JP2006111792A - Adhesive composition - Google Patents
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- JP2006111792A JP2006111792A JP2004302487A JP2004302487A JP2006111792A JP 2006111792 A JP2006111792 A JP 2006111792A JP 2004302487 A JP2004302487 A JP 2004302487A JP 2004302487 A JP2004302487 A JP 2004302487A JP 2006111792 A JP2006111792 A JP 2006111792A
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- adhesive composition
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- alumina powder
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- 239000000853 adhesive Substances 0.000 title claims abstract description 57
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 57
- 239000000203 mixture Substances 0.000 title claims abstract description 51
- 239000000843 powder Substances 0.000 claims abstract description 62
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 26
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052912 lithium silicate Inorganic materials 0.000 claims abstract description 22
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 20
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 16
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 16
- 239000011521 glass Substances 0.000 abstract description 18
- 230000000052 comparative effect Effects 0.000 description 10
- 238000011156 evaluation Methods 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 238000005187 foaming Methods 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 239000008119 colloidal silica Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- ASTDPSSQLZVNNF-UHFFFAOYSA-N diethyl-methyl-[5-(oxiran-2-ylmethoxy)pentan-2-yloxy]silane Chemical compound C(C1CO1)OCCCC(C)O[Si](CC)(CC)C ASTDPSSQLZVNNF-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- -1 γ-aminopropyl Chemical group 0.000 description 1
Abstract
Description
本発明は、接着性組成物に関し、詳しくは高熱伝導性で、電球を構成するガラスバルブを口金、ミラー材料、磁製ベースなどと接着するために好適に用いられる接着性組成物に関する。 The present invention relates to an adhesive composition, and more particularly to an adhesive composition that has high thermal conductivity and is suitably used for bonding a glass bulb constituting a light bulb to a base, a mirror material, a magnetic base, and the like.
光源装置などに用いられる電球を構成するガラスバルブを口金、ミラー材料、磁製ベースなどと接着する方法としては、ガラスバルブと口金等との間の隙間に接着性組成物を充填し、硬化させる方法が一般的であり、接着性組成物としては、隙間への充填が容易で、硬化後には十分な接着力を示し、ガラスバルブ内のフィラメントや、これを支えるリード線からの熱を外部に伝えて放熱するための高い熱伝導性を示すことが求められている。 As a method of adhering a glass bulb constituting a light bulb used in a light source device to a base, a mirror material, a magnetic base, etc., an adhesive composition is filled in a gap between the glass bulb and the base and cured. The method is general, and as an adhesive composition, it is easy to fill in the gap and shows sufficient adhesive force after curing, and heat from the filament in the glass bulb and the lead wire that supports it is externally exposed. It is required to exhibit high thermal conductivity to convey and dissipate heat.
このような接着性組成物として、例えば特許文献１〔特開平１１−１１６８９９号公報〕には、耐火物粉末として窒化アルミニウム粉末を、無機バインダーとして燐酸アルミニウムを含む接着性組成物が開示されている。特許文献２〔特開２００１−３１６６３８号公報〕には、耐火物粉末として炭化珪素粉末を、無機バインダーとしてコロイダルシリカを含む接着性組成物が開示されている。 As such an adhesive composition, for example, Patent Document 1 (Japanese Patent Laid-Open No. 11-116899) discloses an adhesive composition containing an aluminum nitride powder as a refractory powder and an aluminum phosphate as an inorganic binder. . Patent Document 2 (Japanese Patent Laid-Open No. 2001-316638) discloses an adhesive composition containing silicon carbide powder as a refractory powder and colloidal silica as an inorganic binder.
しかし、特許文献１に記載の接着性組成物は、無機バインダーとして燐酸アルミニウムを用いているため、十分な接着力を示すよう硬化させるには、充填後、２４時間、室温で保持した後に加熱する必要があり、実用的ではない。特許文献２に記載の接着性組成物では、硬化させる際に予め加熱された炉内に投入するなどして急速に加熱すると、発泡してしまう。 However, since the adhesive composition described in Patent Document 1 uses aluminum phosphate as an inorganic binder, in order to cure it so as to exhibit a sufficient adhesive force, it is heated after being held at room temperature for 24 hours after filling. Needed and not practical. When the adhesive composition described in Patent Document 2 is rapidly heated, for example, by being placed in a preheated furnace when being cured, the composition is foamed.
