JP6927910B2 - Sealing adhesive composition, sealing member and electronic member - Google Patents

Description

The present invention relates to a sealing adhesive composition, a sealing member and an electronic member.

In recent years, light emitting diodes such as deep ultraviolet LEDs (Light Emitting Diodes); high frequency devices such as crystal oscillators, SAWs (Surface Acoustic Wave), and low noise amplifiers; power devices; seals for acceleration sensors, etc. Stopping technology is attracting attention, and technological development is being repeated. For example, as a sealing of a deep ultraviolet LED, a so-called airtight sealing (hollow PKG) structure is adopted in which a glass lid material and a concave hollow ceramic package (PKG) are hermetically sealed with a sealing agent.

Quartz glass having a high transmittance of wavelengths in the deep ultraviolet region is used as the lid material, and aluminum nitride having high thermal conductivity is often used as the ceramic which is PKG. As a sealant for sealing PKG, there is an inorganic sealant such as gold-tin eutectic solder, which has excellent low moisture permeability, but is caused by the difference in the coefficient of thermal expansion between quartz glass and aluminum nitride. Since the lid material may be peeled off or cracked after the PKG is sealed, complicated know-how is required for blending the inorganic sealing agent and the sealing method. On the other hand, unlike the inorganic encapsulant, the organic encapsulant made of a resin as in Patent Document 1 is advantageous in that the lid material is less likely to be peeled off or cracked due to the difference in thermal expansion. Further, the encapsulant of Patent Document 1 has improved high barrier property against water vapor by containing a hygroscopic agent.

Japanese Patent Application Laid-Open No. 2005-516369

However, in Patent Document 1, only containing a hygroscopic agent, sufficient barrier properties cannot be achieved, and it may be difficult to meet even higher demands. In view of this problem, what the present invention should solve is to provide a resin composition for sealing having better low moisture permeability.

The present inventors have studied diligently and have come to find the following inventions. The present invention includes the following forms.
<1> A sealing adhesive composition containing a resin, a layered inorganic substance, and a hygroscopic agent.
<2> The sealing adhesive composition according to <1>, which contains 0.5 to 15% by volume of the layered inorganic substance.
<3> The sealing adhesive composition according to <1> or <2>, wherein the average area of the layered inorganic substance is 1 to 100 μm ^2.
<4> The sealing adhesive composition according to any one of <1> to <3>, which contains 0.5 to 20% by weight of the hygroscopic agent.
<5> The sealing adhesive composition according to <4>, wherein the average particle size of the hygroscopic agent is 1 nm to 10 μm.
<6> A sealing member, wherein the sealing adhesive according to any one of <1> to <5> is applied to a translucent lid material.
<7> An electronic member in which a sealed component is housed in a package having an opening.
An electronic member characterized in that the opening is sealed by the sealing composition according to any one of <1> to <5>.

The sealing adhesive composition of the present invention contains a resin, a layered inorganic substance and a hygroscopic agent, and the presence of the hygroscopic agent between the layered inorganic substances complicates the passage path of water by the layered inorganic substances. In addition, low moisture permeability can be achieved by the synergistic effect of moisture supplementation by the hygroscopic agent.

It is sectional drawing which shows the adhesive composition for sealing which concerns on this invention. It is sectional drawing which shows the light emitting diode which concerns on embodiment of this invention.

The sealing adhesive composition of the present invention (hereinafter, “adhesive composition” is abbreviated as appropriate), the sealing member and the electronic member will be described in the present embodiment, but the description unreasonably limits the present invention. It's not something to do. The adhesive composition of the present invention contains a resin, a layered inorganic substance, and a hygroscopic agent. The adhesive composition can be cured and can be preferably used for sealing applications such as light emitting diode packages.

〔resin〕
The resin contained in the adhesive composition of the present invention is the basis of the adhesive composition, and includes a so-called main agent, which is a polymer serving as a resin skeleton, and a curing agent that crosslinks the main agents. Further, a curing accelerator and the like are also contained in the resin.

