003080235A1 PCT/KR2003/000589 KR0300589W WO03080235A1 WO 2003080235 A1 WO2003080235 A1 WO 2003080235A1 KR 0300589 W KR0300589 W KR 0300589W WO 03080235 A1 WO03080235 A1 WO 03080235A1
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- desiccant
- moisture
- porous
- polymer binder
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28026—Particles within, immobilised, dispersed, entrapped in or on a matrix, e.g. a resin
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- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0248—Compounds of B, Al, Ga, In, Tl
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Definitions
- the present invention relates to a flexible film-type desiccant body used for electronic devices that are sealed within enclosures to avoid failure by moisture, such as organic electro-luminescence (EL) devices, polymer EL and charge couple devices (CCD) for displaying information, and a method for producing the body.
- EL organic electro-luminescence
- CCD charge couple devices
- MVTR moisture vapor transmission rate
- the performance of a desiccant body used in the enclosed electronic devices is determined by the speed and amount of desiccation and the equilibrium moisture density at an equilibrium state.
- a good desiccant body features a faster desiccation speed and a lower equilibrium moisture density.
- Desiccants are broken down into desiccants using physical absorption such as silica gel and those using chemical absorption.
- the physical desiccants have a high equilibrium moisture density and highly depend on temperature such that if temperature goes up even within the range of typical operation temperature, the physical desiccants release moisture again.
- the desiccants removing moisture by chemical reactions such as alkaline metal oxides, alkaline earth metal oxides, sulfate, metal halides, perchlorates, phosphorus pentoxide, metal hydrides, and other metals with a higher ionization tendency than hydrogen, have a low equilibrium moisture density because inverse reaction hardly occurs in the typical operation temperature range for electronic devices.
- U.S. Pat. No. 4,405,487 discloses a desiccant body which removes moisture by making aluminum and zinc powder react with moisture and removes the resultant hydrogen by coupling the hydrogen with unsaturated organic substance in the presence of a catalyst, and a method for producing this desiccant body in the form of pellet by hot pressing.
- the body and method have drawbacks that the speed of removing hydrogen is slow and it is difficult to make the desiccant body in the form of a flexible film.
- Japanese laid-open patent No. 3(1991 )-261091 discloses a desiccant body for an organic EL device in which phosphorous pentoxide powder is stored in an air-permeable container and is placed inside an organic EL device.
- the body since the body is in the form of power, it is inconvenient to use.
- phosphoric acid which is generated when the phosphorous pentoxide powder reacts with moisture, has a low melting point ranging from 41 to 44°C, the phosphoric acid may leak out of the container even at an ordinary operation temperature and contaminate the electronic circuit device.
- U.S. Pat. No. 5,304,419 discloses a method of blending a pressure sensitive adhesive with a desiccant
- U.S. Pat. No. 5,401 ,536 discloses a method of blending a polymer with alumina silicate powder
- U.S. Pat. No. 5,591 ,379 discloses a method of blending a moisture-permeable binder with a desiccant such as a molecular sieve.
- the methods are based on physical moisture absorption and moisture should permeate the molecular layer of the binder, the speed of moisture absorption is slow and moisture is released again at room temperature.
- desiccant substance which absorbs moisture by chemical reactions is mostly in the form of solid state powder when the substance does not absorb moisture, and in this state the desiccation speed of the substance is the fastest.
- the desiccant substance in order to be placed inside a high-tech electronic device ever-getting smaller and thinner, after securing a predetermined space the desiccant substance should be separated by a moisture-permeable diaphragm, or should be inserted into a moisture-permeable envelop and then attached to the inside, which increases the thickness of the devices and the expenses.
- U.S. Pat. No. 5,882,761 discloses a method using metal oxide, metal sulfate, metal halide and metal perchlorate in the form of powder or using after coating them inside an organic EL device by vapor deposition, sputtering, or spin coating.
- U.S. Pat. No. 6,226,890 discloses a method by which a desiccant body is obtained by blending a polymer having a high MVTR with metal oxide, metal sulfate, metal halide and metal perchlorate, and the body is attached to an enclosed electronic device and then is used.
- This method has an advantage of easiness-to-use.
- water molecules should permeate through the molecular combination layer of the polymer binder. Accordingly, even though a polymer having a high MVTR is used, the desiccation speed is greatly lowered compared to when the desiccant body is used in the form of powder. Disclosure of the Invention
- the present invention provides a desiccant body (12) which has a flexible thin-film shape so as to be conveniently attached to the inside of a thin enclosed electronic device (10) and be used, and has countless fine pores formed inside the desiccant body (22) such that movement of moisture is quickly performed and the speed of desiccation is high, and a method of therefor.
- number 11 is, for example, electronic circuit.
- a desiccant body (12) for enclosed electronic devices comprising: a desiccant substance (23) which removes moisture by reacting with moisture; a porous substance (20) which with fine pores provides transfer passages for moisture, and contains gas or a volatile substance so that when the desiccant body is formed, fine pores can be formed in a polymer binder (21); and a polymer binder which gives a shape to a mixture of the desiccant substance and porous substance and in which, when the desiccant body is formed, fine pores are formed by releasing of the gas or volatile substance contained in the porous substance such that transfer passages for moisture are provided.
