JP5923851B2 - ペースト組成物およびそれを用いた磁性体組成物 - Google Patents
ペースト組成物およびそれを用いた磁性体組成物 Download PDFInfo
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- JP5923851B2 JP5923851B2 JP2010274325A JP2010274325A JP5923851B2 JP 5923851 B2 JP5923851 B2 JP 5923851B2 JP 2010274325 A JP2010274325 A JP 2010274325A JP 2010274325 A JP2010274325 A JP 2010274325A JP 5923851 B2 JP5923851 B2 JP 5923851B2
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
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- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
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- UFDGMXHPQNDESO-UHFFFAOYSA-N methyl n-(4-aminophenyl)carbamate Chemical compound COC(=O)NC1=CC=C(N)C=C1 UFDGMXHPQNDESO-UHFFFAOYSA-N 0.000 description 1
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- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
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- PCILLCXFKWDRMK-UHFFFAOYSA-N naphthalene-1,4-diol Chemical compound C1=CC=C2C(O)=CC=C(O)C2=C1 PCILLCXFKWDRMK-UHFFFAOYSA-N 0.000 description 1
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- PSZYNBSKGUBXEH-UHFFFAOYSA-N naphthalene-1-sulfonic acid Chemical compound C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-N 0.000 description 1
- JRNGUTKWMSBIBF-UHFFFAOYSA-N naphthalene-2,3-diol Chemical compound C1=CC=C2C=C(O)C(O)=CC2=C1 JRNGUTKWMSBIBF-UHFFFAOYSA-N 0.000 description 1
- MNZMMCVIXORAQL-UHFFFAOYSA-N naphthalene-2,6-diol Chemical compound C1=C(O)C=CC2=CC(O)=CC=C21 MNZMMCVIXORAQL-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
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- JFNLZVQOOSMTJK-KNVOCYPGSA-N norbornene Chemical compound C1[C@@H]2CC[C@H]1C=C2 JFNLZVQOOSMTJK-KNVOCYPGSA-N 0.000 description 1
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- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
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- 239000008188 pellet Substances 0.000 description 1
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
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- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
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- 229940033623 potassium lauryl phosphate Drugs 0.000 description 1