The main agent is not particularly limited as long as it does not cause a problem in sealing the light emitting diode or the like. As an example, epoxy resin, urea resin, melamine resin, benzoguanamine resin, acetoguanamine resin, phenol resin, resorcinol resin, xylene resin, furan resin, unsaturated polyester resin, diallyl phthalate resin, isocyanato resin, epoxy resin, maleimide resin, Examples include nadiimide resin and the like. These main agents may be used alone or in combination of two or more. The adhesive composition of the present invention has a basic structure of a resin such as a main agent, and is more flexible than an inorganic encapsulant, and is less likely to peel off or crack.

[Curing agent]
The curing agent is a component that cures the main agent, and the curing agent includes amine compounds such as diaminodiphenylmethane, diaminodiphenylsulfide, diaminobenzophenone, diaminodiphenylsulfone, and diethyltriamine, 2-alkyl-4-methylimidazole, and 2-phenyl. Examples thereof include imidazole derivatives such as -4-alkylimidazole, organic acids such as phthalic anhydride and trimellitic anhydride, boron trifluoride amine complex such as boron trifluoride triethylamine complex, and dicyandiamide, which may be used alone or 2 You may mix and use more than seeds.

Further, a phenol resin such as a resol type or novolak type phenol resin may be used as the curing agent. The phenol resin includes, for example, alkyl-substituted phenols such as phenol, cresol and pt-butylphenol, cyclic alkyl-modified phenols such as terpene and dicyclopentadiene, and heteroatoms such as nitro group, halogen group, amino group and cyano group. Examples thereof include those having a functional group and those having a skeleton such as naphthalene and anthracene.

[Stress relaxation agent]
The stress relaxation agent imparts stress relaxation property to the resin, and is optionally contained in the resin. As stress relaxation properties, polyolefin resins such as polyethylene and polypropylene and their modifications, polyester resins such as polyethylene terephthalate and polybutylene terephthalate, (meth) acrylic resins such as polymethylmethacrylate and polyethylmethacrylate, polystyrene, and acrylonitrile-butadiene- Styrene resin, acrylonitrile-acrylic rubber-styrene resin, acrylonitrile-ethylene rubber-styrene resin, (meth) acrylic acid ester-styrene resin, styrene resin such as styrene-butadiene-styrene resin, ionomer resin, polyacrylic nitrile, 6-nylon , 6,6-nylon, 6T-PA, 9T-PA, MXD6-nylon and other polyamide resins, ethylene-vinyl acetate resin, ethylene-acrylic acid resin, ethylene-ethyl acrylate resin, ethylene-vinyl alcohol resin, polyvinyl chloride Chlorine resin such as or polyvinylidene chloride, fluororesin such as polyvinyl fluoride and vinylidene fluoride, polycarbonate resin, modified polyphenylene ether resin, methylpentene resin, cellulose resin, etc., as well as olefin-based elastomer, glycidyl-modified olefin-based elastomer, maleic acid. Thermoplastic elastomers such as modified olefin-based elastomers, vinyl chloride-based elastomers, styrene-based elastomers, urethane-based elastomers, polyester-based elastomers, polyamide-based elastomers, polyphenylene sulfide resins, polyetherimide resins, polyether ether ketone resins, thermoplastic polyimide resins , Diene rubber and its hydrogenated products [for example, natural rubber, isoprene rubber, epoxidized natural rubber, styrene butadiene rubber, butadiene rubber, nitrile rubber, hydrogenated NBR, hydrogenated SBR], olefin rubber [for example, ethylene propylene Rubber, maleic acid-modified ethylene propylene rubber, butyl rubber, isobutylene and aromatic vinyl or diene monomer copolymer, acrylic rubber, ionomer], halogen-containing rubber [for example, Br-IIR, CI-IIR, brominated isobutylene-p- Methylstyrene copolymer, chloroprene rubber, hydrin rubber, chlorosulfonated polyethylene rubber, chlorinated polyethylene rubber, maleic acid-modified chlorinated polyethylene rubber], silicone rubber [for example, methylvinyl silicone rubber, dimethylsilicone rubber, methylphenylvinyl sis Licorn rubber], sulfur-containing rubber [for example, polysulfide rubber], fluororubber [for example, vinylidene fluoride rubber, fluorovinyl ether rubber, tetrafluoroethylene-propylene rubber, fluorosilicone rubber, fluorophosphazene rubber], etc. Etc. are exemplified. Further, the resin of the present invention may contain various organic substances such as a curing reaction accelerator and an adhesive-imparting agent for layered inorganic substances as long as the purpose of the adhesive composition of the present invention is not impaired.

