Patent Grant
8367768
This application claims priority of U.K. Patent Application No. 0822911.4, filed on Dec. 16, 2008, the entirety of which is incorporated by reference herein.
1. Field of the Invention
The invention relates to an encapsulant composition, and more particularly to an encapsulant composition used for fabricating an encapsulant material with high light transmittance and a method for fabricating the encapsulant material which is suitable for use in packaging solid state light-emitting devices to improve light transmittance thereof.
2. Description of the Related Art
With development of the optical-electronic industry, optical-electronic devices, for example, organic light emitting diodes (OLED), light emitting diodes (LED) and solar cells have been developed. Optical-electronic elements in an optical-electronic device, however, are easily damaged by moisture and oxygen, resulting in a short operating lifespan. Therefore, using suitable materials to package optical-electronic devices are necessary to prevent such optical-electronic elements from moisture and oxygen, increasing operating lifespan.
Conventional encapsulant materials are synthesized by thermal processes. A resin monomer is first synthesized to form a resin, and fillers and hardeners are then added and mixed therewith to obtain an encapsulant material. However, the above thermal processes are time-consuming, normally taking a couple of hours or up to ten hours or more to complete resin synthesis. In addition, since the above thermal processes incorporate solvents, reaction conditions and process safety issues are a concern. Therefore, fabrication time and costs for fabricating encapsulant materials by the thermal processes are not easily reduced.
Thus, a novel method for fabricating encapsulant materials and encapsulant compositions for forming thereof are needed to fabricate encapsulant materials in a faster and safer method, decreasing fabrication time and costs, and improving safety issues during fabrication.
Accordingly, encapsulant compositions and methods for fabricating encapsulant materials having lower production costs, decreased fabrication safety issues and faster fabrication processes are provided.
An exemplary encapsulant composition comprises at least one silane-containing monomer and at least one resin monomer selected from the group consisting of acrylic resin monomers and epoxy resin monomers; a filler of 0.1-15 wt % of the encapsulant composition; and an initiator.
An exemplary method for fabricating encapsulant materials comprises providing an encapsulant composition comprising at least one silane-containing monomer and at least one resin monomer selected from the group consisting of acrylic resin monomers and epoxy resin monomers, a filler and an initiator, wherein the filler is 0.1-15 wt % of the encapsulant composition; and performing a heating process by a microwave source to polymerize the encapsulant composition.
In conventional heating processes, heat energy is transmitted by conduction and convection, for example, a solution in a container is heated by conduction of the heated container. In a microwave heating process, however, heat energy is transmitted by irradiation, for example, a reactant is directly heated by microwave irradiation, with an improved heating efficiency.
Compared to conventional heating processes, the microwave heating process reduces loss of heat energy and increases reaction rate (effective collision probability) by molecule dipole moment rotation under a variation of microwave field. Additionally, using organic solvent is not required therein.
A detailed description is given in the following embodiments with reference to the accompanying drawings.
The present invention can be more fully understood by reading the subsequent detailed description and examples with references made to the accompanying drawings, wherein:
The following description is of the best-contemplated mode of carrying out the invention. This description is made for the purpose of illustrating the general principles of the invention and should not be taken in a limiting sense. The scope of the invention is best determined by reference to the appended claims.
The encapsulant composition and the method for fabricating encapsulant materials of the invention have the advantages of having lower production costs, improved fabrication safety issues, and much faster fabrication processes than that provided by the prior art using thermal processes. The encapsulant materials of the invention also show high moisture resistance and gas blocking ability, thereby making them appropriate for application when packaging light emitting devices, such as light emitting diodes (LED).
In an embodiment, an encapsulant composition mainly comprises a resin monomer comprising at least one silane-containing monomer and at least one acrylic or epoxy resin monomer, a filler and an initiator. Ratios of such materials in the encapsulant composition may be adjusted to form transparent packaging materials having high light transparency. In the encapsulant composition, the resin component is about 100 parts by weight, and the filler and the initiator respectively is about 0.1-15 parts by weight and 0.1-1 part by weight based on the 100 parts by weight of the resin component. The filler is about 0.1-15 wt % of the encapsulant composition, preferably about 5-15 wt %.
In one embodiment, the encapsulant composition comprises a silane-containing monomer and at least one resin monomer such as an acrylic resin monomer, an epoxy resin monomer, and compositions thereof.