- the desiccant substance a chemical desiccant substance which does not release again moisture even though the surrounding temperature goes up after moisture is absorbed is used.
- this desiccant substance alkaline metal oxides, alkaline earth metal oxides, sulfate, metal halides, perchlorates, phosphorus pentoxide, metal hydrides, and other metals with a higher ionization tendency than hydrogen and mixtures thereof are used.
- any one of lithium (Li), potassium (K), sodium (Na), calcium (Ca), barium (Ba), aluminum (Al), and mixtures thereof is selected and used.
- Most porous substances have a characteristic of absorbing moisture by absorption. However, their equilibrium moisture density is very high and the substances release again moisture if temperature goes up. Accordingly, the substances are not appropriate as absorption body for electronic devices sensitive to moisture. In the present invention, since a chemical desiccant substance spread neighboring a porous substance immediately absorbs moisture, the function of the porous substance as a desiccant body can be neglected.
- the porous substance provides a function as a vector of a desiccant substance and a function for providing a passage for moisture transfer.
- a porous substance any one of active carbon, silica gel, active alumina, zeolite, diatomaceous earth, porous resin, and porous fiber, or mixtures thereof, is selected and used as a solid substance in the form of particles with a diameter equal to or less than 1mm, or a filamentous solid substance with a diameter equal to or less than 1mm in which pores with a diameter of 03nm ⁇ 100microns are formed.
- the gas or volatile substance contained in the porous substance has a function for forming fine pores in the polymer binder in the desiccant body manufacturing process.
- the gas or evaporated volatile substance in the pores of the porous substance goes through the polymer binder to the outside such that fine pores are formed in the polymer binder.
- the pores of the polymer binder become moisture transfer passages to improve the desiccation speed.
- the MVTR of the substance used as the polymer binder does not matter greatly. Accordingly, considering the mechanical intensity and chemical stability of the polymer, a shape for the mixture of the desiccant substance and the porous substance is given. If fine pores that will become transfer passages for moisture can be formed by gas or volatile substance contained in a polymer substance in the manufacturing process, the polymer can be used.
- the desiccant body for enclosed electronic devices of the present invention is manufactured by a process comprising producing a mixture of a desiccant substance and a porous substance; blending the mixture of the desiccant substance and the porous substance with a polymer binder; forming a film; and forming fine pores in the polymer binder.
- a step for curing the polymer binder may be added. First, as shown in FIG. 2, the mixture of the desiccant substance and the porous substance is made such that the desiccant substance 23 is dispersed neighboring the surface or pores of the porous substance 20.
- the porous substance Since only physically mixing the desiccant substance and the porous substance has a limit, a more precise method is needed. At this time, after filling fine pores of the porous substance with nitrogen or an inert gas, or a volatile liquid having a low boiling point, the porous substance is used so that after the forming, fine pores can be formed in the polymer binder.
- One method for producing a desiccant substance and a porous substance is vapor deposition or sputtering of a desiccant substance on the porous substance.
- Another method is using a small amount of a liquid substance such as a volatile liquid, a high boiling point liquid having a low vapor pressure enough to no contaminate the inside by natural evaporation, or a coupling body so that the desiccant substance can be evenly dispersed on the surface or pores of the porous substance.
- the two substances are physically blended or are blended by using a solvent.
- the mixture of the polymer binder and the desiccant mixture body (the mixture body of the desiccant substance and the porous substance) may be formed with a desired thickness on a polymer film or release liner by using an ordinary machine tool or equipment, or without forming a separate film, the mixture may be directly applied on the inside of the sealed case of an enclosed electronic device and used.
- the step for forming fine pores in the polymer binder is the most characteristic step. This step may be performed by applying heat to the formed film, or reducing the pressure. If heat is applied to the formed film or the film is placed inside a vacuum container and then pressure is reduced, the gas or volatile substance in the fine pores of the porous substance leaks out from the film, making passages in the polymer binder.
- the desiccant body according to the present invention can select and use a polymer binder virtually irrespective of its MVTR, and has a desiccation speed 5 -20 times higher that of a desiccant film having no fine pores formed.
- the desiccant body according to the present invention can be used by being mixed with an oxygen getter or a hydrogen getter, when necessary.
- FIG. 1 is a conceptual diagram of an enclosed electronic device to which the present invention is applied.
- FIG. 2 is a schematic diagram of a fine structure of a desiccant body of the present invention.
- a white paste was produced and the produced paste was coated on a polyester film. The film was heated at 60°C for 10 minutes with the pressure of 1 Torr so that fine pores could be formed. Then the film was cooled for curing. As a result, a white flexible desiccant film having the thickness of 2mm was produced.
- EXAMPLE 2 Calcium oxide (CaO) was used as a desiccant substance, active carbon as a porous substance and hot melt of ethylenevinylacetate series as a polymer binder to produce the desiccant body.
- Barium oxide (BaO) was used as a desiccant substance, active carbon as a porous substance and UV cured resin of polyurethane series as a polymer binder to produce the desiccant body.
- Phosphorous pentoxide was used as a desiccant substance, active carbon as a porous substance and polybutadiene having a mean molecular weight of 2,500,000 as a pplymer binder to produce the desiccant body.