The content of the resin in the adhesive composition may be appropriately changed according to the type thereof, but in the adhesive composition, it is, for example, 60 to 90% by weight, more preferably 70 to 90% by weight.

[Layered inorganic substances]
The layered inorganic substance has moisture resistance against moisture such as vapor, suppresses the passage of moisture, and contributes to low moisture permeability. Specific examples of the layered inorganic substance include graphene, smectite, montmorillonite, sericite, mica, and pearl mica. Further, the layered inorganic substance more preferably has an ultraviolet blocking effect, whereby deterioration of the resin due to ultraviolet rays can be suppressed.

It is preferable that the average thickness of the layered inorganic substance is thin and the average area is large in order to make the passage of moisture in the adhesive composition a long distance. The average thickness or average area of the layered inorganic substance indicates the arithmetic mean of the thickness or area when the cross section of the resin composition is observed by SEM, and may be calculated from the average value of 100 layered inorganic substances. An optical microscope or the like can be used.

The average thickness of the layered inorganic substance is preferably 0.33 nm or more and 500 nm or less, more preferably 1 nm or more and 300 nm or less. The average area of the layered inorganic material ^{is preferably 1 μm 2} or more and 100 μm ² or less.

In the adhesive composition, the higher the volume ratio occupied by the layered inorganic substance, the more difficult it is for water to permeate. However, considering that the viscosity of the adhesive composition is within a suitable range, the volume filling rate of the layered inorganic substance is preferably 0. It is 5 to 15% by volume, more preferably 1 to 15% by volume, further preferably 3 to 12% by volume, and particularly preferably 5 to 10% by volume. In the case of graphene, the above range is expressed in% by weight, preferably 1 to 41% by weight, more preferably 2 to 41% by weight, still more preferably 6 to 32% by weight, and particularly preferably 11 to 26% by weight. be.

[Hygroscopic agent]
The adhesive composition of the present invention contains a hygroscopic agent. As a result, the moisture contained in the adhesive composition is captured by the hygroscopic agent, and the adhesive composition having excellent low moisture permeability can be provided in addition to the moisture proof property of the layered inorganic substance. The smaller the size of the hygroscopic agent, the more likely it is to exist between the layered inorganic substances, and a synergistic effect with the layered inorganic substances can be obtained more. The average particle size of the hygroscopic agent is, for example, 1 nm to 10 μm, and is calculated from the average value of 100 particle sizes measured by observation with an optical microscope or the like.

The hygroscopic agent may be an organic substance or an inorganic substance as long as it has a water absorbing action. As the water absorbing agent, a known substance may be used, and examples thereof include clay minerals, zeolites, silica gels, mesoporous silicas, and polymer absorbents, which are not particularly limited.

The content of the hygroscopic agent in the adhesive composition may be appropriately set in consideration of the coatability of the adhesive composition and the like. A large content of the hygroscopic agent is desirable because the hygroscopic effect is enhanced, and a small content of the hygroscopic agent improves the coatability of the uncured adhesive composition. The content of the hygroscopic agent in the adhesive composition is appropriately set in consideration of the type of the hygroscopic agent and the balance between the hygroscopic effect and the coatability (viscosity). It is preferably 2 to 15% by weight, more preferably 5 to 10% by weight.

In addition, the adhesive composition contains both a layered inorganic substance and a hygroscopic agent, and when the total content of these is increased when preparing the adhesive composition, the viscosity tends to increase significantly. Therefore, it is very preferable that not only the content of the hygroscopic agent but also the volume% of the layered inorganic substance is in a preferable range.

