JP2017155207A - LED curing moisture-proof insulation coating agent - Google Patents
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Abstract
【課題】電子部品を搭載する回路基板で用いられる防湿絶縁コート剤で、照射する光源がＬＥＤの場合でも短時間に硬化可能で、絶縁信頼性に優れた組成物であると共に、それを用いて絶縁処理した回路基板を提供する。【解決手段】水添ポリブタジエンジオールから合成された数平均分子量が１，０００〜２０，０００であるウレタンアクリレート（Ａ）と単官能 (メタ)アクリレートモノマー（Ｂ）と３８０ｎｍ以上の波長で吸収帯域を持つ開始剤（Ｃ）と、を含む光硬化性樹脂組成物であって、（Ｃ）成分の含有量が（Ａ）成分と（Ｂ）成分の合計１００重量部に対し１０〜１５重量部であるＬＥＤ硬化型防湿絶縁コート剤組成物である。【選択図】なしA moisture-proof insulating coating agent used for a circuit board on which electronic components are mounted, which is a composition that can be cured in a short time even when the illuminating light source is an LED and has excellent insulation reliability. An insulated circuit board is provided. SOLUTION: A urethane acrylate (A) synthesized from hydrogenated polybutadiene diol having a number average molecular weight of 1,000 to 20,000, a monofunctional (meth) acrylate monomer (B), and an absorption band at a wavelength of 380 nm or more. A photocurable resin composition comprising an initiator (C) having a content of (C) component of 10 to 15 parts by weight with respect to a total of 100 parts by weight of component (A) and component (B) It is a certain LED curable moisture-proof insulating coating agent composition. [Selection figure] None
Description
本発明は、電子部品を搭載する回路基板で用いられる防湿絶縁コート剤で、ＬＥＤ（発光ダイオード：ライトエミッティング ダイオード）光源により短時間で硬化が可能な絶縁信頼性に優れた組成物であると共に、それを用いて絶縁処理した実装回路基板に関するものである。 The present invention is a moisture-proof insulating coating agent used in a circuit board on which electronic components are mounted, and is a composition excellent in insulation reliability that can be cured in a short time by an LED (light emitting diode: light emitting diode) light source. Further, the present invention relates to a mounted circuit board that is insulated using the same.
ガラスエポキシ、紙フェノール、ポリイミド等の基材に代表されるプリント配線板へ半導体等の電子部品を実装する際に、その接続部には接続信頼性を高めるため防湿絶縁コート剤が塗布される場合がある。従来このコート剤には熱硬化樹脂の使用、あるいは有機溶剤に溶解した樹脂を塗布後に乾燥する方法が一般的であった。しかし熱硬化樹脂の場合は樹脂硬化に加熱工程が必要で硬化時間がかかるため生産性に問題があり、有機溶剤を使用する樹脂は塗布時に溶剤を揮発させるため環境への負荷が高いという問題が有った。 When mounting electronic components such as semiconductors on printed wiring boards such as glass epoxy, paper phenol, and polyimide, a moisture-proof insulating coating agent is applied to the connection area to improve connection reliability. There is. Conventionally, a thermosetting resin or a method of drying after applying a resin dissolved in an organic solvent is generally used for this coating agent. However, in the case of a thermosetting resin, there is a problem in productivity because a heating process is required for resin curing and it takes a long time to cure, and a resin using an organic solvent has a problem of high environmental load because the solvent is volatilized at the time of application. There was.
こうした問題を解決すべく、短時間で硬化が可能な紫外線硬化性コート剤が開発されてきた。例えば特許文献１では末端がアクリロキシ基またはメタクリロキシ基であるポリブタジエンと、不飽和二重結を有する単量体と重合開始剤を含有する組成物が開示されている。また更に、透湿度が小さく基板材料に対して充分な接着性を持つコート剤として、特許文献２では水添ポリブタジエンジオールから合成したエチレン性不飽和二重結合を有するウレタン化合物と、イソボルニルアクリレートとベンゾフェノンを含む組成物が開示されている。しかしながらこれら組成物は、光源がＬＥＤの場合は硬化性が不十分という課題があった。 In order to solve these problems, ultraviolet curable coating agents that can be cured in a short time have been developed. For example, Patent Document 1 discloses a composition containing polybutadiene having a terminal acryloxy group or methacryloxy group, a monomer having an unsaturated double bond, and a polymerization initiator. Furthermore, as a coating agent having a low moisture permeability and sufficient adhesion to a substrate material, Patent Document 2 discloses a urethane compound having an ethylenically unsaturated double bond synthesized from hydrogenated polybutadiene diol and isobornyl acrylate. And a composition comprising benzophenone is disclosed. However, these compositions have a problem of insufficient curability when the light source is an LED.