- Lithium aluminum hydride (LiAIH 4 ) was used as a desiccant substance, active carbon as a porous substance and polybutadiene having a mean molecular weight of 2,500,000 as a polymer binder to produce the desiccant body.
- Lithium (Li) and aluminum (Al) were used as desiccant substances, active alumina as a porous substance and polybutadiene having a mean molecular weight of 2,500,000 as a polymer binder to produce the desiccant body.
- LiAIH LiAIH
- 500mg diethyl ether solution 500mg diethyl ether solution, and 50mg active alumina in which moisture is removed by vacuum heating, in a glove box in a nitrogen atmosphere, the mixture was heated at 200°C for long hours.
- lithium aluminum hydride was decomposed and hydrogen was removed, and lithium and aluminum metals were coated on the fine pores and surface of active alumina.
- a solution of 100 mg of fluorocarbon elastomer dissolved at 15wt% in tetrahydrofuran was additionally blended.
- a gray paste was produced and the produced paste was coated on polyester film.
- the film was heated at 80°C for 30 minutes with the pressure of 1 Torr so that the film could be cured with fine pores being formed.
- a black flexible desiccant film having the thickness of 0.2mm was produced.
- 100mg polybutadiene in ' the state of gum was blended.
- a white paste was produced and the produced paste was coated on a polyethylene film. The film was heated at 60°C for 10 minutes with the pressure of 1 Torr so that fine pores could be formed. Then, the film was cooled for curing. As a result, a white flexible desiccant film was produced.
- COMPARISON EXAMPLE 2 Calcium oxide (CaO) was used as a desiccant substance, active carbon as a porous substance and hot melt of ethylenevinylacetate series as a polymer binder to produce the desiccant body.
- Barium oxide (BaO) was used as a desiccant substance, active carbon as a porous substance and UV cured resin of polyurethane series as a polymer binder to produce the desiccant body.
- Phosphorous pentoxide was used as a desiccant substance, and polybutadiene having a mean molecular weight of 2,500,000 as a polymer binder to produce the desiccant body, but a porous substance was not used.
- Lithium aluminum hydride (LiAIH ) was used as a desiccant substance and polybutadiene having a mean molecular weight of 2,500,000 as a polymer binder to produce the desiccant body, but a porous substance was not used.
- LiAIH Lithium aluminum hydride
- 50mg lithium aluminum hydride powder and a solution of 100mg polybutadiene dissolved at 15wt% in hexane were blended.
- a white paste was produced and the produced paste was coated on a polyethylene film. The film was heated at 80°C for 30 minutes with the pressure of 1 Torr and then cured. As a result, a white flexible desiccant film having the thickness of 0.2mm was produced.
- the desiccant bodies produced by the examples 1 through 6 and compa ⁇ son examples 1 through 5 had been placed in the air at a temperate of 25°C and a relative humidity of 50% for 30 minutes. Then, by measuring the increased weight of each desiccant body, the mean desiccation speed was measured. The results are shown in the following table 1. Table 1
- the comparison example 5 shows a case in which because of not using a porous substance, even when heating or reduced pressure was applied after forming a film, there was no substance released through the polymer binders from the inside such that fine pores were not formed.
- the comparison samples 1 through 3 show the cases in which though a porous substance was used, the process of forming fine pores by applying heat or reduced pressure was not performed such that no fine pores were formed in polymer binders.
- the table 1 shows that when the desiccant bodies produced by the examples 1 through 5 were compared with those produced by the comparison examples 1 through 5, in which the same desiccant substances and polymer binders as in the examples 1 through 5 were used but the process of forming fine pores was not performed, the absorption speed of the desiccant bodies produced by the examples were ten times or more faster than that of the desiccant bodies produced by the comparison examples.
- the table also shows that, as in the example 2 and the comparison example 2, the desiccation speed difference was widened when polymer binders having a low MVTR was applied.
- a flexible thin film-type desiccant body which has a high desiccation speed and can be conveniently attached and used, without releasing moisture and without generated fluid products damaging electronic circuit devices even when the temperature goes up, and a method of therefor are provided. Accordingly, enclosed electronic devices which are constructed as an enclosure type to avoid moisture, such as organic EL devices and CCD, can be used under appropriate conditions for a longer time.
Abstract
A flexible film-type desiccant body used for electronic devices that are sealed within enclosures to avoid failure by moisture and a method of therefor are provided. The desiccant body has a thin and flexible film shape so as to be easily attached to the inside of a thin enclosed electronic device and provides a fast desiccation due to a number of fine pores inside the film. The desiccant body for enclosed electronic devices of the present invention comprises a desiccant substance which removes moisture by reacting with moisture; a porous substance which with fine pores provides transfer passages for moisture, and contains gas or a volatile substance so that when the desiccant body is formed, fine pores can be formed in a polymer binder; and a polymer binder which gives a shape to a mixture of the desiccant substance and porous substance and in which, when the desiccant body is formed, fine pores are formed by releasing of the gas or volatile substance contained in the porous substance such that transfer passages for moisture are provided.