[UV absorber, UV blocker]
UV absorbers and UV blockers are useful for suppressing deterioration of the binder resin by UV rays, discoloration due to deterioration of the cured resin, and adhesive strength between the curing hardener and the sealing material (package, etc.). The decrease is suppressed. Therefore, when the adhesive composition has an ultraviolet shielding effect, the ultraviolet resistance is further enhanced.

Examples of the ultraviolet absorber include carbon, hydroxyphenyltriazine, benzotriazole, cyanoacrylate, dihydroxybenzophenone and the like, and may be used alone or in combination of two or more in consideration of the absorption wavelength. Further, an ultraviolet absorber and a hindered amine-based light stabilizer may be combined. Examples of the ultraviolet blocking agent include titanium oxide, zinc oxide, titanium oxide and the like, and it is preferable that the surface of these agents is treated with a hydrophobic treatment or an inert treatment.

The particle size of the ultraviolet absorber and the ultraviolet blocking agent is preferably 10 μm or less, more preferably 5 μm or less, because if it is too large, it may interfere with sealing by the adhesive composition.

[Identification method]
Identification of the resin, layered inorganic substance, hygroscopic agent and the like contained in the adhesive composition can be performed by collecting from the adhesive composition and using known measuring methods such as IR, X-ray diffraction and mass spectrometry.

[Physical characteristics of adhesive composition]
The lower the moisture permeability of the adhesive composition, the more preferable it is. If the object, the moisture permeability is preferably from ^{2.0g / (m 2 · 24h)} , and more preferably 1.0g / (m ² · 24h) or less.

Further, it is desirable that the adhesive composition does not easily turn yellow when exposed to ultraviolet rays. When the adhesive composition turns yellow, the adhesive strength decreases. Therefore, the degree of yellowing is preferably 100 or less, and more preferably 50 or less. When the yellowing exceeds 100, particularly 120 or more, the adhesive strength is reduced to less than half of the initial strength, and the appearance quality is also reduced.

[Preparation of adhesive composition]
The adhesive composition is prepared by mixing or kneading the above raw materials. The mixing (kneading) means may be appropriately changed so that the mixture becomes uniform according to the viscosity of the mixture of the raw materials, and examples thereof include a roll mill, a rotating / revolving mixer, a homogenizer, an ultrasonic homogenizer, a ball mill, and a kneader. Be done.

Since the uncured adhesive composition is applied to the object to be sealed or the lid material for sealing before sealing, it is preferable that the viscosity is within a predetermined range. If the viscosity is too low, the adhesive composition Since it has high fluidity, it is difficult to apply it in a predetermined range, and if the viscosity is too high, the fluidity is low and it is difficult to apply it. The viscosity of the adhesive composition preferably at 25 ° C. is 100,000 to 800,000 mPa · s, more preferably 200,000 to 500,000 mPa · s.

The adhesive composition of the present invention is applicable as long as it contains a predetermined raw material, and the degree of curing does not matter. That is, (1) a state in which undried curing has not progressed, (2) a state in which drying is insufficient and curing is incomplete (semi-cured), and (3) sufficiently dried to form a cured product. Regardless of the state, it corresponds to the adhesive composition.

FIG. 1 is a cross-sectional view showing the adhesive composition 10, showing a state in which the adhesive composition is applied to a thin layer. For the sake of simplicity, only the resin 1, the layered inorganic substance 2 and the hygroscopic agent 3 in the cross section of the adhesive composition 10 are shown. In the adhesive composition 10, the resin 1 is used as a base, and the layered inorganic substance 2 and the hygroscopic agent 3 are included therein.

Due to the presence of the plurality of layered inorganic substances 2 in the adhesive composition 10, the moisture that has penetrated from one surface of the adhesive composition 10 can reach the other surface of the adhesive composition 10 at the shortest distance due to the presence of the layered inorganic substances 2. Unreachable. As shown in Path A, the water is forced to move at least along the surface of the layered inorganic material 2. Further, since the moisture is adsorbed by the hygroscopic agent 3, it is very difficult for the moisture to pass through the adhesive composition 10. Due to this structure, the adhesive composition 10 of the present invention has extremely excellent low moisture permeability. Further, as the curing of the adhesive composition 10 progresses, it becomes difficult for water to penetrate into the adhesive composition 10, and the moisture permeability becomes lower, which is preferable.