このようなことから、急速に加熱しても、発泡を伴うことなく硬化し得る接着性組成物が求められている。 For these reasons, there is a need for an adhesive composition that can be cured without foaming even when heated rapidly.
このような状況の下で本発明者は、ガラスバルブと口金等との接着に使用し得る接着性組成物について鋭意検討した結果、耐火物粉末としてアルミナ粉末およびシリカ粉末を含み、無機バインダーとして所定量の珪酸リチウムを含み、更に所定量のシランカップリング剤を含む組成物は、隙間への充填が容易で、急速に加熱しても発砲せず、短時間で硬化し得、硬化後に十分な接着力および高い熱伝導性を示すことを見出し、本発明に至った。 Under such circumstances, the present inventor has intensively studied an adhesive composition that can be used for adhesion between a glass bulb and a base, etc. As a result, the present invention includes alumina powder and silica powder as refractory powders, and serves as an inorganic binder. A composition containing a certain amount of lithium silicate and further containing a predetermined amount of a silane coupling agent is easy to fill in the gap, does not ignite even when heated rapidly, and can be cured in a short time. It has been found that it exhibits adhesive strength and high thermal conductivity, and has led to the present invention.
すなわち本発明は、アルミナ粉末およびシリカ粉末と、該アルミナ粉末およびシリカ粉末の合計量１００重量部あたり珪酸リチウムをＳｉＯ2換算で５重量部〜１０重量部、シランカップリング剤を０．２重量部〜１重量部含むことを特徴とする接着性組成物を提供するものである。 That is, the present invention relates to alumina powder and silica powder, and 5 parts by weight to 10 parts by weight of silicate coupling agent in terms of SiO 2 and 0.2 parts by weight of silane coupling agent per 100 parts by weight of the total amount of the alumina powder and silica powder. An adhesive composition characterized by containing ˜1 part by weight is provided.
本発明の接着性組成物は、急速に加熱しても発泡することがなく、短時間で硬化し得、硬化後の熱伝導性にも優れているので、電球を構成するガラスバルブと口金、ミラー材料、磁製ベースなどとを接着する接着性組成物として有用である。 The adhesive composition of the present invention does not foam even when heated rapidly, can be cured in a short time, and is excellent in thermal conductivity after curing, so a glass bulb and a base constituting a light bulb, It is useful as an adhesive composition for adhering mirror materials, magnetic bases and the like.
本発明の接着性組成物に適用されるアルミナ粉末としては、通常、α−アルミナ粉末が用いられる。シリカ粉末としては、通常、石英粒子が用いられる。アルミナ粉末およびシリカ粉末の粒子径は、十分な接着力を示す点で、通常０．１μｍ以上であり、ガラスバルブと口金等との間に充填し易い点で、通常１００μｍ以下である。 As the alumina powder applied to the adhesive composition of the present invention, α-alumina powder is usually used. Quartz particles are usually used as the silica powder. The particle diameters of the alumina powder and the silica powder are usually 0.1 μm or more in view of sufficient adhesive strength, and are usually 100 μm or less in terms of easy filling between the glass bulb and the base.
ガラスバルブと口金等との間に充填し易く、硬化後の接着力および熱伝導性に優れている点で、アルミナ粉末の中心粒子径が６０μｍ〜７０μｍの範囲であり、シリカ粉末の中心粒子径が３μｍ〜５μｍの範囲であり、シリカ粉末の含有量が、アルミナ粉末およびシリカ粉末の合計量を基準として３０重量％〜７０重量％であることが、好ましい。 The center particle diameter of the alumina powder is in the range of 60 μm to 70 μm, and the center particle diameter of the silica powder is easy to fill between the glass bulb and the base, and is excellent in adhesive strength and thermal conductivity after curing. Is in the range of 3 μm to 5 μm, and the content of the silica powder is preferably 30% by weight to 70% by weight based on the total amount of the alumina powder and the silica powder.