本発明は、電子部品を搭載する回路基板で用いられる防湿絶縁コート剤で、照射する光源がＬＥＤの場合でも短時間に硬化可能で、絶縁信頼性に優れた組成物であると共に、それを用いて絶縁処理した回路基板を提供することにある。 The present invention is a moisture-proof insulating coating agent used in a circuit board on which electronic components are mounted, and is a composition that can be cured in a short time even when the light source to be irradiated is an LED and has excellent insulation reliability. Another object of the present invention is to provide an insulated circuit board.
請求項１記載の発明は、水添ポリブタジエンジオールから合成された数平均分子量が１，０００〜２０，０００であるウレタンアクリレート（Ａ）と単官能 (メタ)アクリレートモノマー（Ｂ）と３８０ｎｍ以上の波長で吸収帯域を持つ開始剤（Ｃ）と、を含む光硬化性樹脂組成物であって、（Ｃ）成分の含有量が（Ａ）成分と（Ｂ）成分の合計１００重量部に対し１０〜１５重量部であるＬＥＤ硬化型防湿絶縁コート剤組成物を提供する。 The invention according to claim 1 is a urethane acrylate (A) synthesized from hydrogenated polybutadiene diol having a number average molecular weight of 1,000 to 20,000, a monofunctional (meth) acrylate monomer (B), and a wavelength of 380 nm or more. And an initiator (C) having an absorption band, wherein the content of the component (C) is 10 to 10 parts by weight with respect to a total of 100 parts by weight of the component (A) and the component (B). Provided is an LED curable moisture-proof insulating coating composition that is 15 parts by weight.
請求項２記載の発明は、前記単官能 (メタ)アクリレートモノマー（Ｂ）が、脂肪族環状骨格を含むモノマーと、水酸基を含むモノマーと、直鎖アルキル基を含むモノマーを含む請求項１記載のＬＥＤ硬化型防湿絶縁コート剤組成物を提供する。 The invention according to claim 2 is the invention according to claim 1, wherein the monofunctional (meth) acrylate monomer (B) includes a monomer containing an aliphatic cyclic skeleton, a monomer containing a hydroxyl group, and a monomer containing a linear alkyl group. An LED curable moisture-proof insulating coating agent composition is provided.
請求項３記載の発明は、前記開始剤（Ｃ）が、０．１％濃度のアセトニトリル溶液において３８０ｎｍの波長吸収率が０．５％以上である、請求項1または２いずれかに記載のＬＥＤ硬化型防湿絶縁コート剤組成物を提供する。 The invention according to claim 3 is the LED according to claim 1 or 2, wherein the initiator (C) has a wavelength absorption at 380 nm of 0.5% or more in a 0.1% acetonitrile solution. A curable moisture-proof insulating coating agent composition is provided.
請求項４記載の発明は、請求項１〜３のいずれか記載のＬＥＤ硬化型防湿絶縁コート剤組成物を用いて絶縁処理されることを特徴とする実装回路基板を提供する。 According to a fourth aspect of the present invention, there is provided a mounted circuit board which is insulated using the LED curable moisture-proof insulating coating composition according to any one of the first to third aspects.
本発明の防湿絶縁コート剤は、防湿および絶縁特性に優れた紫外線硬化型の樹脂組成物で、特に照射する光源がＬＥＤの場合でも短時間に硬化可能な特性を有する。 The moisture-proof insulating coating agent of the present invention is an ultraviolet curable resin composition excellent in moisture-proof and insulating properties, and has a property that it can be cured in a short time even when the light source to be irradiated is an LED.
以下本発明について詳細に説明する。 The present invention will be described in detail below.