[Sealing method]
The coating and curing conditions of the adhesive composition in sealing are not particularly limited, and may be appropriately changed according to the characteristics such as the object to be sealed, the viscosity of the adhesive composition, and the curing temperature. The object to be sealed may have an opening, and the opening is required to be sealed with high airtightness. Examples thereof include light emitting diodes such as deep ultraviolet LEDs (Light Emitting Diodes), crystal oscillators, high frequency devices such as SAWs (Surface Acoustic Waves), surface acoustic waves, and low noise amplifiers, power devices, and acceleration sensors.

When a translucent lid material for sealing the object to be sealed is used, the adhesive composition may be applied to the object to be sealed, may be applied to the lid material, or both may be applied. You can apply it. The translucency indicates a function of transmitting light, and is not particularly limited as long as it does not interfere with the function of the object to be sealed. Examples of the material of the lid material include quartz glass, borosilicate glass, sapphire glass and other translucent glass, and ceramics. The means for applying the adhesive composition to the object to be sealed or the lid material is not particularly limited, and a known method can be used, for example, a dispenser, screen printing, pad printing, or the like may be used.

[Seal member]
The sealing member of the present invention is a lid material coated with an adhesive composition, and the adhesive composition is brought into close contact with the sealing object and then cured to form the sealing object. Seal. For example, a translucent lid material can be mentioned as the lid material, and a sealing member obtained by applying an adhesive composition to the lid material. It can be suitably used for sealing packages in light emitting diodes.

[Providing form of adhesive composition]
The adhesive composition of the present invention may be provided in a state of being contained in a container, or may be provided in a state of being applied to a base film such as a polymer film. Further, a state in which a protective film is attached to the adhesive composition side applied to the lid material may be used as a sealing member and may be provided. The resin composition of the above-mentioned form may be in an uncured, semi-cured or cured state.

[Electronic member]
The electronic member of the present invention is an electronic member in which a component to be sealed is housed in a package having an opening, and the opening is sealed by the sealing composition. Electronic components include light emitting diodes such as deep ultraviolet LEDs (Light Emitting Diodes); high frequency devices such as crystal oscillators, SAWs (Surface Acoustic Wave), and low noise amplifiers; power devices; acceleration sensors, etc. Can be mentioned. Examples of the sealed component include an LED chip, an acceleration sensor, a magnetoresistive element such as a tunnel magnetoresistive element (TMR element), and the like. Examples of the material of the package include known members such as ceramics, which may be appropriately changed according to the characteristics of the electronic member.

FIG. 2 is a cross-sectional view showing a state in which the light emitting diode 20 is sealed with the adhesive composition 10 as an example of the electronic member. As shown in the figure, in the light emitting diode 20, the LED chip (light emitting element) 5 is housed in the package 4, and the opening 6 of the ceramic package 4 is an adhesive applied to the translucent lid material 7. It is sealed with the composition 10. Examples of the LED chip include LED chips of various colors, and a deep ultraviolet LED chip is also included.

As an example of the procedure for sealing the light emitting diode 20, a transparent lid material 7 such as quartz glass coated with the adhesive composition 10 in a heated state at 60 to 80 ° C. after mounting the LED chip 5 on the package 4. Is picked up with a chip mounter, chip bonder, etc., and temporarily attached while aligning. After temporary attachment, it may be sealed by heat-pressing at 150 to 160 ° C. for 1 hour with a high-temperature press that can pressurize while heating. If there is no high-temperature press device, a constant pressure clip that can be pressurized with a spring or the like may be used to clip the package 4 and the transparent lid material 7, and heat-bonded in an oven at 150 to 160 ° C. for 1 hour to seal. ..

Hereinafter, the present invention will be described in more detail based on Examples, but the present invention is not limited to these Examples. Each evaluation of the confirmation powders obtained in Examples and Comparative Examples was performed as follows.