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- ANBFRLKBEIFNQU-UHFFFAOYSA-M potassium;octadecanoate Chemical class [K+].CCCCCCCCCCCCCCCCCC([O-])=O ANBFRLKBEIFNQU-UHFFFAOYSA-M 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
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- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical class [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 1
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- WFRKJMRGXGWHBM-UHFFFAOYSA-M sodium;octyl sulfate Chemical class [Na+].CCCCCCCCOS([O-])(=O)=O WFRKJMRGXGWHBM-UHFFFAOYSA-M 0.000 description 1
- SMECTXYFLVLAJE-UHFFFAOYSA-M sodium;pentadecyl sulfate Chemical class [Na+].CCCCCCCCCCCCCCCOS([O-])(=O)=O SMECTXYFLVLAJE-UHFFFAOYSA-M 0.000 description 1
- UPUIQOIQVMNQAP-UHFFFAOYSA-M sodium;tetradecyl sulfate Chemical class [Na+].CCCCCCCCCCCCCCOS([O-])(=O)=O UPUIQOIQVMNQAP-UHFFFAOYSA-M 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
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- 238000004528 spin coating Methods 0.000 description 1
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- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- BSYVTEYKTMYBMK-UHFFFAOYSA-N tetrahydrofurfuryl alcohol Chemical compound OCC1CCCO1 BSYVTEYKTMYBMK-UHFFFAOYSA-N 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
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- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
- TUQOTMZNTHZOKS-UHFFFAOYSA-N tributylphosphine Chemical compound CCCCP(CCCC)CCCC TUQOTMZNTHZOKS-UHFFFAOYSA-N 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 1
- 229940078499 tricalcium phosphate Drugs 0.000 description 1
- 235000019731 tricalcium phosphate Nutrition 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- 125000004953 trihalomethyl group Chemical group 0.000 description 1
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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- 239000000080 wetting agent Substances 0.000 description 1
- 125000002256 xylenyl group Chemical class C1(C(C=CC=C1)C)(C)* 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
Landscapes
- Hard Magnetic Materials (AREA)
- Soft Magnetic Materials (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
Description