珪酸リチウムの含有量はＳｉＯ2換算である。珪酸リチウムの含有量（ＳｉＯ2換算）が、アルミナ粉末およびシリカ粉末の合計量１００重量部あたり５重量部未満では十分な接着力を得ることができず、１０重量部を超えると粘度が低くなって、ガラスバルブと口金等との間に充填したのち必要量の接着性組成物を保持することが困難となる。 The content of lithium silicate is in terms of SiO 2 . When the content of lithium silicate (in terms of SiO 2 ) is less than 5 parts by weight per 100 parts by weight of the total amount of alumina powder and silica powder, sufficient adhesive strength cannot be obtained, and when it exceeds 10 parts by weight, the viscosity becomes low. Thus, it becomes difficult to hold the necessary amount of the adhesive composition after filling between the glass bulb and the base.
シランカップリング剤は、加水分解により分子中に２個以上のシラノール基を生ずる化合物であり、例えばγ−グリシドキシプロピルトリメトキシシラン、γ−グリシドキシプロピルメチルジエチルエトキシシラン、γ-アミノプロピルトリメトキシシランなどが挙げられる。シランカップリング剤は、その一部または全部が加水分解されていてもよい。 Silane coupling agents are compounds that produce two or more silanol groups in the molecule by hydrolysis, such as γ-glycidoxypropyltrimethoxysilane, γ-glycidoxypropylmethyldiethylethoxysilane, γ-aminopropyl. Examples include trimethoxysilane. A part or all of the silane coupling agent may be hydrolyzed.
本発明の接着性組成物は、通常、水で希釈された状態で用いられる。水の使用量は、接着性組成物を硬化させた後の固形分に対して通常０．２重量倍〜０．４重量倍程度である。水の使用量が０．２重量倍未満であると、粘度が高くなって、ガラスバルブと口金等との間の隙間に充填しにくくなり、０．４重量倍を超えると、充填した後に流れ出して、必要量を保持しにくくなる。 The adhesive composition of the present invention is usually used in a state diluted with water. The usage-amount of water is about 0.2 to 0.4 weight times normally with respect to solid content after hardening an adhesive composition. If the amount of water used is less than 0.2 times by weight, the viscosity will increase and it will be difficult to fill the gap between the glass bulb and the mouthpiece, etc. If it exceeds 0.4 times by weight, it will flow out after filling. This makes it difficult to hold the required amount.
本発明の接着性組成物は、例えばアルミナ粉末、シリカ粉末、珪酸リチウムおよびシランカップリング剤を混合する方法により容易に製造することができる。珪酸リチウムは通常、水溶液として市販されているので、この珪酸リチウム水溶液にアルミナ粉末、シリカ粉末およびシランカップリング剤を加えて混合してもよい。 The adhesive composition of the present invention can be easily produced, for example, by a method of mixing alumina powder, silica powder, lithium silicate and silane coupling agent. Since lithium silicate is usually marketed as an aqueous solution, alumina powder, silica powder and a silane coupling agent may be added to and mixed with this lithium silicate aqueous solution.
かくして得られる本発明の接着性組成物は、例えば大量の電球を製造するために、長時間に亙りノズルから繰り返し吐出しても、ノズルを詰まらせることがなく、ガラスバルブと口金等との間に容易に充填することができ、充填後、急速に加熱しても発砲せず、短時間で硬化し、硬化後の接着力も十分である。そして、熱伝導性が良いので、ガラスバルブ内のフィラメントやリード線からの熱を速やかに放熱することができる。 The adhesive composition of the present invention thus obtained does not clog the nozzle even if it is repeatedly discharged from the nozzle over a long period of time, for example, in order to produce a large number of light bulbs. It can be filled easily, and it does not shoot even if heated rapidly after filling, cures in a short time, and the adhesive strength after curing is sufficient. And since heat conductivity is good, the heat | fever from the filament in a glass bulb and a lead wire can be thermally radiated rapidly.
