JP2006527649A - マイクロ波付着による金属酸化物コーティド有機材料の製造方法 - Google Patents
マイクロ波付着による金属酸化物コーティド有機材料の製造方法 Download PDFInfo
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- JP2006527649A JP2006527649A JP2006516134A JP2006516134A JP2006527649A JP 2006527649 A JP2006527649 A JP 2006527649A JP 2006516134 A JP2006516134 A JP 2006516134A JP 2006516134 A JP2006516134 A JP 2006516134A JP 2006527649 A JP2006527649 A JP 2006527649A
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Abstract
Description
(a)有機基材をフッ素スカベンジャーの水溶液中に懸濁させ;
(b)所望の金属酸化物コーティングの前駆材料であるフッ素含有金属複合体の一種以上の水溶液を加え;及び
(c)該懸濁液にマイクロ波放射を施して該有機材料に金属酸化物を付着させる
を含み、ここで、工程(b)及び(c)を、場合により異なるフッ素含有金属複合体を用いて繰り返して1つ以上の金属酸化物層を生成することができる。
(a)可溶性のフッ化金属塩、
(b)可溶性のフッ化金属複合体、或は
(c)該塩又は複合体を形成する任意の混合物。
そして、(g)該懸濁液にマイクロ波放射を施して該有機材料に金属酸化物を付着させる。
(f’)所望の金属酸化物コーティングの前駆材料であるフッ素含有金属複合体の一種以上の水溶液を加え;及び
(g’)該懸濁液にマイクロ波放射を施して該有機材料に金属酸化物を付着させる。
A)屈折率n£1.8を有する無色のコーティング、及び
B)屈折率n£2.0を有する無色のコーティング
を含む層パケットを少なくとも1つ含む。
(A)屈折率n>1.65を有するコーティング、
(B)屈折率n£1.65を有するコーティング、
(C)屈折率n>1.65を有するコーティング、及び
(D)場合により、外部保護層。
1.5cm×1.5cmポリカーボネートシートの片をエタノール及び脱イオン水でそれぞれすすぎ洗いする。次いで、それを11mlホウ酸水溶液(0.2M、2.2mモル)中に浸漬する。初めに、ヘキサフルオロ第二スズ酸アンモニウム溶液(0.1M、0.1mモル)を加え、マイクロ波オーブン中での反応をパワーレベル1で1分間実施する。混合物を30分間静置して冷却させる。第二に、ヘキサフルオロチタン酸アンモニウム溶液(0.1M、0.1mモル)を加え、マイクロ波処理(パワーレベル1で1分間)を10分間隔で5回繰り返す。ポリカーボネートシートを反応混合物から取り出しそして水及びエタノールですすぎ洗いする。
a)ポリメチルメタクリレート(1.2重量%)の2mlトルエン溶液及びアセトン2mlを、一端をシールさせたガラス管に加える。管は、直径6.0cm及び長さ28.0cmを有する。管を20トル真空に接続しそしてそれを30分間水平に回転させることによって、PMMAのコーティングが内壁上に形成する。脱イオン水10mlを使用してPMMAをすすぎ洗いして落とす。PMMAのフレークがろ過によって収集される。
例2a)からの生成物0.3gをトルエン10ml中に浸漬し、60℃に5分間加熱する。得られたFe2O3フレークを3時間沈降させ、次いでろ過し、アセトンですすぎ洗いする。Fe2O3フレークは、赤/黄色みがかった色を示す。
例2a)の方法で作製したポリメチルメタクリレートフレーク0.1gに、脱イオン水50mlを加える。混合物を20分間音波処理し、Teflonビーカーに移す。攪拌した混合物に、FeCl3・4NH5Fの0.4M水溶液5ml及び0.8Mホウ酸水溶液5mlを同時に0.2ml/分で加える。マイクロ波照射で、温度を50℃に上昇させて30分間保つ。次いで、0.4Mヘキサフルオロチタン酸アンモニウム5ml及び0.8Mホウ酸水溶液5mlを同時に0.4ml/分で加える。更に30分マイクロ波照射した後に、反応混合物を冷却させて室温にする。FeCl3・4NH5Fの0.4M水溶液5ml及び0.8Mホウ酸水溶液5mlによる酸化鉄のコーティングプロセスを繰り返す。粉末0.5gがろ過によって収集され、真空オーブン中で12時間乾燥させる。
例4からのフレーク0.4gをトルエン10ml中に浸漬し、60℃に5分間加熱する。得られたTiO2/Fe2O3/TiO2フレークを3時間沈降させ、次いでろ過し、アセトンですすぎ洗いする。TiO2/Fe2O3/TiO2フレークは、緑/黄色みがかった色を示す。
Claims (15)
- 有機基材及び周期表の3〜15族からなる群より選択する金属の一種以上の酸化物からなる少なくとも1つの誘電体層を含む有機材料を製造する方法であって、下記の工程:
(a)有機基材をフッ素スカベンジャーの水溶液中に懸濁させ;
(b)所望の金属酸化物コーティングの前駆材料であるフッ素含有金属複合体の一種以上の水溶液を加え;及び