Description
FLEXIBLE FILM-TYPE DESICCANT BODY FOR ENCLOSED ELECTRONIC DEVICE AND PRODUCTION METHOD OF THE SAME
Technical Field
The present invention relates to a flexible film-type desiccant body used for electronic devices that are sealed within enclosures to avoid failure by moisture, such as organic electro-luminescence (EL) devices, polymer EL and charge couple devices (CCD) for displaying information, and a method for producing the body.
In an enclosed electronic device, electronic circuit elements are formed inside a sealed case and the case is encapsulated by an adhesive polymer having a low moisture vapor transmission rate (MVTR). However, if moisture inflowing in the encapsulation process or moisture penetrating through an encapsulator is not removed, the function of the electronic device is gradually degraded. Accordingly, in addition to the encapsulation, the desiccant body is placed inside the sealed case.
The performance of a desiccant body used in the enclosed electronic devices is determined by the speed and amount of desiccation and the equilibrium moisture density at an equilibrium state. A good desiccant body features a faster desiccation speed and a lower equilibrium moisture density.
Background Art
Desiccants are broken down into desiccants using physical absorption such as silica gel and those using chemical absorption. The physical desiccants have a high equilibrium moisture density and highly depend on temperature such that if temperature goes up even within the range of typical operation temperature, the physical desiccants release moisture again. However, the desiccants removing moisture by chemical reactions, such as alkaline metal oxides, alkaline earth metal
oxides, sulfate, metal halides, perchlorates, phosphorus pentoxide, metal hydrides, and other metals with a higher ionization tendency than hydrogen, have a low equilibrium moisture density because inverse reaction hardly occurs in the typical operation temperature range for electronic devices.
U.S. Pat. No. 4,405,487 discloses a desiccant body which removes moisture by making aluminum and zinc powder react with moisture and removes the resultant hydrogen by coupling the hydrogen with unsaturated organic substance in the presence of a catalyst, and a method for producing this desiccant body in the form of pellet by hot pressing. However, the body and method have drawbacks that the speed of removing hydrogen is slow and it is difficult to make the desiccant body in the form of a flexible film.
Japanese laid-open patent No. 3(1991 )-261091 discloses a desiccant body for an organic EL device in which phosphorous pentoxide powder is stored in an air-permeable container and is placed inside an organic EL device. However, since the body is in the form of power, it is inconvenient to use. In addition, since phosphoric acid, which is generated when the phosphorous pentoxide powder reacts with moisture, has a low melting point ranging from 41 to 44°C, the phosphoric acid may leak out of the container even at an ordinary operation temperature and contaminate the electronic circuit device.
As methods for manufacturing desiccant bodies for enclosed electronic devices, U.S. Pat. No. 5,304,419 discloses a method of blending a pressure sensitive adhesive with a desiccant, U.S. Pat. No. 5,401 ,536 discloses a method of blending a polymer with alumina silicate powder, and U.S. Pat. No. 5,591 ,379 discloses a method of blending a moisture-permeable binder with a desiccant such as a molecular sieve. As the methods are based on physical moisture absorption and moisture should permeate the molecular layer of the binder, the speed of moisture absorption is slow and moisture is released again at room temperature.
In general, desiccant substance which absorbs moisture by chemical reactions is mostly in the form of solid state powder when the substance does not absorb moisture, and in this state the desiccation speed of the substance is the fastest. However, in order to be placed inside a high-tech electronic device ever-getting smaller and thinner, after securing a predetermined space the desiccant substance should be separated by a moisture-permeable diaphragm, or should be inserted into a moisture-permeable envelop and then attached to the inside, which increases the thickness of the devices and the expenses. Also, there are methods of applying desiccant substances to the inside of sealed cases through vapor deposition or sputtering. However, the processes of the methods are difficult. If absorbing moisture, unit molecules swell and leak from the sealed case and it is highly probable that the substance contaminates the inside. Accordingly, to avoid this problem, a diaphragm should be used. In order to solve this drawback, a method using a polymer binder having a high MVPR has been researched.
U.S. Pat. No. 5,882,761 discloses a method using metal oxide, metal sulfate, metal halide and metal perchlorate in the form of powder or using after coating them inside an organic EL device by vapor deposition, sputtering, or spin coating.
U.S. Pat. No. 6,226,890 discloses a method by which a desiccant body is obtained by blending a polymer having a high MVTR with metal oxide, metal sulfate, metal halide and metal perchlorate, and the body is attached to an enclosed electronic device and then is used. This method has an advantage of easiness-to-use. However, in order for moisture to be transferred to a desiccant substance from the outside, water molecules should permeate through the molecular combination layer of the polymer binder. Accordingly, even though a polymer having a high MVTR is used, the desiccation speed is greatly lowered compared to when the desiccant body is used in the form of powder.
Disclosure of the Invention
To solve the above problems, the present invention provides a desiccant body (12) which has a flexible thin-film shape so as to be conveniently attached to the inside of a thin enclosed electronic device (10) and be used, and has countless fine pores formed inside the desiccant body (22) such that movement of moisture is quickly performed and the speed of desiccation is high, and a method of therefor. In FIG. 1 , number 11 is, for example, electronic circuit.
