JP4851453B2 - 歯科用組成物の屈折率を調整するためのナノ粒子の使用 - Google Patents
歯科用組成物の屈折率を調整するためのナノ粒子の使用 Download PDFInfo
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- JP4851453B2 JP4851453B2 JP2007527214A JP2007527214A JP4851453B2 JP 4851453 B2 JP4851453 B2 JP 4851453B2 JP 2007527214 A JP2007527214 A JP 2007527214A JP 2007527214 A JP2007527214 A JP 2007527214A JP 4851453 B2 JP4851453 B2 JP 4851453B2
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- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 1
- FZUGPQWGEGAKET-UHFFFAOYSA-N parbenate Chemical compound CCOC(=O)C1=CC=C(N(C)C)C=C1 FZUGPQWGEGAKET-UHFFFAOYSA-N 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 239000006072 paste Substances 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000005365 phosphate glass Substances 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 239000000068 pit and fissure sealant Substances 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001444 polymaleic acid Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- QTECDUFMBMSHKR-UHFFFAOYSA-N prop-2-enyl prop-2-enoate Chemical compound C=CCOC(=O)C=C QTECDUFMBMSHKR-UHFFFAOYSA-N 0.000 description 1
- UFUASNAHBMBJIX-UHFFFAOYSA-N propan-1-one Chemical compound CC[C]=O UFUASNAHBMBJIX-UHFFFAOYSA-N 0.000 description 1
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 150000003585 thioureas Chemical class 0.000 description 1
- 239000013008 thixotropic agent Substances 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- UIERETOOQGIECD-ONEGZZNKSA-N tiglic acid Chemical compound C\C=C(/C)C(O)=O UIERETOOQGIECD-ONEGZZNKSA-N 0.000 description 1
- UAXOELSVPTZZQG-UHFFFAOYSA-N tiglic acid Natural products CC(C)=C(C)C(O)=O UAXOELSVPTZZQG-UHFFFAOYSA-N 0.000 description 1
- MHMUCYJKZUZMNJ-OWOJBTEDSA-N trans-3-chloroacrylic acid Chemical compound OC(=O)\C=C\Cl MHMUCYJKZUZMNJ-OWOJBTEDSA-N 0.000 description 1
- GTZCVFVGUGFEME-UHFFFAOYSA-N trans-aconitic acid Natural products OC(=O)CC(C(O)=O)=CC(O)=O GTZCVFVGUGFEME-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 150000003628 tricarboxylic acids Chemical class 0.000 description 1
- IEKWPPTXWFKANS-UHFFFAOYSA-K trichlorocobalt Chemical compound Cl[Co](Cl)Cl IEKWPPTXWFKANS-UHFFFAOYSA-K 0.000 description 1
- 150000003673 urethanes Chemical class 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/70—Preparations for dentistry comprising inorganic additives