(c)該懸濁液にマイクロ波放射を施して該有機材料に金属酸化物を付着させる
を含み、工程(b)及び(c)を、場合により異なるフッ素含有金属複合体を用いて繰り返して1つ以上の金属酸化物層を又は厚さ方向に二種の異なる金属酸化物の濃度の勾配を生成することができる有機材料を製造する方法。 - フッ素スカベンジャーを、ホウ酸、アルカリ金属ホウ酸塩、特にホウ酸ナトリウム、ホウ酸アンモニウム、ホウ素無水物及び一酸化ホウ素からなる群より選択する、請求項1記載の方法。
- フッ素含有金属複合体を、ヘキサフルオロチタン酸アンモニウム;ヘキサフルオロ第二スズ酸アンモニウム;ヘキサフルオロケイ酸アンモニウム;塩化鉄(III)、フッ化水素酸及びフッ化アンモニウムの混合物;塩化アルミニウム(III)、フッ化水素酸及びフッ化アンモニウム混の合物;ヘキサフルオロゲルマニウム酸アンモニウム;フッ化インジウム(III)、フッ化水素酸及びフッ化アンモニウムの混合物;並びにフッ化インジウム(III)三水和物とヘキサフルオロ第二スズ酸アンモニウムとの組合せからなる群より選択する、請求項1記載の方法。
- 反応媒体の凝固点と沸点との間、特に約15℃〜約95℃の間の温度で実施する、請求項1記載の方法。
- 金属酸化物が二酸化チタンであり、フッ素含有金属複合体を、ヘキサフルオロチタン酸アンモニウム、フッ化アンモニウム及び塩化チタン又は塩化チタン、フッ化アンモニウム及びフッ化水素から調製する複合体からなる群より選択し、或は金属酸化物が酸化鉄であり、フッ素含有金属複合体を、塩化鉄(III)、フッ化水素酸及びフッ化アンモニウム混合物からなる群より選択する、請求項1記載の方法。
- 金属酸化物が二酸化ケイ素であり、フッ素含有金属複合体がヘキサフルオロケイ酸アンモニウム又はペンタフルオロケイ酸アンモニウムである、請求項1記載の方法。
- 有機基材を、ポリカーボネート、ポリアミド、ポリエチレン、ポリエチレンテレフタレート、ポリメチルメタクリレート(PMMA)、エポキシ樹脂、ABS(アクリロニトリル/ブタジエン/スチレン)、ポリオレフィンマトリックスからなる群より選択する、請求項1記載の方法。
- 更に、下記の工程:
(d)工程(b)における酸化物コーティングと異なる所望の金属酸化物コーティングの前駆材料であるフッ素含有金属複合体の一種以上の水溶液を加え;及び
(e)該懸濁液にマイクロ波放射を施してコーテッド有機基材に金属酸化物を付着させる
を含む請求項1記載の方法。 - 有機基材がポリカーボネートであり、フッ素含有金属複合体がヘキサフルオロチタン酸アンモニウム、又はフルオロケイ酸アンモニウム塩である、請求項1記載の方法。
- 有機基材がポリカーボネートであり、工程(b)のフッ素含有金属複合体がヘキサフルオロチタン酸アンモニウム、工程(d)のフッ素含有金属複合体がフルオロケイ酸アンモニウム塩である、請求項8記載の方法。
- 有機基材がPMMAの板又は板様PMMAであり、工程(b)のフッ素含有金属複合体がヘキサフルオロチタン酸アンモニウム、フルオロケイ酸アンモニウム塩、又は塩化鉄(III)/フッ化アンモニウムであり、更に(d’) PMMAを有機液体、例えばトルエン、又はアセトンに溶解することを含み、それによりTiO2、SiO2、又はFe2O3フレークを製造する、請求項1記載の方法。
- (e’)工程(d’)で得られたTiO2、SiO2、又はFe2O3フレークをフッ素スカベンジャーの水溶液中に懸濁させ;
(f’)所望の金属酸化物コーティングの前駆材料であるフッ素含有金属複合体の一種以上の水溶液を加え;及び
(g’)該懸濁液にマイクロ波放射を施して該有機材料に金属酸化物を付着させる、請求項11記載の方法。 - 更に、下記の工程:
(f)工程(d)における酸化物コーティングと異なる所望の金属酸化物コーティングの前駆材料であるフッ素含有金属複合体の一種以上の水溶液を加え;及び
(g)該懸濁液にマイクロ波放射を施してコーテッド有機基材に金属酸化物を付着させる
を含む請求項8記載の方法。 - 工程(b)及び(f)における金属酸化物が酸化鉄でありかつフッ素含有金属複合体を、塩化鉄(III)、フッ化水素酸及びフッ化アンモニウム混合物からなる群より選択し、工程(d)における金属酸化物が二酸化チタンでありかつフッ素含有金属複合体を、ヘキサフルオロチタン酸アンモニウム、フッ化アンモニウム及び塩化チタン又は塩化チタン、フッ化アンモニウム及びフッ化水素から調製する複合体からなる群より選択する、請求項13記載の方法。
- (e’)工程(d’)で得られた金属酸化物フレークが二酸化チタンフレークであり、第一金属酸化物層を、Fe2O3、Fe3O4、FeOOH、Cr2O3、CuO、Ce2O3、Al2O3、SiO2、BiVO4、NiTiO3、CoTiO3及びアンチモン−ドープト、フッ素−ドープト又はインジウム−ドープト酸化スズ酸化鉄から選択し、場合により存在する第二金属酸化物層を、酸化アルミニウム又は酸化アルミニウム水和物、二酸化ケイ素又は二酸化ケイ素水和物、Fe2O3、Fe3O4、FeOOH、TiO2、ZrO2、Cr2O3並びにアンチモン−ドープト、フッ素−ドープト又はインジウム−ドープト酸化スズから選択し;或は(e’)工程(d’)で得られた金属酸化物フレークが二酸化鉄フレークであり、第一金属酸化物層が、屈折率n£1.8を有する無色のコーティング、例えば酸化ケイ素、酸化ケイ素水和物、酸化アルミニウム、酸化アルミニウム水和物及びこれらの混合物であり、場合により存在する第二金属酸化物層が、屈折率n32.0を有する無色のコーティング、例えば二酸化チタン、酸化チタン水和物、二酸化ジルコニウム、酸化ジルコニウム水和物、二酸化スズ、酸化スズ水和物、酸化亜鉛、酸化亜鉛水和物及びこれらの混合物である、請求項12記載の方法。