According to an aspect of the present invention, there is provided a desiccant body (12) for enclosed electronic devices comprising: a desiccant substance (23) which removes moisture by reacting with moisture; a porous substance (20) which with fine pores provides transfer passages for moisture, and contains gas or a volatile substance so that when the desiccant body is formed, fine pores can be formed in a polymer binder (21); and a polymer binder which gives a shape to a mixture of the desiccant substance and porous substance and in which, when the desiccant body is formed, fine pores are formed by releasing of the gas or volatile substance contained in the porous substance such that transfer passages for moisture are provided. For the desiccant substance, a chemical desiccant substance which does not release again moisture even though the surrounding temperature goes up after moisture is absorbed is used. As this desiccant substance, alkaline metal oxides, alkaline earth metal oxides, sulfate, metal halides, perchlorates, phosphorus pentoxide, metal hydrides, and other metals with a higher ionization tendency than hydrogen and mixtures thereof are used.
As a metal having a higher ionization tendency than hydrogen, any one of lithium (Li), potassium (K), sodium (Na), calcium (Ca), barium (Ba), aluminum (Al), and mixtures thereof is selected and used. Most porous substances have a characteristic of absorbing moisture by absorption. However, their equilibrium moisture density is
very high and the substances release again moisture if temperature goes up. Accordingly, the substances are not appropriate as absorption body for electronic devices sensitive to moisture. In the present invention, since a chemical desiccant substance spread neighboring a porous substance immediately absorbs moisture, the function of the porous substance as a desiccant body can be neglected. The porous substance provides a function as a vector of a desiccant substance and a function for providing a passage for moisture transfer. For a porous substance, any one of active carbon, silica gel, active alumina, zeolite, diatomaceous earth, porous resin, and porous fiber, or mixtures thereof, is selected and used as a solid substance in the form of particles with a diameter equal to or less than 1mm, or a filamentous solid substance with a diameter equal to or less than 1mm in which pores with a diameter of 03nm~100microns are formed. The gas or volatile substance contained in the porous substance has a function for forming fine pores in the polymer binder in the desiccant body manufacturing process. In other words, in the forming process, the gas or evaporated volatile substance in the pores of the porous substance goes through the polymer binder to the outside such that fine pores are formed in the polymer binder. The pores of the polymer binder become moisture transfer passages to improve the desiccation speed.
Since in the present invention fine pores are forcibly formed inside the polymer binder in the manufacturing process to provide moisture transfer passages, the MVTR of the substance used as the polymer binder does not matter greatly. Accordingly, considering the mechanical intensity and chemical stability of the polymer, a shape for the mixture of the desiccant substance and the porous substance is given. If fine pores that will become transfer passages for moisture can be formed by gas or volatile substance contained in a polymer substance in the manufacturing process, the polymer can be used. For example,
according to a method by which a polymer is used, any one of gum-type polymers, multi-component series reaction curing polymers which are polymerized by a catalyst or heat, hot-melt polymers, radiation curing polymers which are cured by visible light, ultraviolet (UV), and electronic beam (EV), solvent evaporation curing polymers which are used after polymers are melt into a solvent, and mixtures thereof is selected and used.
The desiccant body for enclosed electronic devices of the present invention is manufactured by a process comprising producing a mixture of a desiccant substance and a porous substance; blending the mixture of the desiccant substance and the porous substance with a polymer binder; forming a film; and forming fine pores in the polymer binder. Alternatively, after the step for forming fine pores in the polymer binder, a step for curing the polymer binder may be added. First, as shown in FIG. 2, the mixture of the desiccant substance and the porous substance is made such that the desiccant substance 23 is dispersed neighboring the surface or pores of the porous substance 20. Since only physically mixing the desiccant substance and the porous substance has a limit, a more precise method is needed. At this time, after filling fine pores of the porous substance with nitrogen or an inert gas, or a volatile liquid having a low boiling point, the porous substance is used so that after the forming, fine pores can be formed in the polymer binder.
One method for producing a desiccant substance and a porous substance is vapor deposition or sputtering of a desiccant substance on the porous substance. Another method is using a small amount of a liquid substance such as a volatile liquid, a high boiling point liquid having a low vapor pressure enough to no contaminate the inside by natural evaporation, or a coupling body so that the desiccant substance can be evenly dispersed on the surface or pores of the porous substance.
In the step for blending the mixture of the desiccant substance and the porous substance with the polymer binder, the two substances are physically blended or are blended by using a solvent.
When a film is formed, the mixture of the polymer binder and the desiccant mixture body (the mixture body of the desiccant substance and the porous substance) may be formed with a desired thickness on a polymer film or release liner by using an ordinary machine tool or equipment, or without forming a separate film, the mixture may be directly applied on the inside of the sealed case of an enclosed electronic device and used.
When compared to the conventional methods, the step for forming fine pores in the polymer binder is the most characteristic step. This step may be performed by applying heat to the formed film, or reducing the pressure. If heat is applied to the formed film or the film is placed inside a vacuum container and then pressure is reduced, the gas or volatile substance in the fine pores of the porous substance leaks out from the film, making passages in the polymer binder.
When the curing step is added, attention should be paid not to remove thus formed passages, and when viscosity is high enough such that the polymer binder is desired to be used without curing, attention should be paid not to directly apply pressure on the film.
Since the fine pores formed in the polymer binder are main passages for moisture, the desiccant body according to the present invention can select and use a polymer binder virtually irrespective of its MVTR, and has a desiccation speed 5 -20 times higher that of a desiccant film having no fine pores formed.
