JP7289019B2 - 窒化ホウ素粉末及び樹脂組成物 - Google Patents
窒化ホウ素粉末及び樹脂組成物 Download PDFInfo
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- JP7289019B2 JP7289019B2 JP2022575455A JP2022575455A JP7289019B2 JP 7289019 B2 JP7289019 B2 JP 7289019B2 JP 2022575455 A JP2022575455 A JP 2022575455A JP 2022575455 A JP2022575455 A JP 2022575455A JP 7289019 B2 JP7289019 B2 JP 7289019B2
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- boron nitride
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- nitride powder
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims description 157
- 229910052582 BN Inorganic materials 0.000 title claims description 155
- 239000000843 powder Substances 0.000 title claims description 83
- 239000011342 resin composition Substances 0.000 title claims description 22
- 239000002245 particle Substances 0.000 claims description 87
- 229920005989 resin Polymers 0.000 claims description 31
- 239000011347 resin Substances 0.000 claims description 31
- 239000011148 porous material Substances 0.000 claims description 19
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 28
- 239000000463 material Substances 0.000 description 26
- 229910052796 boron Inorganic materials 0.000 description 23
- 238000005121 nitriding Methods 0.000 description 23
- 238000005259 measurement Methods 0.000 description 22
- 229910052580 B4C Inorganic materials 0.000 description 21
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- 238000010438 heat treatment Methods 0.000 description 15
- 239000000203 mixture Substances 0.000 description 12
- 238000001878 scanning electron micrograph Methods 0.000 description 12
- 238000011049 filling Methods 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 10
- 229910001873 dinitrogen Inorganic materials 0.000 description 10
- 238000005261 decarburization Methods 0.000 description 9
- 230000017525 heat dissipation Effects 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000002156 mixing Methods 0.000 description 7
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- 238000000034 method Methods 0.000 description 6
- 229920000647 polyepoxide Polymers 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- -1 fluororesins Polymers 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 5
- 239000003607 modifier Substances 0.000 description 5
- 238000010298 pulverizing process Methods 0.000 description 5
- 238000004435 EPR spectroscopy Methods 0.000 description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 4
- 239000004327 boric acid Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000001965 increasing effect Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000012546 transfer Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 description 2