本発明の組成物の構成は、水添ポリブタジエンジオールから合成された数平均分子量が１，０００〜２０，０００であるウレタンアクリレート（Ａ）と単官能 (メタ)アクリレートモノマー（Ｂ）と３８０ｎｍ以上の波長で吸収帯域を持つ開始剤（Ｃ）である。なお、本明細書において（メタ）アクリレートとは、アクリレートとメタクリレートの双方を包含する。 The composition of the present invention comprises a urethane acrylate (A) synthesized from hydrogenated polybutadiene diol having a number average molecular weight of 1,000 to 20,000, a monofunctional (meth) acrylate monomer (B) and 380 nm or more. An initiator (C) having an absorption band at a wavelength. In the present specification, (meth) acrylate includes both acrylate and methacrylate.
本発明の水添ポリブタジエンジオールから合成された数平均分子量が１，０００〜２０，０００であるウレタンアクリレート（Ａ）は、防湿絶縁層を構成するベースオリゴマーであり、ポリオールに、複数のイソシアネート基を有する化合物、および水酸基を有する（メタ）アクリレートを反応させて得られる。使用するポリオールは、透湿度が低く絶縁性に優れまた成形皮膜に適度な柔軟性を付与する水添ポリブタジエン系である。数平均分子量が１，０００未満では得られる硬化物の粘着性が強く表面にべとつき感が残り、２０，０００を超えると組成物の粘度が高くなり、作業性に悪影響を及ぼす。数平均分子量は、ゲル透過クロマトグラフィー法により、スチレンジビニルベンゼン基材のカラムでテトラハイドロフラン展開溶媒を用いて、標準ポリスチレン換算の分子量を測定・算出した。 The urethane acrylate (A) having a number average molecular weight of 1,000 to 20,000 synthesized from the hydrogenated polybutadiene diol of the present invention is a base oligomer constituting a moisture-proof insulating layer, and a polyol has a plurality of isocyanate groups. It is obtained by reacting a compound having a hydroxyl group and a (meth) acrylate having a hydroxyl group. The polyol to be used is a hydrogenated polybutadiene system having a low moisture permeability and excellent insulating properties and imparting appropriate flexibility to the molded film. If the number average molecular weight is less than 1,000, the resulting cured product has strong tackiness and a sticky feeling remains on the surface. If the number average molecular weight exceeds 20,000, the viscosity of the composition increases, which adversely affects workability. The number average molecular weight was measured and calculated by a gel permeation chromatography method using a tetrahydrofuran solvent in a styrene divinylbenzene-based column and a standard polystyrene equivalent molecular weight.
本発明で使用される（Ａ）の原料である、複数のイソシアネート基を持つ化合物としては、例えばヘキサメチレンジイソシアネート、ヘプタメチレンジイソシアネート、オクタメチレンジイソシアネート、トリレンジイソシアネート、メチルシクロヘキサンジイソシアネート、ジシクロヘキシルメタンジイソシアネート、イソホロンジイソシアネート、ジフェニルメタンジイソシアネート、キシリレンジイソシアネートがあり、単独または２種類以上を組み合わせて使用できる。これらの中では、イソホロンジイソシアネートが好ましい。また水酸基を有する（メタ）アクリレートとしては、例えば２−ヒドロキシエチルアクリレート、２−ヒドロキシプロピルアクリレート、４−ヒドロキシブチルアクリレート、２−ヒドロキシエチルメタクリレートがあり、これらの中では２-ヒドロキシエチルアクリレート好ましい。 Examples of the compound having a plurality of isocyanate groups used in the present invention (A) include hexamethylene diisocyanate, heptamethylene diisocyanate, octamethylene diisocyanate, tolylene diisocyanate, methylcyclohexane diisocyanate, dicyclohexylmethane diisocyanate, isophorone. There are diisocyanate, diphenylmethane diisocyanate, and xylylene diisocyanate, which can be used alone or in combination of two or more. Of these, isophorone diisocyanate is preferred. Examples of the (meth) acrylate having a hydroxyl group include 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 4-hydroxybutyl acrylate, and 2-hydroxyethyl methacrylate. Among these, 2-hydroxyethyl acrylate is preferable.