本発明の接着性組成物を用いて電球を構成するガラスバルブを金属製の口金、金属製のミラー材料、セラミックス製の磁製ベースなどと接着するには、ガラスバルブと、これら口金等との間の隙間に本発明の接着性組成物を充填し、加熱すればよい。加熱温度は通常１５０℃〜２００℃程度である。加熱は、例えば５℃／分〜３０℃／分程度の昇温速度で昇温して加熱してもよいが、予め加熱された炉内に投入するなどして急速に加熱しても、本発明の接着性組成物は発泡することなく硬化する。 In order to bond a glass bulb constituting a light bulb using the adhesive composition of the present invention to a metal base, a metal mirror material, a ceramic magnetic base, etc., the glass bulb and the base, etc. What is necessary is just to fill the adhesive composition of this invention in the clearance gap between them, and to heat. The heating temperature is usually about 150 ° C to 200 ° C. The heating may be performed by heating at a temperature rising rate of, for example, about 5 ° C./min to 30 ° C./min. The adhesive composition of the invention cures without foaming.
以下、実施例によって本発明をより詳細に説明するが、本発明は、かかる実施例によって限定されるものではない。 EXAMPLES Hereinafter, although an Example demonstrates this invention in detail, this invention is not limited by this Example.
なお、各実施例で用いた粉末および得られた接着性組成物は、以下の方法で評価した。
（１）粒子径分布および中心粒子径
レーザー回折式粒度分布測定装置〔(株)島津製作所製、「ＳＡＬＤ２１００」〕を用いて粒度分布を測定し、重量累積粒度分布の累積５０％粒子径(Ｄ50)を求め、中心粒子径とした。
（２）粘度
粘度計〔リオン(株)製、「ビスコテスターＶＴ−０４」〕を用い、同装置に付属のＮｏ．２号ローターを用いて２５℃にて１分後の粘度を測定した。
（３）発泡性および熱伝導率
内寸法１００ｍｍ×５０ｍｍ×１５ｍｍの成形型に接着性組成物を入れ、１５０℃まで１０℃／分で昇温し、この昇温過程での発泡の有無を目視で観察した。１５０℃に昇温後、同温度で１時間保持することにより硬化させて、１００ｍｍ×５０ｍｍ×１５ｍｍの直方体状の硬化物を得、この硬化物３個について熱伝導率計〔京都電子工業(株)製、「ＱＴＭ−２００」〕にて熱伝導率を測定し、その平均値を求めた。
（４）電球封止部の温度評価
接着性組成物をＪＤＲタイプの電球〔定格電圧１１０Ｖ、定格電力７５Ｗ〕のガラスバルブと口金との間に充填し、予め１５０℃に加熱された炉内に入れて同温度で硬化させ、１時間後に取出して電球を作成する。このようにして作成した電球５個について、それぞれ消費電力８１Ｗ〔定格の１０８％〕で点灯させて、ＪＩＳ Ｃ７５０１に準拠してリード線（モリブデン製）を封止している部分の温度を測定し、その平均値と３σを求めた。
（５）接着力
内径１２ｍｍのガラス管内に、外径９ｍｍのガラス製の丸棒を入れ、管と丸棒との間に接着性組成物１．５ｇを均一に充填し、１５０℃にて１時間保持して硬化させた。その後、精密万能試験機〔(株)島津製作所製、「オートグラフＡＧＳ１０００Ｂ型」〕にて丸棒をガラス管から押し抜くに要する力を測定して、接着力とした。
（６）自動充填性
ステンレス製ニードルバルブ〔岩下エンジニアリング(株)製、「ＡＶ−５０１」〕およびニードルノズル〔ＪＩＳ規格に規定の１３Ｇ型のニードル（内径１．５ｍｍ、外径２．０ｍｍ、長さ４０ｍｍ、ステンレス製、電解研磨注射針）〕を備え、コントローラー〔岩下エンジニアリング(株)製、「ＡＤ−３０００」〕により吐出時間および吐出サイクルを調整可能に構成した定量供給装置を用いて、ニードルノズルから、吐出時間１．２秒、吐出間隔７秒で繰り返し連続して２０００ショット、接着性組成物を吐出し、その間の１回あたりの吐出量を測定して評価した。
In addition, the powder used in each Example and the obtained adhesive composition were evaluated by the following methods.
(1) Particle size distribution and central particle size The particle size distribution is measured using a laser diffraction particle size distribution measuring apparatus (“SALD2100”, manufactured by Shimadzu Corporation), and the 50% cumulative particle size (D50 ) And determined as the center particle size.
(2) Using a viscometer [manufactured by Rion Co., Ltd., “Viscotester VT-04”], No. The viscosity after 1 minute was measured at 25 ° C. using a No. 2 rotor.