In addition, the desiccant body according to the present invention can be used by being mixed with an oxygen getter or a hydrogen getter, when necessary.
Brief Description of the Drawings
FIG. 1 is a conceptual diagram of an enclosed electronic device to which the present invention is applied; and
FIG. 2 is a schematic diagram of a fine structure of a desiccant body of the present invention.
Best mode for carrying out the Invention
The characteristics and advantages of the present invention are further illustrated by the following various examples:
EXAMPLE 1
Barium oxide (BaO) was used as a desiccant substance, silica gel as a porous substance and polybutadiene in the state of gum (viscosity = 40-90 poise at 45°C) as a polymer binder to produce the desiccant body. After blending 150mg BaO powder and 50mg silica gel, in which moisture is removed by vacuum heating, in a glove box in a nitrogen atmosphere, then 100mg polybutadiene in the state of gum was blended. A white paste was produced and the produced paste was coated on a polyester film. The film was heated at 60°C for 10 minutes with the pressure of 1 Torr so that fine pores could be formed. Then the film was cooled for curing. As a result, a white flexible desiccant film having the thickness of 2mm was produced.
EXAMPLE 2 Calcium oxide (CaO) was used as a desiccant substance, active carbon as a porous substance and hot melt of ethylenevinylacetate series as a polymer binder to produce the desiccant body.
After blending 70mg CaO powder and 50mg active carbon, in which moisture is removed by vacuum heating, in a glove box in a nitrogen atmosphere, then 100mg of the hot melt which was dissolved at
150°C was blended. A black paste was produced and the produced paste was coated on glass. The paste was heated at 150°C for 10 minutes with the pressure of 1 Torr so that fine pores could be formed and then cooled for curing. As a result, a black flexible desiccant film having the thickness of 0.2mm was produced. .
EXAMPLE 3
Barium oxide (BaO) was used as a desiccant substance, active carbon as a porous substance and UV cured resin of polyurethane series as a polymer binder to produce the desiccant body.
After blending 50mg BaO power and 50mg active carbon, in which moisture is removed by vacuum heating, in a glove box in a nitrogen atmosphere, then 100mg UV cured resin was blended. A black paste was produced and the produced paste was coated on a release liner with the thickness of 0.2 mm. The release liner was heated at 60°C for 10 minutes with the pressure of 1 Torr so that fine pores could be formed and then was cured by UV radiation for 10 seconds. As a result, a black flexible desiccant film having the thickness of 0.2mm was formed.
EXAMPLE 4
Phosphorous pentoxide was used as a desiccant substance, active carbon as a porous substance and polybutadiene having a mean molecular weight of 2,500,000 as a pplymer binder to produce the desiccant body.
After blending 50mg Hexane, 50mg phosphorous pentoxide and 50mg active carbon, in which moisture is removed by vacuum heating, in a glove box in a nitrogen atmosphere, then a solution of 100mg polybutadiene dissolved at 15wt% in hexane was blended. A black paste was produced and the produced paste was coated on polyester
film. The film was heated at 80°C for 30 minutes with the pressure of 1 Torr so that the film could be cured with fine pores being formed. As a result, a black flexible desiccant film having the thickness of 0.2mm was produced.
EXAMPLE 5
Lithium aluminum hydride (LiAIH4) was used as a desiccant substance, active carbon as a porous substance and polybutadiene having a mean molecular weight of 2,500,000 as a polymer binder to produce the desiccant body.
After blending 1 ,500mg tetrahydrofuran, 50mg lithium aluminum hydride powder, and 50mg active carbon, in which moisture is removed by vacuum heating, in a glove box in a nitrogen atmosphere, then by drying the mixture under vacuum, a mixture of active carbon coated with lithium aluminum hydride was produced. Then, a solution of 100mg polybutadiene dissolved at 15wt% in hexane was additionally blended. A black paste was produced and the produced paste was coated on a polyester film. The film was heated at 80°C for 30 minutes with the pressure of 1 Torr so that the film could be cured with fine pores being formed. As a result, a black flexible desiccant film having the thickness of 0.2mm was produced.
EXAMPLE 6
Lithium (Li) and aluminum (Al) were used as desiccant substances, active alumina as a porous substance and polybutadiene having a mean molecular weight of 2,500,000 as a polymer binder to produce the desiccant body.
After blending a solution in which 50mg lithium aluminum hydride
(LiAIH ) is dissolved in 500mg diethyl ether solution, and 50mg active alumina in which moisture is removed by vacuum heating, in a glove box
in a nitrogen atmosphere, the mixture was heated at 200°C for long hours. Then, lithium aluminum hydride was decomposed and hydrogen was removed, and lithium and aluminum metals were coated on the fine pores and surface of active alumina. By doing so, a mixture in which lithium and aluminum metals are coated on active alumina was produced. Then, a solution of 100 mg of fluorocarbon elastomer dissolved at 15wt% in tetrahydrofuran was additionally blended. A gray paste was produced and the produced paste was coated on polyester film. The film was heated at 80°C for 30 minutes with the pressure of 1 Torr so that the film could be cured with fine pores being formed. As a result, a black flexible desiccant film having the thickness of 0.2mm was produced.