配合量は（Ｃ）を除く全組成物１００重量部に対し、硬化物の透湿度と組成物の特性バランスから２５〜４５重量部が好ましく、３０〜４０重量部である事がより好ましい。２５重量部未満では透湿度が高くなる傾向があり、４５重量部を超えると粘度が高くなり作業性が悪化する。市販の水添ポリブタジエン骨格を持つウレタンクリレートとしてはＥｘｃｅｌａｔｅＲＸ７１−４４（商品名：亜細亜工業社製、数平均分子量３，０００）、ＲＸ７１−６７（商品名：亜細亜工業社製、数平均分子量１３，０００）がある。 The blending amount is preferably from 25 to 45 parts by weight, more preferably from 30 to 40 parts by weight, based on the moisture permeability of the cured product and the property balance of the composition with respect to 100 parts by weight of the entire composition excluding (C). If the amount is less than 25 parts by weight, the moisture permeability tends to increase. If the amount exceeds 45 parts by weight, the viscosity increases and the workability deteriorates. Examples of commercially available urethane acrylates having a hydrogenated polybutadiene skeleton include Excelate RX 71-44 (trade name: manufactured by Asia Industries, number average molecular weight 3,000), RX 71-67 (trade name: manufactured by Asia Industries, number average molecular weight 13, 000).
本発明で使用される単官能の（メタ）アクリレートモノマー（Ｂ）は、（Ａ）を希釈すると同時に（Ａ）と反応して皮膜硬度を上げるために配合される。基材との密着力、透湿性、（Ａ）との相溶性など観点から、脂肪族環式および水酸基含有および直鎖アルキル構造を持つ単官能の（メタ）アクリレートであることが好ましい。配合量は（Ｃ）を除く全組成物１００重量部に対し、皮膜強度と粘度等の特性バランスから５５〜７５重量部が好ましく、６０〜７０重量部が更に好ましい。 The monofunctional (meth) acrylate monomer (B) used in the present invention is blended to dilute (A) and simultaneously react with (A) to increase the film hardness. From the viewpoints of adhesion to the substrate, moisture permeability, compatibility with (A), etc., it is preferably a monofunctional (meth) acrylate having an aliphatic cyclic group and a hydroxyl group-containing and linear alkyl structure. The blending amount is preferably 55 to 75 parts by weight, more preferably 60 to 70 parts by weight, based on the balance of properties such as film strength and viscosity, with respect to 100 parts by weight of the total composition excluding (C).
脂肪族環式の（メタ）アクリレートとしては、例えばジシクロペンテニル（メタ）アクリレート、ジシクロペンテニルオキシエチル（メタ）アクリレート、イソボルニル（メタ）アクリレート、アダマンタニル（メタ）アクリレート、シクロヘキシル（メタ）アクリレートなどがあげられ、単独または２種類以上を組み合わせて使用できる。これらの中ではイソボルニルアクリレートが、低粘度で皮膚刺激性や臭気の観点から好ましい。 Examples of the aliphatic cyclic (meth) acrylate include dicyclopentenyl (meth) acrylate, dicyclopentenyloxyethyl (meth) acrylate, isobornyl (meth) acrylate, adamantanyl (meth) acrylate, and cyclohexyl (meth) acrylate. Can be used alone or in combination of two or more. Among these, isobornyl acrylate is preferable from the viewpoint of low viscosity and skin irritation and odor.
水酸基を含有する（メタ）アクリレートとしては、例えば２−ヒドロキシエチル（メタ）アクリレート、２‐ヒドロキシプロピル（メタ）アクリレート、３−ヒドロキシプロピル（メタ）アクリレート、４−ヒドロキシブチル（メタ）アクリレート、１，４−シクロヘキサンジメタノールモノアクリレートなどがあげられ、これらの中では安全性や汎用性、柔軟性の観点から４-ヒドロキシブチルアクリレートが好ましい。また直鎖アルキル構造を有する（メタ）アクリレートとしては、例えばメチル（メタ）アクリレート、エチル（メタ）アクリレート、ｎ-プロピル（メタ）アクリレート、ｎ-ブチル（メタ）アクリレート、ｎ-ペンチル（メタ）アクリレート、ｎ-ヘキシル（メタ）アクリレート、ｎ-オクチル（メタ）アクリレート、ラウリル（メタ）アクリレート、トリデシル（メタ）アクリレート、ステアリル（メタ）アクリレートなどがあり、これらの中では汎用性、良希釈性、低臭気、低アウトガスの観点からｎ-オクチルアクリレートが好ましい。 Examples of the (meth) acrylate containing a hydroxyl group include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, 1, 4-cyclohexane dimethanol monoacrylate and the like can be mentioned. Among these, 4-hydroxybutyl acrylate is preferable from the viewpoint of safety, versatility, and flexibility. Examples of the (meth) acrylate having a linear alkyl structure include methyl (meth) acrylate, ethyl (meth) acrylate, n-propyl (meth) acrylate, n-butyl (meth) acrylate, and n-pentyl (meth) acrylate. , N-hexyl (meth) acrylate, n-octyl (meth) acrylate, lauryl (meth) acrylate, tridecyl (meth) acrylate, stearyl (meth) acrylate, etc. Among these, versatility, good dilution, low From the viewpoint of odor and low outgas, n-octyl acrylate is preferred.