<Viscosity of mixture>
The viscosity of the adhesive composition is measured using a cone-plate type rotational viscometer (E-type viscometer manufactured by Toki Sangyo Co., Ltd.) according to the JIS Z8803 liquid viscosity measurement method.
The test conditions were a test temperature of 25 ° C. and a shear rate of 1.0 s ^-1 (cone rotor: 3.0 ° x R14 mm, rotation speed 0.5 rpm).

<Humidity permeability>
The instruments used in the measurement of moisture permeability are as follows.
・ Moisture permeable cup jig Manufacturer: Made by Tester Sangyo Co., Ltd. Model number: PA-201, cup transmission dimension φ60mm (transmission area 28.26cm2)
・ Constant temperature and humidity device Manufacturer: ESPEC CO., LTD. Model number: Small environmental tester SH-241
・ Weighing scale Manufacturer: Sartorius Japan Model number: BP210D

The measurement sample is prepared by the following procedure. First, about 4 to 5 g of uncured liquid resin (adhesive composition) is placed on a release PET film, another release PET film is placed on the liquid resin, and a spacer with a thickness of 300 μm is placed between the PET films. It is pressed while sandwiched to adjust the thickness of the liquid resin to 300 μm, and then cured to form a sheet.
Cut the sheet to φ70 mm, put a petri dish containing calcium chloride in a moisture permeable cup, cover it with a sample, and seal it with a wax sealant.
The moisture permeability of the above sample is measured according to the JIS Z0280 moisture permeability test method for moisture-proof materials.
Temperature / humidity test conditions: Temperature 40 ± 0.5 ° C, Relative humidity 90 ± 2%, Test time: 24 hours After putting the above sample in the environmental test device for 16 hours or more, measure the test start weight and return it to the environmental test device again. After 24 hours, measure the mass of the cup and calculate the moisture permeability from the following formula.

Considering deep ultraviolet light emitting diode, moisture ^{permeability, 2.0g / (m 2 · 24h} ) good if less, it is determined that the better the 1.0g / (m ² · 24h) or less.

<Yellowness>
The instruments used to measure the degree of yellowing are as follows.
・ Ultraviolet irradiation machine Manufacturer: Ushio, Inc. Model number: SP7 250DB (with direct irradiation optical unit installed)
・ Lamp manufacturer: Ushio, Inc. Model number: Deep UV lamp UXM-Q256BY
・ Integrated photometer (illuminance meter)
Manufacturer: Ushio, Inc. Body model number UIT-250
Light receiving sensor Model number: UVD-S254
・ Sample image shooting Manufacturer: KEYENCE Co., Ltd. Model number: Digital microscope VHX-5000
-Color information collection software Manufacturer: Free software Model number: Power dropper Ver. 2.2

Apply 0.0020 to 0.0030 g of uncured liquid resin to a 5 mm x 5 mm x 0.5 tmm quartz glass chip (cover material), and semi-cure at 65 ° C for 24 hours. The semi-cured product is adhered to an alumina substrate having an aluminum oxide purity of 96%, and heated and pressurized at 150 to 160 ° C. for 1 hour to be fully cured.

・ Ultraviolet irradiation test conditions Illuminance: 1000mW / cm ² @ wavelength 254nm
Irradiation time: 20 hours
(= Integrated light intensity 72,000 J / cm ² )
Under the above-mentioned ultraviolet irradiation conditions, images of the sample before and after the ultraviolet irradiation test are taken, and RGB values are collected from the images using a power dropper. Further, the RGB color system is converted to the XYZ color system, the yellowness is simply calculated, and the yellowing degree is calculated. When the adhesive composition turns yellow, the adhesive strength decreases. Therefore, the degree of yellowing is preferably 100 or less, more preferably 50 or less. When the yellowing is 120 or more, the adhesive strength is reduced to less than half of the initial strength, and the appearance quality is also reduced.