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 2
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 description 2
- 229910052810 boron oxide Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 2
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- 238000009736 wetting Methods 0.000 description 2
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- ZQXCQTAELHSNAT-UHFFFAOYSA-N 1-chloro-3-nitro-5-(trifluoromethyl)benzene Chemical compound [O-][N+](=O)C1=CC(Cl)=CC(C(F)(F)F)=C1 ZQXCQTAELHSNAT-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
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- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 description 1
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- UUQQGGWZVKUCBD-UHFFFAOYSA-N [4-(hydroxymethyl)-2-phenyl-1h-imidazol-5-yl]methanol Chemical compound N1C(CO)=C(CO)N=C1C1=CC=CC=C1 UUQQGGWZVKUCBD-UHFFFAOYSA-N 0.000 description 1
- PPWPWBNSKBDSPK-UHFFFAOYSA-N [B].[C] Chemical compound [B].[C] PPWPWBNSKBDSPK-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229920006243 acrylic copolymer Polymers 0.000 description 1
- 229920000800 acrylic rubber Polymers 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
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- 229920001400 block copolymer Polymers 0.000 description 1
- HVABKWYVQHSGHW-UHFFFAOYSA-N boron;ethanamine Chemical compound [B].CCN HVABKWYVQHSGHW-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 150000001733 carboxylic acid esters Chemical class 0.000 description 1
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- 238000001035 drying Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- GOAJGXULHASQGJ-UHFFFAOYSA-N ethene;prop-2-enenitrile Chemical group C=C.C=CC#N GOAJGXULHASQGJ-UHFFFAOYSA-N 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 125000005647 linker group Chemical group 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
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- 229920003986 novolac Polymers 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920001955 polyphenylene ether Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
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- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/38—Boron-containing compounds
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0646—Preparation by pyrolysis of boron and nitrogen containing compounds
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
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Description
[測定条件]
磁場掃引範囲:0~3290gauss(0~329mT)
磁場変調:5gauss(0.5mT)
時定数:0.3s
照射電磁波:0.5mW、約9.16GHz(照射電磁波の周波数は、共鳴周波数となるように測定ごとに微調整する)
掃引時間:15min
アンプゲイン:200
Mnマーカー:750
測定環境:室温(25℃)
標準試料:日本電子社製Coal標準試料(スピン量:3.56×1013個/g)