COMPARISON EXAMPLE
The same desiccant substances and polymer binders as in the previous examples were used for production in the following comparison examples. The step for forming fine pores in the polymer binders was not used in the comparison examples 1 through 3, while the porous substances were not used in the comparison example 5.
COMPARISON EXAMPLE 1
Barium oxide (BaO) was used as a desiccant substance, silica gel as a porous substance and polybutadiene in the state of gum (viscosity = 40 to 90 poise at 45°C) as a polymer binder to produce the desiccant body. After blending 150mg BaO powder and 50mg silica gel in which moisture is removed by vacuum heating, in a glove box in a nitrogen atmosphere, 100mg polybutadiene in'the state of gum was blended. A white paste was produced and the produced paste was coated on a polyethylene film. The film was heated at 60°C for 10 minutes with the pressure of 1 Torr so that fine pores could be formed. Then, the film
was cooled for curing. As a result, a white flexible desiccant film was produced.
COMPARISON EXAMPLE 2 Calcium oxide (CaO) was used as a desiccant substance, active carbon as a porous substance and hot melt of ethylenevinylacetate series as a polymer binder to produce the desiccant body.
After blending 70mg CaO powder and 50mg active carbon in which moisture is removed by vacuum heating, in a glove box in a nitrogen atmosphere, then 100mg of the hot melt which was dissolved at 150°C was blended. A black paste was produced and the produced paste was coated on glass and then cooled for curing. As a result, a black flexible desiccant film having the thickness of 0.2mm was produced.
COMPARISON EXAMPLE 3
Barium oxide (BaO) was used as a desiccant substance, active carbon as a porous substance and UV cured resin of polyurethane series as a polymer binder to produce the desiccant body.
After blending 50mg BaO power and 50mg active carbon in which moisture is removed by vacuum heating, in a glove box in a nitrogen atmosphere, then 100mg UV cured resin was blended. A black paste was produced and the produced paste was coated on a release liner. Without the process of forming fine pores, the paste was cured by UV radiation for 10 seconds. As a result, a black flexible desiccant film having the thickness of 0.2mm was produced.
COMPARISON EXAMPLE 4
Phosphorous pentoxide was used as a desiccant substance, and polybutadiene having a mean molecular weight of 2,500,000 as a polymer binder to produce the desiccant body, but a porous substance
was not used.
In a glove box in a nitrogen atmosphere, 50mg phosphorous pentoxide powder and a solution of 100mg polybutadiene dissolved at 15 wt% in hexane were blended. A white paste was produced and the produced paste was coated on a polyethylene film. The film was heated at 80°C for 30 minutes with the pressure of 1 Torr and then cured. As a result, a white flexible desiccant film having the thickness of 0.2mm was produced.
COMPARISON EXAMPLE 5
Lithium aluminum hydride (LiAIH ) was used as a desiccant substance and polybutadiene having a mean molecular weight of 2,500,000 as a polymer binder to produce the desiccant body, but a porous substance was not used. In a glove box in a nitrogen atmosphere, 50mg lithium aluminum hydride powder and a solution of 100mg polybutadiene dissolved at 15wt% in hexane were blended. A white paste was produced and the produced paste was coated on a polyethylene film. The film was heated at 80°C for 30 minutes with the pressure of 1 Torr and then cured. As a result, a white flexible desiccant film having the thickness of 0.2mm was produced.
EXAMPLE 7
The desiccant bodies produced by the examples 1 through 6 and compaπson examples 1 through 5 had been placed in the air at a temperate of 25°C and a relative humidity of 50% for 30 minutes. Then, by measuring the increased weight of each desiccant body, the mean desiccation speed was measured. The results are shown in the following table 1. Table 1
The comparison example 5 shows a case in which because of not using a porous substance, even when heating or reduced pressure was applied after forming a film, there was no substance released through the polymer binders from the inside such that fine pores were not formed. The comparison samples 1 through 3 show the cases in which though a porous substance was used, the process of forming fine pores by applying heat or reduced pressure was not performed such that no fine pores were formed in polymer binders. The table 1 shows that when the desiccant bodies produced by the examples 1 through 5 were compared with those produced by the comparison examples 1 through 5, in which the same desiccant substances and polymer binders as in the examples 1 through 5 were used but the process of forming fine pores was not performed, the absorption speed of the desiccant bodies produced by the examples were ten times or more faster than that of the desiccant bodies produced by the comparison examples. The table also shows that, as in the example 2 and the comparison example 2, the desiccation speed
difference was widened when polymer binders having a low MVTR was applied.
Industrial Applicability According to the present invention, a flexible thin film-type desiccant body which has a high desiccation speed and can be conveniently attached and used, without releasing moisture and without generated fluid products damaging electronic circuit devices even when the temperature goes up, and a method of therefor are provided. Accordingly, enclosed electronic devices which are constructed as an enclosure type to avoid moisture, such as organic EL devices and CCD, can be used under appropriate conditions for a longer time.
Claims
1. A desiccant body for enclosed electronic devices comprising: a desiccant substance which removes moisture by reacting with moisture; a porous substance which with fine pores provides transfer passages for moisture, and contains gas or a volatile substance so that when the desiccant body is formed, fine pores can be formed in a polymer binder; and a polymer binder which gives a shape to a mixture of the desiccant substance and porous substance and in which, when the desiccant body is formed, fine pores are formed by releasing of the gas or volatile substance contained in the porous substance such that transfer passages for moisture are provided.