本発明で使用される光重合開始剤（Ｃ）は、紫外線や電子線などの吸収でラジカルを生じ、そのラジカルが重合反応のきっかけとなるもので、ＬＥＤの発光波長である３８０ｎｍ以上で吸収帯域をもつ特性が必要である。配合量は（Ａ）成分と（Ｂ）成分の合計１００重量部に対し１０〜１５重量部であり、１０重量部以上とすることで速硬化性を得られ、１５量部以下とすることで長期信頼性を確保できる。 The photopolymerization initiator (C) used in the present invention generates radicals by absorption of ultraviolet rays, electron beams, and the like, and the radicals trigger a polymerization reaction, and has an absorption band at an emission wavelength of 380 nm or more of the LED. The characteristic with is necessary. The blending amount is 10 to 15 parts by weight with respect to 100 parts by weight of the total of component (A) and component (B), and quick curability can be obtained by setting it to 10 parts by weight or more. Long-term reliability can be secured.
３８０ｎｍ以上で吸収帯域をもつ指標としては、アセトニトリルに０．１％溶解した（Ｃ）溶液を分光硬度計で各波長の吸収スペクトルを測定した時の３８０ｎｍにおける吸収量が０．５％以上である事が望ましい。例えば２-ベンジル−２−ジメチルアミノ−１−（４−モルフォリノフェニル）-ブタノン−１、２-ジメチルアミノ−２−（４−メチル-ベンジル）−１−（４−モリフォリン−４−イル−フェニル）−ブタン−１−オン、ビス（２.４.６−トリメチルベンゾイル）−フェニルフォスフィンオキサイド、２.４.６−トリメチルベンゾイル−ジフェニル−フォスフィンオキザイドがあり、単独または２種以上を組み合わせて使用できる。市販品ではＩｒｇａｃｕｒｅ３７９、３７９ＥＧ、３６９および３６９Ｅ、Ｌｕｃｉｒｉｎ ＴＰＯ、Ｄａｒｏｃｕｒ４２６５（商品名：ＢＡＳＦジャパン社製）などがある。 As an index having an absorption band at 380 nm or more, the absorption amount at 380 nm when the absorption spectrum of each wavelength is measured with a spectroscopic hardness meter in a solution (C) 0.1% dissolved in acetonitrile is 0.5% or more. Things are desirable. For example, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) -butanone-1,2-dimethylamino-2- (4-methyl-benzyl) -1- (4-morpholin-4-yl- Phenyl) -butan-1-one, bis (2.4.6-trimethylbenzoyl) -phenylphosphine oxide, 2.4.6-trimethylbenzoyl-diphenyl-phosphine oxazide, alone or in combination Can be used in combination. Examples of commercially available products include Irgacure 379, 379EG, 369 and 369E, Lucirin TPO, Darocur 4265 (trade name: manufactured by BASF Japan).
さらに必要に応じ、光増感剤、酸化防止剤、消泡剤、難燃剤、充填剤、重合禁止剤、着色剤、可塑剤、レベリング剤、分散剤、チクソ付与剤などの添加剤も併用することができる。 If necessary, additives such as photosensitizers, antioxidants, antifoaming agents, flame retardants, fillers, polymerization inhibitors, colorants, plasticizers, leveling agents, dispersants, thixotropic agents are also used in combination. be able to.
光増感剤としては、例えばニトロ系、アンスラキノン系、チオキサントン系、アンスロン系化合物がある。 Examples of the photosensitizer include nitro, anthraquinone, thioxanthone, and anthrone compounds.