作製したコア−シェル構造粒子をH−7100FA((株)日立製作所製)を用いてTEM観察を行い、100nmが実測で5cmとなるまで拡大した(50万倍)。この状態で、測定対象としたいコア−シェル構造粒子について10箇所のシェルの厚さを測定し、最大値と最小値を除いた8つの値の平均値をシェルの平均厚さとした。なお、粒子同士がシェル樹脂を介して接触している場合には、接触している部分については測定個所には含めなかった。
まず、ペースト組成物をCr膜付きシリコン基板上に塗布した後、熱風オーブン炉で60℃で30分乾燥した。次いで、イナートオーブン“INL−60”(商品名、光洋サーモシステム(株)製)を用いて大気雰囲気下、各実施例および比較例記載の温度で1時間加熱処理し、磁性体組成物を得、さらに、磁性体組成物の上に、Au電極(電極面積1cm2)を蒸着した。Au電極とCr膜付きシリコン基板間で、DC電圧5Vを印加し、その時得られた抵抗値と磁性体組成物の膜厚から、体積抵抗率を求めた。体積抵抗率は、“絶縁抵抗計6517A”(商品名、ケースレーインスツルメンツ(株)製)を用いて測定した。磁性体組成物の膜厚は、サンプル断面のSEM(走査型電子顕微鏡)観察から測定した。
まず、ガラス基板上にペースト組成物を塗布した後、熱風オーブン炉で60℃で30分乾燥した。次いで、イナートオーブン“INL−60”(商品名、光洋サーモシステム(株)製)を用いて大気雰囲気下、各実施例および比較例記載の温度で1時間加熱処理し、磁性体組成物を得た。磁性体組成物の膜厚は100μmであった。その磁性体組成物を5mm角にカットした後、そのサンプルを高周波薄膜透磁率測定装置((株)東栄科学産業製)に入れて、透磁率測定を行った。測定は、その薄膜試料をコイル中に配置し、コイル近傍のストリップ線路からコイルに磁束が鎖交するように10M〜2GHzまでの交流磁界をかけ、ネットワークアナライザーでSパラメータの伝達係数S21を測定し、試料をコイル中に配置しない場合と比べてS21がどの程度変化するかによって透磁率を求めた。また、透磁率の補正には、測定で得られた伝達係数S11、S22等を用いた。
透磁率は、μ=μ’+iμ”(μ’:実部、μ”:虚部)で表され、各実施例における透磁率はμ’の値を、また、tanδは、μ”/ μ’の値を記載した。なお、各実施例においては、1GHzでの値を代表して示した。
<膜観察>
上述の透磁率測定で利用した5mm角のサンプルの断面を1万倍でSEM観察し、コア−シェル構造粒子と樹脂との濡れ性を評価した。コア−シェル構造粒子と樹脂が接触している箇所を観察し、その箇所において濡れている(分離していない)場合を○とし、分離している場合を×とした。
塗膜の膜厚は、塗膜と基板の段差をサーフコム1400(東京精密(株)製)を用いて触針法により測定することで求めた。
<マトリックス樹脂II>オグゾールEG250(商品名、大阪ガスケミカル(株)製、フルオレン骨格を有する液状エポキシ樹脂)
<マトリックス樹脂III>HP7200H(商品名、DIC(株)製、ジシクロペンタジエン型エポキシ樹脂)
<マトリックス樹脂IV>157S70(商品名、三菱化学(株)製、エポキシ樹脂)
<マトリックス樹脂V>EP828US(商品名、三菱化学(株)製、エポキシ樹脂)。
<硬化剤II>4,4’−ジヒドロキシジフェニルスルホン
<硬化剤III>ビスフェノールA(商品名、東京化成工業(株)製)
<硬化剤IV>NV203R4(商品名、大阪ガスケミカル(株)製)
<硬化剤V>KAYAHARD KTG105(商品名、日本化薬(株)製)
<硬化剤VI>2PZ(商品名、四国化成工業(株)製)
<硬化剤VII>2P4MZ(商品名、四国化成工業(株)製)
硬化剤I〜Vはフェノール系硬化剤であり、硬化剤VI、VIIはアミン系硬化剤である。
<磁性体無機粒子II>HS粉(商品名、BASF製カルボニル鉄粉末、平均粒子径2.1μm)
<磁性体無機粒子III>OM粉(商品名、BASF製カルボニル鉄粉末、平均粒子径4μm)。
<樹脂モノマーII>ニカレヂンS−176(商品名、日本カーバイド工業(株)、メチロール基を有するメラミン樹脂モノマー)
<樹脂モノマーIII>26DMPC(商品名、旭有機材工業(株)、メチロール基を有するフェノール樹脂モノマー)。
<界面活性剤II>ラウリル硫酸ナトリウム(和光純薬工業(株)製)
<界面活性剤III>ステアリン酸ナトリウム(和光純薬工業(株)製)。
<シランカップリング剤II>KBM903(商品名、信越シリコーン(株)製、3−アミノプロピルトリメトキシシラン)。
<溶媒II>N,N−ジメチルアセトアミド(三菱ガス化学(株)製、沸点165℃)
<溶媒III>乳酸エチル(和光純薬工業(株)製、沸点155℃)
<溶媒IV>プロピレングリコールモノメチルエーテルアセテート(和光純薬工業(株)製、沸点146℃)
<溶媒V>1−エトキシ−2−プロパノール(和光純薬工業(株)製、沸点132℃)
<溶媒VI>1,4−ジオキサン(東邦化学工業(株)製、沸点101℃)
<溶媒VII>プロピレングリコールジメチルエーテル(東邦化学工業(株)製、沸点97℃)
実施例1