In another embodiment, an acrylic resin monomer may be present having a structure represented by a formula of:
wherein each of R1 and R2 is an alkyl group having 1 to 12 carbon atoms, a tert-butyl group, an ester group having 1 to 12 carbon atoms, an alkanol group having 1 to 12 carbon atoms or a cyclo-alkoxy group having 1 to 12 carbon atoms.
In one embodiment, an epoxy resin monomer may be present having a structure represented by a formula of:
wherein R1 is an alkyl group having 1 to 12 carbon atoms, a tert-butyl group, an ester group having 1 to 12 carbon atoms, an alkanol group having 1 to 12 carbon atoms or a cyclo-alkoxy group having 1 to 12 carbon atoms.
In one embodiment, the silane-containing monomer may comprise a structure represented by a formula of:
wherein R1′, R1″ and R1′″ are the same or different, and each of R1′, R1″, R1′″, R2 and R3 is an alkyl group having 1 to 12 carbon atoms, a tert-butyl group, an ester group having 1 to 12 carbon atoms, an alkanol group having 1 to 12 carbon atoms or a cyclo-alkoxy group having 1 to 12 carbon atoms.
In one embodiment, the filler may comprise metal oxide such as silicon oxide or silicon aluminum, metal halides such as zinc chloride, metal nitride such as aluminum nitride or other powders such as calcium carbonate.
In one embodiment, the initiator may comprise peroxides such as benzoyl peroxide, azo compounds such as azobisisobutyronitrile (AIBN), free radical initiators such as 1-hydroxy-cyclohexyl-phenyl-ketone, cationic initiators such as iodonium 4-methylphenyl and 4-(2-methylpropyl)phenyl]-hexafluorophosphate, or metallocene complexes such as bis(eta 5-2,4-cyclopentadien-1-yl)bis[2,6-difluoro-3-(1H-pyrrol-1-yl)phenyl]titanium.
In one embodiment, the encapsulant composition mainly comprises a plurality of acrylic monomers such as benzyl methacrylate (BZMA), methyl methacrylate (MAA), and 2-hydroxyl ethyl mathacrylate (2-HEMA), a filler such as silicon dioxide, and an initiator such as AIBN, thereby forming an acrylic copolymer. In this embodiment, the acrylic monomer is about 89 parts by weight, and the filler and the initiator respectively is 8-10 parts by weight and 1-3 parts by weight based on the 100 parts by weight of the acrylic monomer. The filler is about 1-40 wt % of the encapsulant composition, preferably about 10-20 wt %.
In another embodiment, the encapsulant composition mainly comprises a polyurethane (PU)-acrylics comonomer, a filler such as silicon dioxide, and an initiator such as azobisisobutyronitrile, thereby forming a PU-acrylics copolymer. In the encapsulant composition of this embodiment, the PU-acrylics comonomer is about 72 parts by weight, and the filler and the initiator respectively is 20-25 parts by weight and 2-5 parts by weight based on the 100 parts by weight of the PU-acrylics comonomer. The filler is about 1-40 wt % of the encapsulant composition, preferably about 10-20 wt %.
In yet another embodiment, the encapsulant composition mainly comprises a silicone-acrylics comonomer, a filler such as silicon dioxide, and an initiator such as AIBN, thereby forming a silicone-acrylics copolymer. In the encapsulant composition of this embodiment, the silicone-acrylics monomer is about 71 parts by weight, and the filler and the initiator respectively is about 20-25 parts by weight and 2-5parts by weight based on the 100 parts by weight of the silicone-acrylics comonomer. The filler is about 1-40 wt % of the encapsulant composition, preferably about 10-20 wt %.
In another embodiment, the encapsulant composition mainly comprises an epoxy monomer, a filler such as silicon dioxide, and an initiator such as 2-ethyl-4-methyl imidazole (EMID), thereby forming an epoxy polymer. In the encapsulant composition of this embodiment, the epoxy monomer is about 90 parts by weight, and the filler and the initiator respectively is 5-9 parts by weight and 1-5 parts by weight based on the 100 parts by weight of the epoxy monomer. The filler is about 1-30 wt % of the encapsulant composition, preferably about 5-15 wt %.
The encapsulant composition is polymerized with heating by a microwave source to form an encapsulant material. Heating time and power of the microwave source may be properly adjusted to prepare the encapsulant material with a viscosity of about 1-100,000 cps, preferably between 5,000-30,000 cps, and a light transparency exceeding 85%, suitable for use in packaging light emitting devices, such as organic light emitting diodes, light emitting diodes or solar cells.