以下、本発明を実施例、比較例に基づき詳細に説明するが、具体例を示すものであって特にこれらに限定するものではない。なお表記が無い場合は、室温は２５℃相対湿度６５％の条件下で測定を行った。 EXAMPLES Hereinafter, although this invention is demonstrated in detail based on an Example and a comparative example, a specific example is shown and it does not specifically limit to these. In addition, when there is no description, it measured on the conditions of 25 degreeC relative humidity 65% of room temperature.
実施例１
水添ポリブタジエンジオールから合成された数平均分子量が１，０００〜２０，０００であるウレタンアクリレート（Ａ）としてＥｘｃｅｌａｔｅＲＸ７１−４４（商品名：亜細亜工業社製、数平均分子量３，０００ ）を、単官能 (メタ)アクリレートモノマー（Ｂ）としてＩＢ−ＸＡ（商品名：共栄社化学社製、イソボルニルアクリレート）および４ＨＢＡ（商品名：大阪有機化学工業社製、４ヒドロキシブチルアクリレート）およびＮＯＡＡ（商品名：大阪有機化学工業社製、ｎ−オクチルアクリレート）を、開始剤（Ｃ）としてＩｒｇａｃｕｒｅ３７９ＥＧ（商品名：ＢＡＳＦジャパン社製）を用い、表１記載の配合で均一に溶解するまで撹拌し実施例１の防湿絶縁コート剤組成物を調整した。
Example 1
As a urethane acrylate (A) synthesized from hydrogenated polybutadiene diol having a number average molecular weight of 1,000 to 20,000, Exelate RX71-44 (trade name: manufactured by Asia Industries, number average molecular weight 3,000) is monofunctional. As (meth) acrylate monomer (B), IB-XA (trade name: manufactured by Kyoeisha Chemical Co., Ltd., isobornyl acrylate) and 4HBA (trade name: manufactured by Osaka Organic Chemical Industry Co., Ltd., 4 hydroxybutyl acrylate) and NOAA (trade name: Example 1 of the present invention was stirred until n-octyl acrylate (produced by Osaka Organic Chemical Industry Co., Ltd.) was uniformly dissolved with the formulation shown in Table 1, using Irgacure 379EG (trade name: manufactured by BASF Japan) as the initiator (C). A moisture-proof insulating coating agent composition was prepared.
実施例２〜６
実施例１で用いた材料の他、（Ａ）としてＲＸ７１−６７（商品名：亜細亜工業社製、数平均分子量１３，０００）、（Ｃ）としてＩｒｇａｃｕｒｅ３６９Ｅ（商品名：ＢＡＳＦジャパン社製）を、光増感剤としてＫＡＹＡＣＵＲＥＤＥＴＸ−Ｓ（商品名：日本化薬社製、チオキサントン系）およびカレンズＰＥ１（商品名：昭和電工社製、チオール系）を用い、表１記載の配合で均一に溶解するまで撹拌し実施例２〜６の防湿絶縁コート剤組成物を調整した。
Examples 2-6
In addition to the materials used in Example 1, (A) RX71-67 (trade name: manufactured by Asia Industrial Co., Ltd., number average molecular weight 13,000), (C) as Irgacure 369E (trade name: manufactured by BASF Japan), Using KAYACUREDETX-S (trade name: manufactured by Nippon Kayaku Co., Ltd., thioxanthone series) and Karenz PE1 (trade name: manufactured by Showa Denko Co., Ltd., thiol series) as photosensitizers, until uniformly dissolved with the formulation shown in Table 1 The moisture-proof insulation coating agent composition of Examples 2-6 was prepared by stirring.