まず、磁性体無機粒子I 28g、純水を300g、トレセラムφ0.4mm(商品名、東レ(株)製ジルコニアビーズ)500g、界面活性剤I 14gを混合し、ボールミルで、回転数170rpmで30分粉砕を行った。その後、得られた磁性体無機粒子分散液の濾過を行い、ビーズを除去した。濾過にはメッシュフィルターを利用した。また、別途、エチレングリコール42gに樹脂モノマーI 6gを、超音波を用いて溶解させ、それを濾過して得られた樹脂モノマー溶液を作製した。
表1に示すように、硬化剤の種類を変えた以外は実施例1と同様の組成のペースト組成物を作製し、上述の方法に従って、体積抵抗率と透磁率、膜観察の評価を行った。その結果を表1に示した。フェノール系の硬化剤を用いた場合、絶縁性磁性体材料として優れた性能を示すだけでなく、コア−シェル構造粒子と樹脂の濡れ性も良好であることがわかる。
表1に示すように、マトリックス樹脂の種類を変えた以外は実施例1と同様の組成のペースト組成物を作製し、上述の方法に従って、体積抵抗率と透磁率、膜観察の評価を行った。その結果を表1に示した。
表1に示すように、磁性体無機粒子、シェルを構成する樹脂のモノマー、または分散時に用いる界面活性剤の種類を変えた以外は実施例1と同様の組成のコア−シェル構造粒子を用いたペースト組成物を作製し、上述の方法に従って、体積抵抗率と透磁率、膜観察の評価を行った。その結果を表1に示した。平均粒子径が3μm以下の無機粒子を用いた場合、透磁率が大きくてもtanδを小さく保てることがわかる。また、界面活性剤としてスチレンマレイン酸樹脂アンモニウムを用いた場合、コア−シェル構造粒子のシェル厚みが厚くなり、磁性体組成物の体積抵抗率が大きくなることがわかる。
まず、磁性体無機粒子I 28g、純水を300g、トレセラムφ0.4mm(商品名、東レ(株)製ジルコニアビーズ)500g、シランカップリング剤I 3gを混合し、ボールミルで、回転数170rpmで60分粉砕を行った。その後、得られた磁性体無機粒子分散液の濾過を行い、ビーズを除去した。濾過にはメッシュフィルターを利用した。得られた濾物を熱風オーブン炉で110℃1時間乾燥させ、シランカップリング剤で処理した磁性体無機粒子を25g得た。
表1に示すように、溶媒の種類を変えた以外は実施例1と同様の組成のペースト組成物を作製し、上述の方法に従って、体積抵抗率と透磁率、膜観察の評価を行った。その結果を表1に示した。沸点が150℃以上の溶媒を使用する場合に特に透磁率が大きくなり、tanδも小さく保つことができることがわかる。
表1に示すように、ペースト組成物中の固形成分に対するコア−シェル構造粒子の含有量を変えた以外は実施例1と同様の組成のペースト組成物を作製し、上述の方法に従って、体積抵抗率と透磁率、膜観察の評価を行った。その結果を表1に示した。コア−シェル構造粒子の含有量が多いほど透磁率が大きくなることがわかる。なお、後述の比較例3〜5との対比により、コア−シェル構造粒子の含有量が少ない場合でも、沸点が120℃以上の溶媒を使用することにより透磁率が相対的に大きくなる一方でtanδは小さく保てていることがわかる。
表1に示すように、実施例1と同様の組成のペースト組成物を作製し、ペースト組成物のキュア温度を変えた以外は実施例1と同様の方法で磁性体組成物を作製した。上述の方法に従って、体積抵抗率と透磁率、膜観察の評価を行った。その結果を表1に示した。
表2に示すように、溶媒の種類を変えた以外は実施例1と同様の組成のペースト組成物を作製し、上述の方法に従って、体積抵抗率と透磁率、膜観察の評価を行った。その結果を表2に示した。実施例1と対比して、沸点が120℃未満の溶媒を使用することにより透磁率が小さくなる一方でtanδが大きくなった。
表2に示すように、ペースト組成物中の固形成分に対するコア−シェル構造粒子の含有量を変えた以外は実施例1と同様の組成のペースト組成物を作製し、上述の方法に従って、体積抵抗率と透磁率、膜観察の評価を行った。その結果を表2に示した。実施例24〜26と対比して、沸点が120℃未満の溶媒を使用することにより透磁率が小さくなる一方でtanδが大きくなった。
Claims (9)
- 磁性体無機粒子をコアとするコア−シェル構造粒子、マトリックス樹脂、および120℃以上の沸点を有する溶媒を含み、前記コア−シェル構造粒子のシェルとして、メラミン樹脂を有することを特徴とするペースト組成物。
- 前記マトリックス樹脂がエポキシ樹脂である請求項1記載のペースト組成物。
- さらに硬化剤を含む請求項1または2記載のペースト組成物。
- 前記硬化剤がフェノール系化合物である請求項3記載のペースト組成物。
- 前記溶媒が、150℃以上の沸点を有する溶媒を含む請求項1〜4のいずれかに記載のペースト組成物。
- 前記磁性体無機粒子の平均粒子径が3μm以下である請求項1〜5のいずれかに記載のペースト組成物。
- 請求項1〜6のいずれかに記載のペースト組成物を塗布し、熱処理する工程を含む磁性体組成物の製造方法。
- ペースト組成物の熱処理が230℃以下での加熱処理である請求項7記載の磁性体組成物の製造方法。
- 前記磁性体組成物の体積抵抗率が1×1010Ωcm以上である請求項7または8記載の磁性体組成物の製造方法。
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