The encapsulant composition of the invention provides the following advantages:
1. Light transparency of the encapsulant material is adjusted by adjusting content of the filler, thereby providing a transparent encapsulant material having a light transparency exceeding 85%, and sometimes even more than 90%.
2. The encapsulant material of the invention has a great adhesive strength of up to 2.1 kg/cm.
3. The encapsulant material of the invention shows better gas and moisture proof abilities than that of the encapsulant material of the prior art using thermal processes, improving device lifespan.
4. The encapsulant material of the invention can be applied in packaging optical-electronic devices such as light emitting diodes, organic light emitting diodes and solar cells and is an appropriate packaging industry material.
Moreover, in an embodiment, a method for fabricating an encapsulant material comprising providing the disclosed encapsulant composition and performing a heating process by a microwave source to polymerize the encapsulant composition is provided. The heating process is performed for about 1 to 200 minutes and may be performed under a power of about 1 to 20,000 watts.
In addition, since the encapsulant material may still have some flow properties after the heating process, the encapsulant material may be formed over an optical-electronic device by, for example, spin-coating, acting as a final packaging layer. In an embodiment, the method for fabricating the encapsulant material may further comprise an illumination process performed by a light source to solidify the encapsulant composition. The illumination process is performed for a time of about 1 to 200 minutes and under a power of about 1 to 20,000 watts.
The light source used in the illumination processes may be, for example an ultraviolet (UV) light source, a visible light source or an infrared (IR) light source and may be decided according to the type of the initiator used therein.
The method for fabricating encapsulant materials of the invention provides the following advantages:
1. There is no requirement to control reaction pressure and temperature during fabrication of the encapsulant material of the invention as all that is required is steady stirring thereof. Thus, fabricating method for forming the encapsulant material of the invention is simplified.
2. No solvent is required for forming the encapsulant material of the invention, thus improving fabrication safety.
3. The encapsulant material of the invention is synthesized during fabrication thereof and thus fabrication time and costs are reduced.
4. The filler in the encapsulant material of the invention shows great disparity and the moisture and gas proof ability thereof is improved, thereby improving operating lifespan of packaged devices using the encapsulant material of the invention.
5. Light transparency of the encapsulant material is adjusted by adjusting contents of the filler, thereby providing a transparent encapsulant material having a light transparency exceeding 90%.
6. The method for fabricating the encapsulant material of the invention is applied in packaging optical-electronic devices such as light emitting diodes, organic light emitting diodes and solar cells and is an appropriate packaging industry material.
In conventional heating processes, heat energy is transmitted by conduction and convection, for example, a solution in a container is heated by conduction of the heated container. In a microwave heating process, however, heat energy is transmitted by irradiation, for example, a reactant is directly heated by microwave irradiation, with an improved heating efficiency.
Compared to conventional heating processes, the microwave heating process reduces loss of heat energy and increases reaction rate (effective collision probability) by molecule dipole moment rotation under a variation of microwave field. Additionally, using organic solvent is not required therein.
The encapsulant composition, the method for fabricating the encapsulant materials, and the related measurement results of the examples and comparative examples are described in detail as below. Chemical vendors and formulas of the chemicals used in the following examples and comparative examples are provided in the following tables, wherein Table 1 shows information of resin monomers applied therein, Table 2 shows information of the initiators applied therein and Table 3 shows information of the optical-electronic materials applied therein.
The above monomers and comonomers have structures represented as follows:
The above initiators have structures represented as follows:
The above optical-electronic materials have structures represented as follows:
117 g benzyl methacrylate (BZMA), 86 g methyl methacrylate (MAA), 130 g 2-hydroxyl ethyl mathacrylate (2-HEMA), 39 g silica and 6 g initiator AIBN were mixed in a container. The above materials were then stirred by a mechanic agitator at a normal pressure and normal temperature such that an encapsulant composition was obtained. Next, a heating process was performed to polymerize the obtained encapsulant composition by a microwave source (about 800 W) for 10 minutes. Then turned off the microwave oven and added I-184 (6 g). After mechanically stirred for 30 min, acrylics copolymer I was obtained. The acrylic copolymer I was fabricated by synthesizing the encapsulant composition according to the following Formula (1):
Physical properties such as viscosity, molecular weight, adhesive strength, hardness, light transparency and reflective index of acrylic copolymer I were tested and results thereof are shown in Tables 5 and 6. Tests performed on the acrylic polymer I are described in Table 4, and measurements of adhesive strength, hardness, light transparency and reflective index were achieved by testing a substrate sample of 5 square centimeters coated over a substrate such as a glass substrate by the measuring instruments and measuring method described in Table 4. The substrate sample was previously cured by a DUV light illumination source for 3 minutes before tests were completed.