比較例１〜７
実施例で用いた材料の他、ポリテトラメチレングリコール骨格のウレタンアクリレートＲＸ８−７（商品名：亜細亜工業社製）を、（Ｂ）としてＡＣＭＯ（商品名：ＫＪケミカルズ社製、アクリロイルモルホリン）を、開始剤としてＩｒｇａｃｕｒｅ１８４（商品名：ＢＡＳＦジャパン社製、３８０ｎｍの波長吸収率が０．１％以下）およびＬｕｃｉｒｉｎＴＰＯ（商品名：ＢＡＳＦジャパン社製）を、２官能の（メタ）アクリレートモノマーとしてライトアクリレートＤＣＰ−Ａ（商品名：共栄社化学社製、ジメチロールトリシクロデカンジアクリレート）を用い、表１記載の配合で均一に溶解するまで撹拌し比較例１〜７の防湿絶縁コート剤組成物を調整した。
Comparative Examples 1-7
In addition to the materials used in the examples, urethane acrylate RX8-7 (trade name: manufactured by Asia Kogyo Co., Ltd.) having a polytetramethylene glycol skeleton and ACMO (trade name: manufactured by KJ Chemicals, acryloylmorpholine) as (B), Irgacure 184 (trade name: manufactured by BASF Japan Ltd.) and Lucirin TPO (trade name: manufactured by BASF Japan Corp.) as initiators and light acrylate DCP as bifunctional (meth) acrylate monomers Using -A (trade name: manufactured by Kyoeisha Chemical Co., Ltd., dimethylol tricyclodecanediacrylate), the moisture-proof insulating coating agent composition of Comparative Examples 1 to 7 was prepared by stirring until it was uniformly dissolved with the formulation shown in Table 1. .
表１
Table 1
評価方法は以下の通りとした。 The evaluation method was as follows.
表面硬化性：ガラス板上に厚さ１００μｍとなるよう防湿絶縁コート剤組成物を塗布し、その上からパナソニック製のＬＥＤ−ＵＶ照射装置ＵＤ−４０を用い、出力４００ｍＷ/ｃｍ２、積算光量が１０００ｍＪ／ｃｍ２となる様に紫外線照射により硬化させ、皮膜表面のべたつき有無を指触で確認し、べたつき無を○、べたつきは有るが樹脂が指に付かないを△、べたつき有で樹脂が指に付くを×とした。 Surface curability: A moisture-proof insulating coating agent composition is applied on a glass plate to a thickness of 100 μm, and an LED-UV irradiation device UD-40 manufactured by Panasonic is used from above, and the output is 400 mW / cm 2 and the integrated light quantity is It is cured by ultraviolet irradiation so that it becomes 1000 mJ / cm 2, and the presence or absence of stickiness on the surface of the film is confirmed by finger touch. The mark attached to was marked with ×.
粘度：東機産業製のコーンプレート型粘度計ＲＣ−５５０を用い、コーン角３°×Ｒ１７．６５で２５±１℃、回転数２０ｒｐｍで測定した。作業性の観点から１，０００ｍＰａ・ｓ未満を○とした、１，０００ｍＰａ・ｓ以上を×とした。 Viscosity: Using a cone plate viscometer RC-550 manufactured by Toki Sangyo Co., Ltd., a cone angle of 3 ° × R17.65 was measured at 25 ± 1 ° C. and a rotation speed of 20 rpm. From the viewpoint of workability, less than 1,000 mPa · s was marked as “◯”, and 1,000 mPa · s or more was marked as “x”.
剥離強度：ガラス板上に厚さ１００μｍとなるよう防湿絶縁コート剤組成物を塗布し、その上に２４ｍｍ幅にカットしたＰＥＴフィルム（商品名、東洋紡製、Ａ４３００、厚み１２５μｍ）を重ね合わせ、その上から同上の条件で紫外線照射して硬化させ、当該ＰＥＴフィルム端部をミネベア製の引張圧縮試験機テクノグラフ ＴＧＩ-１ｋＮを用いて１８０度方向にクロスヘッドスピード３００ｍｍ／分で引張った際の剥離強度を測定し、剥離強度が1．０Ｎ/ｍ以上を○、1．０Ｎ/ｍ未満を×とした。なお紫外線の照射条件は、特別な表記が無い場合は以下も同じとする。 Peel strength: A moisture-proof insulating coating agent composition was applied on a glass plate to a thickness of 100 μm, and a PET film (trade name, manufactured by Toyobo, A4300, thickness 125 μm) cut to a width of 24 mm was superimposed on the glass plate. Peeling when the PET film end is pulled at 180 ° direction at a crosshead speed of 300 mm / min using Minebea's tensile compression tester Technograph TGI-1kN under the same conditions as above. The strength was measured, and a peel strength of not less than 1.0 N / m was marked with ◯, and less than 1.0 N / m was marked with x. The ultraviolet irradiation conditions are the same in the following unless there is a special notation.