平均粒子径55μmの炭化ホウ素粒子をカーボンルツボに充填し、カーボンルツボを窒素ガス雰囲気下で、2000℃、0.8MPaの条件で20時間加熱することにより炭窒化ホウ素粒子を得た。得られた炭窒化ホウ素粒子100質量部と、ホウ酸66.7質量部とをヘンシェルミキサーを用いて混合し、混合物中の炭窒化ホウ素1molに対して、ホウ素源のホウ素原子の量が1.2molである混合物を得た。得られた混合物を窒化ホウ素ルツボに充填し、ルツボに蓋をして、ルツボと蓋との隙間の全てにエポキシ樹脂を充填した。混合物を充填した窒化ホウ素ルツボを抵抗加熱炉内に配置したカーボンケース内で、常圧、窒素ガス雰囲気下、保持温度2000℃の条件で10時間加熱することにより、粗大な窒化ホウ素粒子を得た。得られた粗大な窒化ホウ素粒子を乳鉢により10分間解砕し、篩目109μmのナイロン篩にて分級を行って、窒化ホウ素粒子(窒化ホウ素粉末)を得た。
混合物中の炭窒化ホウ素1molに対して、ホウ素源のホウ素原子の量が1.4molとなるようにホウ酸の量を変更した以外は、実施例1と同様の条件で窒化ホウ素粒子(窒化ホウ素粉末)を得た。得られた窒化ホウ素粒子の断面をSEMで確認したところ、複数の窒化ホウ素片同士が化学的に結合していることが確認された。
混合物中の炭窒化ホウ素1molに対して、ホウ素源のホウ素原子の量が1.6molとなるようにホウ酸の量を変更した以外は、実施例1と同様の条件で窒化ホウ素粒子(窒化ホウ素粉末)を得た。得られた窒化ホウ素粒子の断面をSEMで確認したところ、複数の窒化ホウ素片同士が化学的に結合していることが確認された。
混合物中の炭窒化ホウ素1molに対して、ホウ素源のホウ素原子の量が1.8molとなるようにホウ酸の量を変更した以外は、実施例1と同様の条件で窒化ホウ素粒子(窒化ホウ素粉末)を得た。得られた窒化ホウ素粒子の断面をSEMで確認したところ、複数の窒化ホウ素片同士が化学的に結合していることが確認された。
混合物中の炭窒化ホウ素1molに対して、ホウ素源のホウ素原子の量が1.1molとなるようにホウ酸の量を変更した以外は、実施例1と同様の条件で窒化ホウ素粒子(窒化ホウ素粉末)を得た。
混合物中の炭窒化ホウ素1molに対して、ホウ素源のホウ素原子の量が2.7molとなるようにホウ酸の量を変更した以外は、実施例1と同様の条件で窒化ホウ素粒子(窒化ホウ素粉末)を得た。
ベックマンコールター製レーザー回折散乱法粒度分布測定装置(LS-13 320)を用いて、窒化ホウ素粉末の平均粒子径を測定した。平均粒子径の測定結果を表1に示す。
JIS R 1655:2003に準拠して水銀ポロシメーター(株式会社島津製作所製、オートポアIV9500)によって窒化ホウ素粉末の平均細孔径を測定した。測定結果を表1に示す。
JIS Z 8830:2013に準拠して窒素ガスを使用してBET多点法により窒化ホウ素粉末のBET比表面積を測定した。測定結果を表1に示す。
走査型電子顕微鏡(日本電子株式会社製、JSM-7001F)を用いて、観察倍率10000倍で、窒化ホウ素粒子の表面を観察した。得られた窒化ホウ素粉末中の窒化ホウ素粒子の表面のSEM画像を画像解析ソフトウェア(株式会社マウンテック製、Mac-view)に取り込み、窒化ホウ素粒子の表面に配置されている窒化ホウ素片の厚さ及び長径(厚さ方向に対して垂直方向の最大長さ)を測定した。40個の窒化ホウ素片の厚さ及び長径をそれぞれ測定し、測定した厚さ及び長径から窒化ホウ素粒子を構成する窒化ホウ素片の平均厚さ及び平均長径を算出した。また、測定した厚さ及び長径から各窒化ホウ素片のアスペクト比(長径/厚さ)を算出し、40個の窒化ホウ素片のアスペクト比から平均アスペクト比を算出した。平均厚さ、平均長径及び平均アスペクト比の算出結果を表1に示す。実施例1及び比較例1の窒化ホウ素粒子の表面のSEM画像を図2及び3にそれぞれ示す。
得られた各窒化ホウ素粉末中の20個の窒化ホウ素粒子について、JIS R 1639-5:2007に準拠して圧壊強度を測定した。測定装置としては、微小圧縮試験機(島津製作所社製、MCT-211)を用いた。各窒化ホウ素粒子の圧壊強度σ(単位:MPa)は、粒子内の位置によって変化する無次元数α(=2.48)と圧壊試験力P(単位:N)と平均粒子径d(単位:μm)から、σ=α×P/(π×d2)の式を用いて算出した。20個の窒化ホウ素粒子について圧壊強度を測定し、その平均値を表1に示す。
ナフタレン型エポキシ樹脂(DIC社製、HP4032)100質量部と、硬化剤としてイミダゾール化合物(四国化成社製、2E4MZ-CN)10質量部とを混合し、次いで、各実施例及び比較例において得られた窒化ホウ素粉末81質量部を更に混合して樹脂組成物を得た。この樹脂組成物を、500Paの減圧脱泡を10分間行い、PET製シート上に厚みが1.0mmになるように塗布した。その後、温度150℃、圧力160kg/cm2条件で60分間のプレス加熱加圧を行って、0.5mmのシート状の放熱材を作製した。作製した放熱材から10mm×10mmの大きさの測定用試料を切り出し、キセノンフラッシュアナライザ(NETZSCH社製、LFA447NanoFlash)を用いたレーザーフラッシュ法により、測定用試料の熱拡散率A(m2/秒)を測定した。また、測定用試料の比重B(kg/m3)をアルキメデス法により測定した。また、測定用試料の比熱容量C(J/(kg・K))を、示差走査熱量計(株式会社リガク製、ThermoPlusEvoDSC8230)を用いて測定した。これらの各物性値を用いて、熱伝導率H(W/(m・K))をH=A×B×Cの式から求めた。熱伝導率の測定結果を表1に示す。実施例1及び比較例1の窒化ホウ素粉末を用いて作製した放熱材の断面のSEM画像を図4及び5にそれぞれ示す。
Claims (4)
- 窒化ホウ素粒子の集合体である窒化ホウ素粉末であって、
BET比表面積が5.7m2/g以上12.0m2/g以下であり、平均細孔径が0.10μm以上0.40μm以下である、窒化ホウ素粉末。 - 前記窒化ホウ素粒子が複数の窒化ホウ素片により構成されており、前記複数の窒化ホウ素片同士が化学的に結合している、請求項1に記載の窒化ホウ素粉末。
- 圧壊強度の平均値が8MPa以上である、請求項1又は2に記載の窒化ホウ素粉末。
- 請求項1~3のいずれか一項に記載の窒化ホウ素粉末と、樹脂とを含有する、樹脂組成物。
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