2. The desiccant body for enclosed electronic devices of claim 1 , wherein a desiccant substance is selected from alkaline metal oxides, alkaline earth metal oxides, sulfate, metal halides, perchlorates, phosphorus pentoxide, metal hydrides, and other metals with a higher ionization tendency than hydrogen and mixtures thereof.
3. The desiccant body for enclosed electronic devices of claim 1 , wherein a metal with a higher ionization tendency than hydrogen is selected from lithium (Li), potassium (K), sodium (Na), calcium (Ca), barium (Ba), aluminum (Al), and mixtures thereof.
4. The desiccant body for enclosed electronic devices of claim 1 , wherein the porous substance is a solid substance in the form of particles with a diameter equal to or less than 1mm, or a filamentous solid substance with a diameter equal to or less than 1mm, in which pores with an average diameter of 03nm~1 OOmicrons are formed.
5. The desiccant body for enclosed electronic devices of claim 1 , wherein the porous substance is selected from active carbon, silica gel, active alumina, zeolite, diatomaceous earth, porous resin, and porous fiber, or mixtures thereof.
6. The desiccant body for enclosed electronic devices of claim 1 , wherein the polymer binder is selected from gum-type polymers, multi- component series reaction curing polymers which are polymerized by a catalyst or heat, hot-melt polymers, radiation curing polymers which are cured by visible light, ultraviolet (UV), and electronic beam (EV), solvent evaporation curing polymers which are used after polymers are melt into a solvent, and mixtures thereof.
7. A method for producing a desiccant body for film-type enclosed electronic devices comprising: producing a mixture of a desiccant substance and a porous substance; blending the mixture of the desiccant substance and the porous substance with a polymer binder; forming a film; and forming fine pores in the polymer binder.
8. The method of claim 7, after the step for forming fine pores, further comprising: curing the polymer binder.
9. The method of any one of claims 7 and 8, wherein the step for producing a desiccant substance and a porous substance is performed by vapor deposition or sputtering of a desiccant substance on the porous substance.
10. The method of any one of claims 7 and 8, wherein the step for producing a desiccant substance and a porous substance is performed by using a small amount of a liquid substance such as a volatile liquid, a high boiling point liquid or a coupling body so that the desiccant substance is evenly dispersed on the surface or pores of the porous substance.
11. The method of any one of claims 7 and 8, wherein the step for forming fine pores in the polymer binder is performed by applying heat.
12. The method of any one of claims.7 and 8, wherein the step for forming fine pores in the polymer binder is performed by reducing pressure.
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KR10-2002-0078635A KR100500194B1 (en) | 2002-03-26 | 2002-12-11 | flexible film-type desiccant body for enclosed electronic devices and production method of the same |
KR10-2002-0078635 | 2002-12-11 |
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WO2006069781A2 (en) * | 2004-12-30 | 2006-07-06 | Grace Gmbh & Co. Kg | Flexible adsorbent bodies |
US8829634B2 (en) | 2009-03-23 | 2014-09-09 | Dow Global Technologies Llc | Optoelectronic device |
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DE3738285A1 (en) * | 1987-11-11 | 1989-05-24 | Bayer Ag | Mixtures containing phosphorus pentoxide and esters of acids of phosphorus, and use of these mixtures as desiccants |
US5591379A (en) * | 1990-07-06 | 1997-01-07 | Alpha Fry Limited | Moisture getting composition for hermetic microelectronic devices |
US6214255B1 (en) * | 1995-04-19 | 2001-04-10 | Capitol Specialty Plastics, Inc. | Desiccant entrained polymer |
US6226890B1 (en) * | 2000-04-07 | 2001-05-08 | Eastman Kodak Company | Desiccation of moisture-sensitive electronic devices |
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EP1652581A1 (en) * | 2004-10-21 | 2006-05-03 | E.I. Dupont De Nemours And Company | Curable thick film paste compositions for use in moisture control |
US7371335B2 (en) | 2004-10-21 | 2008-05-13 | E.I. Dupont De Nemours And Company | Curable thick film compositions for use in moisture control |
US7494604B2 (en) | 2004-10-21 | 2009-02-24 | E.I. Du Pont De Nemours And Company | Curable thick film paste compositions for use in moisture control |
WO2006069781A2 (en) * | 2004-12-30 | 2006-07-06 | Grace Gmbh & Co. Kg | Flexible adsorbent bodies |
WO2006069781A3 (en) * | 2004-12-30 | 2006-09-21 | Grace Gmbh & Co Kg | Flexible adsorbent bodies |
KR101318541B1 (en) * | 2004-12-30 | 2013-10-16 | 그라세 게엠베하 운트 캄파니 카게 | Flexible adsorbent bodies |
US8829634B2 (en) | 2009-03-23 | 2014-09-09 | Dow Global Technologies Llc | Optoelectronic device |
EP2438629A4 (en) * | 2009-06-01 | 2015-08-19 | Sumitomo Chemical Co | Formulations for improved electrodes for electronic devices |
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