333 g PU-acrylics comonomer a, 39 g silica and 6 g initiator AIBN were mixed in a container. The above materials were then stirred by a mechanic agitator at a normal pressure and normal temperature such that an encapsulant composition was obtained. Next, a heating process was in-situ performed to polymerize the obtained encapsulant composition by a microwave source (about 800 W) for 10 minutes. Then turned off the microwave oven and added I-184 (6 g) and I-369 (4 g). After mechanically stirred for 30 min, PU-Acrylics I polymer were obtained. The PU-Acrylics I polymer was fabricated by synthesizing the encapsulant composition according to the following Formula (2):
Physical properties of PU-acrylics polymer I of Example 2 were examined according to similar methods as described in Example 1 and results are shown in Tables 5 and 6.
333 g PU-acrylics comonomer b, 39 g silicon oxide and 6 g initiator AIBN were mixed in a container. The above materials were then stirred by a mechanic agitator at a normal pressure and normal temperature such that an encapsulant composition was obtained. Next, a heating process was in-situ performed to polymerize the obtained encapsulant composition by a microwave source (about 800 W) for 10 minutes. Then turned off the microwave oven and added I-184 (6 g) and I-369 (4 g). After mechanically stirred for 30 min, PU-Acrylics II polymer was obtained. The PU-Acrylics II polymer was fabricated by synthesizing the encapsulant composition according to the following Formula (3):
Physical properties of PU-acrylics polymer II of Example 3 were examined according to similar methods as described in Example 1 and results are shown in Tables 5 and 6.
333 g PU-acrylics comonomer c, 39 g silicon oxide and 6 g initiator AIBN were mixed in a container. The above materials were then stirred by a mechanic agitator at a normal pressure and normal temperature such that an encapsulant composition was obtained. Next, a heating process was in-situ performed to polymerize the obtained encapsulant composition by a microwave source (about 800 W) for 10 minutes. Then turned off the microwave oven and added I-184 (6 g) and I-369 (4 g). After mechanically stirred for 30 min, PU-Acrylics III polymer was obtained. The PU-Acrylics III polymer was fabricated by synthesizing the encapsulant composition according to the following Formula (4):
Physical properties of PU-acrylics polymer III of Example 4 were examined according to similar methods as described in Example 1 and results are shown in Tables 5 and 6.
333 g silicone monomer a, 39 g silicon oxide and 6 g initiator AIBN were mixed in a container. The above materials were then stirred by a mechanic agitator at a normal pressure and normal temperature such that an encapsulant composition was obtained. Next, a heating process was in-situ performed to polymerize the obtained encapsulant composition by a microwave source (about 800 W) for 10 minutes. Then turned off the microwave oven and added I-184 (3 g), I-369 (1.5 g) and I-ITX (1.5 g). After mechanically stirred for 30 min, silicone-acrylics polymer I was obtained. The silicone-acrylics polymer I was fabricated by synthesizing the encapsulant composition according to the following Formula (5):
Physical properties of silicone-acrylics polymer I of Example 5 were measured according to similar methods as described in Example 1 and measuring results are shown in Tables 5 and 6.
166.5 g silicone monomer a, 166.5 g 2-HEMA, 39 g silicon oxide and 6 g initiator AIBN were mixed in a container. The above materials were then stirred by a mechanic agitator at a normal pressure and normal temperature such that an encapsulant composition was obtained. Next, a heating process was in-situ performed to polymerize the obtained encapsulant composition by a microwave source (about 800 W) for 10 minutes. Then turned off the microwave oven and added I-184 (3 g), I-369 (1.5 g) and I-ITX (1.5 g). After mechanically stirred for 30 min, silicone-acrylics copolymer II was obtained. The silicone-acrylics copolymer II was fabricated by synthesizing the encapsulant composition according to the following Formula (6):
Physical properties of silicone-acrylics copolymer II of Example 6 were measured according to similar methods as described in Example 1 and measuring results are shown in Tables 5 and 6.