(3) Foamability and thermal conductivity The adhesive composition is put into a mold having dimensions of 100 mm × 50 mm × 15 mm, and the temperature is raised to 150 ° C. at 10 ° C./min. Observed at. After the temperature was raised to 150 ° C., it was cured by holding at the same temperature for 1 hour to obtain a 100 mm × 50 mm × 15 mm rectangular solid cured product, and a thermal conductivity meter [Kyoto Electronics Industry Co., Ltd. ), “QTM-200”], the thermal conductivity was measured, and the average value was obtained.
(4) Temperature evaluation of the bulb sealing part The adhesive composition is filled between a glass bulb and a base of a JDR type bulb [rated voltage 110 V, rated power 75 W], and preheated to 150 ° C. Put in and cure at the same temperature and take out after 1 hour to make a light bulb. Each of the five light bulbs thus created was turned on at a power consumption of 81 W (108% of the rating), and the temperature of the portion where the lead wire (made of molybdenum) was sealed in accordance with JIS C7501 was measured. The average value and 3σ were obtained.
(5) A glass round bar with an outer diameter of 9 mm is placed in a glass tube with an inner diameter of 12 mm, and 1.5 g of the adhesive composition is uniformly filled between the tube and the round bar. Hold for time to cure. Thereafter, the force required to push out the round bar from the glass tube was measured with a precision universal testing machine [manufactured by Shimadzu Corporation, “Autograph AGS1000B type”] to obtain an adhesive force.
(6) Self-filling stainless steel needle valve (“AV-501” manufactured by Iwashita Engineering Co., Ltd.) and needle nozzle [13G type needle defined by JIS standard (inner diameter 1.5 mm, outer diameter 2.0 mm, long 40 mm, stainless steel, electrolytic polishing needle), and a needle using a quantitative supply device configured to adjust the discharge time and the discharge cycle by a controller (“AD-3000” manufactured by Iwashita Engineering Co., Ltd.) From the nozzle, 2000 shots of the adhesive composition were repeatedly and continuously discharged at a discharge time of 1.2 seconds and a discharge interval of 7 seconds, and the discharge amount per one time was measured and evaluated.
実施例１
アルミナ粉末〔太平洋ランダム(株)製「５０Ａ」、粒子径範囲１μｍ〜１５０μｍ、中心粒子径（Ｄ50）６５μｍ〕７３５ｇ、シリカ粉末〔龍森(株)製、「クリスタライトＶＸ−Ｓ２」、粒子径範囲０．３μｍ〜３０μｍ、中心粒子径（Ｄ50）５μｍ〕９７３ｇ、珪酸リチウム液〔日産化学(株)製、「リチウムシリケートＬ−４５」、ＳｉＯ2換算含有量２０重量％、Ｌｉ含有量がＳｉＯ2に対して４．５モル倍の水溶液〕７９３ｇ（ＳｉＯ2換算１５９ｇ）、シランカップリング剤〔東レダウコーニングシリコーン(株)製、「ＳＨ６０４０」、γ−グリシドキシプロピルトリメトキシシラン〕８ｇを混合し、３０分かけて撹拌して、接着性組成物を得た。
Example 1
Alumina powder [Pacific Random Co., Ltd. “50A”, particle size range 1 μm to 150 μm, center particle size (D50) 65 μm] 735 g, silica powder [Tatsumori Co., Ltd., “Crystallite VX-S2”, particle size Range 0.3 μm to 30 μm, center particle diameter (D50) 5 μm] 973 g, lithium silicate liquid [manufactured by Nissan Chemical Co., Ltd., “lithium silicate L-45”, SiO 2 conversion content 20 wt%, Li content is SiO 2 with respect to 4.5 mol per mol of the aqueous solution] 793G (SiO 2 in terms of 159 g), silane coupling agent [Dow Corning Toray silicone Co., Ltd., "SH6040", the γ- glycidoxypropyltrimethoxysilane] 8g The mixture was mixed and stirred for 30 minutes to obtain an adhesive composition.