<Raw materials>
The raw materials in Table 1 used in Examples and Comparative Examples are as follows.
Epoxy resin: Bisphenol A type epoxy resin Amine-based curing agent: Diaminodiphenylmethane-based curing agent Imidazole: 2,4-diamino-6- [2'methylimidazolyl- (1')]-ethyl-s-triazine isocyanuric acid adduct silane Coupling agent: 3-glycidoxypropyltrimethoxysilane silica carbon black graphene 1 (average layer thickness 0.09 μm, average cross-sectional area 10 μm ² ),
Graphene 2 (average layer thickness 0.0015 μm, average cross-sectional area 90 μm ² )
Graphene 3 (average layer thickness 0.00025 μm, average cross-sectional area 49 μm ² )
Hygroscopic material 1: Synthetic imogolite (average particle size 1.3 μm)
Hygroscopic material 2: Synthetic zeolite (average particle size 4 to 6 μm)
Isoprene rubber: Maleic anhydride adduct of isoprene polymer

[Example 1]
In preparing the adhesive composition, the raw materials (weight unit is gram) shown in Table 1 are stirred and mixed by a rotating stirring mixer, and then the layered inorganic substances are sufficiently dispersed in the resin by three rolls to obtain a vacuum. An uncured liquid resin (adhesive composition) was obtained by defoaming and stirring.

[Examples 2 to 4, Comparative Examples 1 and 2]
In Examples 2 to 4 and Comparative Examples 1 and 2, the formulation of the raw materials was changed as shown in Table 1 in the same procedure as in Example 1 to obtain a liquid resin. In Table 1, the vol% volume%, wt% indicates% by weight, viscosity unit is mPa · s, a unit of the moisture permeability is ^{2.0g / (m 2 · 24h)} .

In Example 1, when 5% by volume of graphene 1 was used and 10% by weight of the adsorbent 1 was used, an adhesive composition having 170000 clay, 0.8 moisture permeability, and 43 yellowing degree was obtained. .. Since the adhesive composition contains a small amount of graphene 1, the viscosity is relatively easy to handle, and the degree of yellowing is 43. Therefore, graphene does not contain an ultraviolet absorber or an ultraviolet shielding agent. It can be seen that 1 indicates that the product has high UV resistance.

In Example 2, when graphene 1 was increased to 7% by volume, the viscosity increased to 402000, which was within the permissible range for use as a sealing application, and the moisture permeability and yellowing degree were also good. rice field. In Example 3, two kinds of hygroscopic agents were used in combination, but both the moisture permeability and the degree of yellowing were good. In Examples 4 and 5, when graphenes 2 and 3 having an average layer thickness thinner than that of graphene 1 were used, good results were obtained in terms of both moisture permeability and yellowing degree.

On the other hand, in Comparative Example 1, neither graphene (layered inorganic substance) nor a hygroscopic agent was used, and the moisture permeability was as high as 3.8, which is the same in Comparative Example 2. Further, in Comparative Example 3, graphene 1 was used, but the hygroscopic agent 1 was not used, and the moisture permeability was as high as 2.1, indicating that the combined use of the hygroscopic agent is important. Further, in Comparative Example 4, graphene was not used and no hygroscopic agent was used. In this case as well, the moisture permeability was high, and unlike the adhesive composition of the present invention, low moisture permeability could not be realized.

1 Resin 2 Layered inorganic substance 3 Hygroscopic agent 4 Package 5 LED chip (light emitting element)
6 Opening 7 Closure 10 Adhesive composition 20 Light emitting diode

Claims (7)

A sealing adhesive composition comprising a resin, graphene, and a hygroscopic agent. The sealing adhesive composition according to claim 1, wherein the graphene is contained in an amount of 0.5 to 15% by volume. The sealing adhesive composition according to claim 1 or 2, wherein the graphene has an average area of 1 to 100 μm ^2. The sealing adhesive composition according to any one of claims 1 to 3, wherein the hygroscopic agent is contained in an amount of 0.5 to 20% by weight. The sealing adhesive composition according to claim 4, wherein the hygroscopic agent has an average particle size of 1 nm to 10 μm. A sealing member, wherein the sealing adhesive according to any one of claims 1 to 5 is applied to a translucent lid material. An electronic member in which a sealed component is housed in a package having an opening.
An electronic member characterized in that the opening is sealed by the sealing composition according to any one of claims 1 to 5.

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