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- 2004-06-07 AU AU2004247894A patent/AU2004247894A1/en not_active Abandoned
- 2004-06-07 CN CN2004800169635A patent/CN1809654B/zh not_active Expired - Fee Related
- 2004-06-07 MX MXPA05013497A patent/MXPA05013497A/es unknown
- 2004-06-07 KR KR1020057024243A patent/KR101125084B1/ko not_active IP Right Cessation
- 2004-06-07 ES ES04741739T patent/ES2380329T3/es not_active Expired - Lifetime
- 2004-06-07 JP JP2006516134A patent/JP4908204B2/ja not_active Expired - Fee Related
- 2004-06-07 CA CA002528661A patent/CA2528661A1/en not_active Abandoned
- 2004-06-07 EP EP04741739A patent/EP1631698B1/en not_active Expired - Lifetime
- 2004-06-07 WO PCT/EP2004/051040 patent/WO2004111298A1/en active Application Filing
- 2004-06-07 AT AT04741739T patent/ATE549430T1/de active
- 2004-06-10 US US10/870,643 patent/US7459182B2/en not_active Expired - Fee Related
- 2004-06-16 TW TW093117319A patent/TW200508330A/zh unknown
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006527779A (ja) * | 2003-06-17 | 2006-12-07 | チバ スペシャルティ ケミカルズ ホールディング インコーポレーテッド | コア材料および少なくとも1層の誘電体層を含む顔料の製造方法 |
JP4767845B2 (ja) * | 2003-06-17 | 2011-09-07 | チバ ホールディング インコーポレーテッド | コア材料および少なくとも1層の誘電体層を含む顔料の製造方法 |
JP2011518919A (ja) * | 2008-04-25 | 2011-06-30 | スリーエム イノベイティブ プロパティズ カンパニー | 粒子の表面改質のためのプロセス |
WO2013099478A1 (ja) * | 2011-12-26 | 2013-07-04 | 株式会社 日立製作所 | 複合部材 |
JP2013132757A (ja) * | 2011-12-26 | 2013-07-08 | Hitachi Ltd | 複合部材 |
Also Published As
Publication number | Publication date |
---|---|
EP1631698A1 (en) | 2006-03-08 |
US7459182B2 (en) | 2008-12-02 |
ES2380329T3 (es) | 2012-05-10 |
CA2528661A1 (en) | 2004-12-23 |
WO2004111298A1 (en) | 2004-12-23 |
CN1809654B (zh) | 2010-12-29 |
ATE549430T1 (de) | 2012-03-15 |
EP1631698B1 (en) | 2012-03-14 |
AU2004247894A1 (en) | 2004-12-23 |
TW200508330A (en) | 2005-03-01 |
KR20060019603A (ko) | 2006-03-03 |
CN1809654A (zh) | 2006-07-26 |
US20040265507A1 (en) | 2004-12-30 |
MXPA05013497A (es) | 2006-03-09 |
JP4908204B2 (ja) | 2012-04-04 |
KR101125084B1 (ko) | 2012-03-21 |
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