上記で得た接着性組成物の粘度は１４０Ｐ（１４０００ｃＰ）であり、昇温時の発泡は見られず、熱伝導率は１．８６Ｗ／ｍ・Ｋであり、この接着性組成物を用いて電球封止部の温度を評価したところ、平均温度は２８１．９℃、３σは１１．７℃であった。接着力を評価したところ、３０ｋｇｆ（２９４Ｎ）であった。自動充填性を評価したところ、１ショット目から２０００ショット目までの１ショット当りの吐出量は概ね０．４ｇ±０．１ｇの範囲で一定であった。評価結果を第１表に示す。 The viscosity of the adhesive composition obtained above is 140 P (14000 cP), no foaming is observed at the time of temperature rise, and the thermal conductivity is 1.86 W / m · K. Using this adhesive composition When the temperature of the bulb sealed portion was evaluated, the average temperature was 281.9 ° C. and 3σ was 11.7 ° C. When the adhesive strength was evaluated, it was 30 kgf (294N). When the automatic filling property was evaluated, the discharge amount per shot from the first shot to the 2000th shot was generally constant within a range of 0.4 g ± 0.1 g. The evaluation results are shown in Table 1.
実施例２
アルミナ粉末〔５０Ａ〕の使用量を１２２５ｇ、シリカ粉末〔クリスタライトＶＸ−Ｓ２〕の使用量を６９２ｇ、珪酸リチウム液〔リチウムシリケートＬ−４５〕の使用量を６６７ｇ（ＳｉＯ2換算１３３ｇ）とし、シランカップリング剤〔ＳＨ６０４０〕の使用量を７ｇとした以外は実施例１と同様に操作して、接着性組成物を得た。この接着性組成物の評価結果を第１表に示す。
Example 2
The amount of alumina powder [50A] used is 1225 g, the amount of silica powder [Crystallite VX-S2] is 692 g, the amount of lithium silicate liquid [lithium silicate L-45] is 667 g (133 g in terms of SiO 2 ), and silane An adhesive composition was obtained in the same manner as in Example 1 except that the amount of the coupling agent [SH6040] used was 7 g. The evaluation results of this adhesive composition are shown in Table 1.
第 １ 表
━━━━━━━━━━━━━━━━━━━━━━━━
実施例１ 実施例２
━━━━━━━━━━━━━━━━━━━━━━━━
アルミナ粉末 (ｇ) 735 1225
シリカ粉末 (ｇ) 973 692
ムライト粉末 (ｇ) − −
ジルコニア粉末 (ｇ) − −
珪酸リチウム（ＳｉＯ2)(ｇ) 159 133
シランカップリング剤 (ｇ) 8 7
────────────────────────
粘度 (ｃＰ) 14000 14000
発泡の有無 なし なし
熱伝導率 (Ｗ／ｍ・Ｋ) 1.86 2.03
電球封止部 (℃) 281.9 280.7
３σ (℃) 11.7 15.1
接着力 (ｋｇｆ) 30 −
吐出量 (ｇ) 0.4±0.1 −
━━━━━━━━━━━━━━━━━━━━━━━━
Table 1
━━━━━━━━━━━━━━━━━━━━━━━━
Example 1 Example 2
━━━━━━━━━━━━━━━━━━━━━━━━
Alumina powder (g) 735 1225
Silica powder (g) 973 692
Mullite powder (g) − −
Zirconia powder (g) − −
Lithium silicate (SiO 2 ) (g) 159 133
Silane coupling agent (g) 8 7
────────────────────────
Viscosity (cP) 14000 14000
No foaming None None
Thermal conductivity (W / m · K) 1.86 2.03
Bulb seal (° C) 281.9 280.7
3σ (℃) 11.7 15.1
Adhesive strength (kgf) 30 −
Discharge rate (g) 0.4 ± 0.1 −
━━━━━━━━━━━━━━━━━━━━━━━━
比較例１
ムライト粉末〔村田窯業(株)製〕１７００ｇ、珪酸リチウム液〔リチウムシリケートＬ−４５〕６２０ｇ（ＳｉＯ2換算１２４ｇ）およびシランカップリング剤〔ＳＨ６０４０〕６ｇを混合し、３０分かけて撹拌して、接着性組成物を得た。この接着性組成物の評価結果を第２表に示す。
Comparative Example 1
1700 g of mullite powder [Murata Ceramics Co., Ltd.], 620 g of lithium silicate liquid [lithium silicate L-45] (124 g in terms of SiO 2 ) and 6 g of silane coupling agent [SH6040] were mixed and stirred for 30 minutes. An adhesive composition was obtained. The evaluation results of this adhesive composition are shown in Table 2.