耐マイグレーション試験：２５×５０ｍｍの板ガラス上に０．６×１０．２ｍｍのエリアに描画したＩＴＯ電極基板（アノード／カソード間のライン／スペース＝１５／１５μｍ）上に、厚さ１００μｍとなるよう防湿絶縁コート剤を塗布し、同上の条件で紫外線照射して硬化させた試験片を作製し、６０℃／９０％ＲＨの環境下でＤＣ５Ｖを印加し、３００時間経過後の絶縁抵抗変化と腐食性について評価し、目視で腐食無しを○、腐食有りを×とした。 Migration resistance test: Moisture-proof to a thickness of 100 μm on an ITO electrode substrate (line / space between anode / cathode = 15/15 μm) drawn in a 0.6 × 10.2 mm area on a 25 × 50 mm plate glass A test piece was prepared by applying an insulating coating agent and cured by irradiating with ultraviolet rays under the same conditions as above, applying DC5V in an environment of 60 ° C./90% RH, and changing the insulation resistance and corrosiveness after 300 hours. The result was evaluated by visually observing the absence of corrosion as ◯ and the presence of corrosion as x.
評価結果
表２
Evaluation results <br/> Table 2
実施例は表面硬化性、粘度、剥離強度、マイグレーション試験すべての面で問題は無く良好であった。 The examples were satisfactory with no problems in all aspects of surface curability, viscosity, peel strength, and migration test.
一方、開始剤の配合量が１０％未満および請求項３に非該当となる（Ｃ）を一部含む比較例１、２、３、４、５、６は表面硬化性が劣り、（Ａ）の代わりにＰＴＭＧ骨格のウレタンアクリレートを用いた比較例７はマイグレーション試験で腐食が発生し、いずれも本願発明に適さないものであった。 On the other hand, Comparative Examples 1, 2, 3, 4, 5, and 6 including a part of (C) that contains less than 10% of the initiator and (C) not corresponding to claim 3 have poor surface curability, (A) In Comparative Example 7 in which PTMG skeleton urethane acrylate was used instead of corrosion, corrosion occurred in the migration test, and none of them was suitable for the present invention.
本発明は、電子部品を搭載する回路基板で用いられる防湿絶縁コート剤で、照射する光源がＬＥＤの場合でも短時間に硬化可能で、絶縁信頼性に優れた組成物として有用である。
INDUSTRIAL APPLICABILITY The present invention is a moisture-proof insulating coating agent used for circuit boards on which electronic components are mounted, and can be cured in a short time even when the light source to be irradiated is an LED, and is useful as a composition having excellent insulation reliability.
Claims (4)
A mounting circuit board that is insulated using the LED curable moisture-proof insulating coating composition according to claim 1.
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| JP2020158674A (en) * | 2019-03-27 | 2020-10-01 | アイカ工業株式会社 | Resin composition of ultraviolet curable insulating coating agent |
| JP2021091850A (en) * | 2019-12-03 | 2021-06-17 | アイカ工業株式会社 | Ultraviolet curable resin composition |
| WO2023101497A1 (en) * | 2021-12-03 | 2023-06-08 | 주식회사 동진쎄미켐 | Curable composition and display device including dam structure fabricated therefrom |
| CN117004311A (en) * | 2023-06-06 | 2023-11-07 | 德阳展源新材料科技有限公司 | UV photo-moisture curing three-proofing paint and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2020158674A (en) * | 2019-03-27 | 2020-10-01 | アイカ工業株式会社 | Resin composition of ultraviolet curable insulating coating agent |
| JP7245096B2 (en) | 2019-03-27 | 2023-03-23 | アイカ工業株式会社 | UV curable insulating coating agent resin composition |
| JP2021091850A (en) * | 2019-12-03 | 2021-06-17 | アイカ工業株式会社 | Ultraviolet curable resin composition |
| JP7448390B2 (en) | 2019-12-03 | 2024-03-12 | アイカ工業株式会社 | UV curable resin composition |
| WO2023101497A1 (en) * | 2021-12-03 | 2023-06-08 | 주식회사 동진쎄미켐 | Curable composition and display device including dam structure fabricated therefrom |
| CN117004311A (en) * | 2023-06-06 | 2023-11-07 | 德阳展源新材料科技有限公司 | UV photo-moisture curing three-proofing paint and preparation method thereof |
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