166.5 g silicone monomer a, 166.5 g PU-acrylics comonomer b, 39 g silicon oxide and 6 g initiator AIBN were mixed in a container. The above materials were then stirred by a mechanic agitator at a normal pressure and normal temperature such that an encapsulant composition was obtained. Next, a heating process was in-situ performed to illuminate the obtained encapsulant composition by a microwave source (about 800 W) for 10 minutes. Then turned off the microwave oven and added I-184 (2.7 g), I-369 (1.35 g), I-ITX (1.35 g) and I-127 (0.6 g). After mechanically stirred for 30 min, silicone-PU-acrylics copolymer I was obtained. The silicone-PU-acrylics copolymer I was fabricated by synthesizing the encapsulant composition according to the following Formula (7):
Physical properties of silicone-PU-acrylics copolymer I of Example 7 were measured according to similar methods as described in Example 1 and measuring results are shown in Tables 5 and 6.
333 g epoxy monomer a, 39 g silicon oxide and 6 g initiator 2-ethyl-4-methyl imidazole were mixed in a container. The above materials were then stirred by a mechanic agitator at a normal pressure and normal temperature such that an encapsulant composition was obtained. Next, a heating process was in-situ performed to polymerize the obtained encapsulant composition by a microwave source (about 800 W) for 10 minutes. Then turned off the microwave oven and added I-250 (6 g). After mechanically stirred for 30 min, epoxy polymer I was obtained. The epoxy polymer I was fabricated by synthesizing the encapsulant composition according to the following Formula (8):
Physical properties of epoxy polymer I of Example 8 were measured according to similar methods as described in Example 1 and measuring results are shown in Tables 5 and 6.
117 g benzyl methacrylate (BZMA), 86 g methyl Methacrylate (MAA), 130 g 2-hydroxyl ethyl mathacrylate (2-HEMA), 39 g silicon dioxide, 6 g initiator AIBN and 300 g propylene glycol monomethyl ether acetate (PGMEA), as a solvent, were mixed in a container. The above material was then stirred by a mechanic agitator at a normal pressure and normal temperature and was then heated up to 90° C. and maintained at this temperature for 6 hours. Then turned off the heater and added I-184 (6 g). After mechanically stirred for 30 min, acrylics copolymer I was obtained. Herein, the acrylic copolymer I was obtained by synthesizing the encapsulant composition according to the following Formula (9):
Physical properties of the acrylic polymer I of Comparative Example 1 were measured according to similar methods as described in Example 1 and results are shown in Tables 5 and 6.
Referring to
The fabrication steps in Example 9 are repeated and the glass substrate 100 was replaced by a polyethylene terephthalate (PET) substrate 200, thereby forming a packaged flexible OLED device. Herein, as shown in
Referring to
An ITO glass 400 was provided and immersed in a cleaning solution including acetone, methanol and DI water. The ITO glass 400 was cleaned by a supersonic cleaner for 5 minutes and then treated by an O2 plasma for 90 seconds. An electron transport layer 402 (PEDOT) and an active layer 404 (P3HT/PCBM of a weight ratio of 1:1), were sequentially formed over the ITO glass 400 by, for example, spin coating. Coating conditions thereof were stage I 1,500 rpm for 20 second and stage II 3,500 rpm for 30 seconds for forming the hole transport layer 402, and stage I 1,000 rpm for 20 second and stage II 2,000 rpm for 30 seconds for forming the active layer 404. An electron injecting layer 406 (LiF) and a cathode 408 (Al) were sequentially formed over the active layer 404 by, for example, by an evaporation method. The silicone-PU-acrylics copolymer obtained in Example 7 was then coated over the cathode 408 and encapsulate thereof (coating condition: stage I 1,500 rpm for 20 second, and stage II 3,500 rpm for 30 seconds). The encapsulant material was then cured by illumination of ultraviolet light for 10 seconds and thereby formed an encapsulant layer 470 on the top and sidewall surfaces, thus forming a packaged solar cell. Herein, the solar cell received light 480 passing through the ITO glass 400. After 48 hours, compared to a conventional solar cell (having a decay ratio of 55%) packaged by an encapsulant material prepared using thermal processes, the solar cell packaged by an encapsulant material prepared using microwave processes had a lesser decay ratio of 14%, with an improved lifespan.
While the invention has been described by way of example and in terms of the preferred embodiments, it is to be understood that the invention is not limited to the disclosed embodiments. To the contrary, it is intended to cover various modifications and similar arrangements (as would be apparent to those skilled in the art). Therefore, the scope of the appended claims should be accorded the broadest interpretation so as to encompass all such modifications and similar arrangements.
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