比較例２
アルミナ粉末〔５０Ａ〕９１０ｇ、ジルコニア粉末〔日本ガイシ(株)製〕１４００ｇ、珪酸リチウム液〔リチウムシリケートＬ−４５〕５５３ｇ（ＳｉＯ2換算１１１ｇ）およびシランカップリング剤〔ＳＨ６０４０〕６ｇを混合し、３０分かけて撹拌して、接着性組成物を得た。この接着性組成物の評価結果を第２表に示す。
Comparative Example 2
910 g of alumina powder [50A], 1400 g of zirconia powder [manufactured by NGK Co., Ltd.], 553 g of lithium silicate liquid [lithium silicate L-45] (111 g in terms of SiO 2 ), and 6 g of silane coupling agent [SH6040] are mixed. It stirred over minutes and obtained the adhesive composition. The evaluation results of this adhesive composition are shown in Table 2.
比較例３
アルミナ粉末〔住友化学工業(株)製、「ＡＭ−２１Ａ」、粒子径範囲０．５μｍ〜４０μｍ、中心粒子径（Ｄ50）７μｍ〕１７９０ｇ、珪酸リチウム液〔リチウムシリケートＬ−４５〕５５３ｇ（ＳｉＯ2換算１１１ｇ）およびシランカップリング剤〔ＳＨ６０４０〕６ｇを混合し、３０分かけて撹拌して、接着性組成物を得た。この接着性組成物の評価結果を第２表に示す。
Comparative Example 3
Alumina powder [manufactured by Sumitomo Chemical Co., Ltd., “AM-21A”, particle size range 0.5 μm to 40 μm, center particle size (D50) 7 μm] 1790 g, lithium silicate liquid [lithium silicate L-45] 553 g (SiO 2 111 g) and 6 g of a silane coupling agent [SH6040] were mixed and stirred for 30 minutes to obtain an adhesive composition. The evaluation results of this adhesive composition are shown in Table 2.
比較例４
シリカ粉末〔クリスタライトＶＸ−Ｓ２〕１６８０ｇ、珪酸リチウム液〔リチウムシリケートＬ−４５〕６００ｇ（ＳｉＯ2換算１２０ｇ）およびシランカップリング剤〔ＳＨ６０４０〕６ｇを混合し、３０分かけて撹拌して、接着性組成物を得た。この接着性組成物の評価結果を第２表に示す。
Comparative Example 4
1680 g of silica powder [crystallite VX-S2], lithium silicate liquid [lithium silicate L-45] 600 g (120 g in terms of SiO 2 ) and 6 g of silane coupling agent [SH6040] are mixed and stirred for 30 minutes to bond Sex composition was obtained. The evaluation results of this adhesive composition are shown in Table 2.
比較例５
アルミナ粉末〔５０Ａ〕７３５ｇ、シリカ粉末〔クリスタライトＶＸ−Ｓ２〕９７３ｇ、コロイダルシリカ液〔「アデライトＡＴ−４０」、旭電化工業(株)製、コロイダルシリカが水に分散された分散液〕８１０ｇ（ＳｉＯ2換算３２４ｇ）およびシランカップリング剤〔ＳＨ６０４０〕８ｇを混合し、３０分かけて撹拌して、接着性組成物を得た。この接着性組成物の評価結果を第２表に示す。
Comparative Example 5
Alumina powder [50A] 735 g, silica powder [Crystallite VX-S2] 973 g, colloidal silica liquid [“Adelite AT-40”, manufactured by Asahi Denka Kogyo Co., Ltd., dispersion in which colloidal silica is dispersed in water] 810 g ( in terms of SiO 2 324 g) and silane coupling agent [SH6040] 8g were mixed and stirred over a period of 30 minutes to obtain an adhesive composition. The evaluation results of this adhesive composition are shown in Table 2.
第 ２ 表
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
比較例１ 比較例２ 比較例３ 比較例４ 比較例５
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
アルミナ粉末 (ｇ) − 910 1790 − 735
シリカ粉末 (ｇ) − − − 1680 973
ムライト粉末 (ｇ) 1700 − − − −
ジルコニア粉末 (ｇ) − 1400 − − −
珪酸リチウム(SiO2) (ｇ) 124 111 111 120 −
コロイダルシリカ(SiO2)(ｇ) − − − − 324
シランカップリング剤 (ｇ) 6 6 6 6 8
───────────────────────────────────────
粘度 (ｃＰ) 14000 14000 14000 15000 14000
発泡の有無 なし なし なし なし 有り
熱伝導率 (Ｗ／ｍ・Ｋ) 0.80 1.61 1.49 1.16 1.85
電球封止部平均温度 (℃) 307.8 302.2 297.2 287.2 −
３σ (℃) 23.8 16.1 15.3 16.5 −
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Table 2
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Alumina powder (g) − 910 1790 − 735
Silica powder (g) − − − 1680 973
Mullite powder (g) 1700 − − − −
Zirconia powder (g) − 1400 − − −
Lithium silicate (SiO 2 ) (g) 124 111 111 120 −
Colloidal silica (SiO 2 ) (g) − − − − 324
Silane coupling agent (g) 6 6 6 6 8
───────────────────────────────────────
Viscosity (cP) 14000 14000 14000 15000 14000
No foaming No No No No Yes Yes
Thermal conductivity (W / m · K) 0.80 1.61 1.49 1.16 1.85
Average temperature of sealed bulb (° C) 307.8 302.2 297.2 287.2 −
3σ (° C) 23.8 16.1 15.3 16.5 −
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
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|---|---|---|---|---|
| JPH02256134A (en) * | 1989-03-29 | 1990-10-16 | Toshiba Lighting & Technol Corp | Base adhesive for bulb |
| JPH0374483A (en) * | 1989-08-14 | 1991-03-29 | Nissan Chem Ind Ltd | Inorganic adhesive having high strength |
| JPH04311785A (en) * | 1991-04-09 | 1992-11-04 | Nissan Chem Ind Ltd | Inorganic adhesive |
| JPH0582109A (en) * | 1991-09-25 | 1993-04-02 | Toshiba Lighting & Technol Corp | Halogen lamp and downlight |
| JPH08157638A (en) * | 1994-12-07 | 1996-06-18 | Toray Ind Inc | Resin composition |
| JPH08212983A (en) * | 1995-02-01 | 1996-08-20 | Matsushita Electron Corp | Bulb |
| JPH11166158A (en) * | 1997-12-04 | 1999-06-22 | Nippon Muki Co Ltd | Inorganic adhesive |
| JP2001329230A (en) * | 2000-05-22 | 2001-11-27 | Asahi Kagaku Kogyo Co Ltd | Inorganic adhesive composition, its manufacturing method and bonding method |
| JP2006114421A (en) * | 2004-10-18 | 2006-04-27 | Matsushita Electric Ind Co Ltd | Tubular bulb |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02256134A (en) * | 1989-03-29 | 1990-10-16 | Toshiba Lighting & Technol Corp | Base adhesive for bulb |
| JPH0374483A (en) * | 1989-08-14 | 1991-03-29 | Nissan Chem Ind Ltd | Inorganic adhesive having high strength |
| JPH04311785A (en) * | 1991-04-09 | 1992-11-04 | Nissan Chem Ind Ltd | Inorganic adhesive |
| JPH0582109A (en) * | 1991-09-25 | 1993-04-02 | Toshiba Lighting & Technol Corp | Halogen lamp and downlight |
| JPH08157638A (en) * | 1994-12-07 | 1996-06-18 | Toray Ind Inc | Resin composition |
| JPH08212983A (en) * | 1995-02-01 | 1996-08-20 | Matsushita Electron Corp | Bulb |
| JPH11166158A (en) * | 1997-12-04 | 1999-06-22 | Nippon Muki Co Ltd | Inorganic adhesive |
| JP2001329230A (en) * | 2000-05-22 | 2001-11-27 | Asahi Kagaku Kogyo Co Ltd | Inorganic adhesive composition, its manufacturing method and bonding method |
| JP2006114421A (en) * | 2004-10-18 | 2006-04-27 | Matsushita Electric Ind Co Ltd | Tubular bulb |
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