- A61K6/71—Fillers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/30—Compositions for temporarily or permanently fixing teeth or palates, e.g. primers for dental adhesives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/20—Protective coatings for natural or artificial teeth, e.g. sealings, dye coatings or varnish
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
- A61K6/887—Compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- A61K6/889—Polycarboxylate cements; Glass ionomer cements
Landscapes
- Health & Medical Sciences (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Dental Preparations (AREA)
Description
「硬化性」は、例えば加熱、化学的架橋、放射線重合または架橋などにより組成物をキュアさせ、または凝固させることができることを意味する。
前述のように、本発明の硬化性歯科用組成物は、場合によっては重合性成分を含む。重合性成分は、場合によっては、酸官能基の有無にかかわらないエチレン性不飽和化合物とすることができる。
重合性成分は、存在する場合、酸官能基を有するエチレン性不飽和化合物を場合によっては含む。好ましくは、酸官能基には、炭素、硫黄、リン、またはホウ素のオキシ酸(すなわち、酸素含有酸)が含まれる。
ラジカル重合(例えば、硬化)では、開始反応系は、放射線、熱、またはレドックス/自己キュア化学反応により重合を開始する系から選択することができる。ラジカルとして活性な官能基の重合を開始することができる開始剤のクラスには、光増感剤または促進剤と場合によっては組み合わせてラジカルを発生させる光開始剤が含まれる。このような開始剤は、通常は200〜800nmの波長を有する光エネルギーに曝露させて付加重合するためのラジカルを発生することができる。
本発明の組成物には、少なくとも1つのポリ酸が含まれ、非硬化性もしくは非重合性のポリ酸、または硬化性もしくは重合性のポリ酸(例えば、樹脂改質ポリ酸)とすることができる。通常は、ポリ酸は、複数の酸性の繰返し単位および複数の重合性基を有するポリマーである。代替実施例では、ポリ酸は、重合性基を実質的に含まない場合がある。ポリ酸は、完全に水溶性である必要はないが、他の水性成分と組み合わせた場合に実質的な沈降を起こさないように少なくとも十分に水混和性であるべきである。適切なポリ酸は、(特許文献41)(ウィルソン(Wilson)ら)、第2欄62行から第3欄6行に記載されている。ポリ酸は、良好な貯蔵、取扱い、および混合特性を提供するのに十分な分子量を有するべきである。典型的な重量平均分子量は、ゲルパーミエーションクロマトグラフィーを使用してポリスチレン標準物質に比べて評価して、5,000〜100,000である。
適切な酸反応性フィラーには、金属酸化物、ガラス、および金属塩が含まれる。典型的な金属酸化物には、酸化バリウム、酸化カルシウム、酸化マグネシウム、および酸化亜鉛が含まれる。典型的なガラスには、ホウ酸塩ガラス、リン酸塩ガラス、およびフルオロアルミノケイ酸(「FAS」)ガラスが含まれる。FASガラスが特に好ましい。FASガラスは、通常は十分な溶離可能カチオンを含み、したがってガラスを硬化性組成物の成分と混合すると硬化した歯科用組成物が形成する。ガラスは、通常は十分な溶離可能フッ化物イオンも含み、したがって硬化した組成物が齲蝕特性を有する。ガラスは、FASガラス製造技術分野の当業者によく知られている技法を使用して、フッ化物、アルミナ、および他のガラス形成材料を含む溶融物から作製することができる。FASガラスは、通常は十分に微細化された粒子の形であり、したがって他のセメント成分と都合よく混合することができ、得られた混合物を口中で使用するとうまく機能する。
本発明のアイオノマー組成物は、望ましい美的特性(例えば、高い光学的透過性)を組成物に付与する1つまたは複数のナノフィラーと配合される。適切なナノフィラーは、酸反応性でもよく、または酸反応性でなくてもよく、シリカ;ジルコニア;チタン、アルミニウム、セリウム、スズ、イットリウム、ストロンチウム、バリウム、ランタン、亜鉛、イッテルビウム、ビスマス、鉄、およびアンチモンの酸化物;ならびにその組合せが含まれるが、これらに限定されない。より典型的なナノフィラーにジルコニア(ZrO2);チタン(例えば、TiO2)およびイッテルビウム(例えば、Y2O3)の酸化物;および高屈折率を有する他の金属酸化物が含まれ得る。本明細書では、「高屈折率」は、通常は少なくとも1.5、より典型的には少なくとも2.0の屈折率を意味する。チタニアジオキシドおよびジルコニアは、非常に高い屈折率を有し、屈折率に適切に整合させるのにより低い屈折率の材料より少ない重量の材料ですむので、特に有用なナノフィラーである。
酸反応性フィラーおよびナノフィラー成分に加えて、本発明の組成物は、場合によっては1つまたは複数の他のフィラーも含むことができる。このようなフィラーは、歯科用および/または歯科矯正用の組成物での使用に適した広範囲の材料の1つまたは複数から選択することができる。
本発明の組成物は水を含有する。水は、蒸留水、脱イオン水、または淡水の水道水とすることができる。通常は、脱イオン水を使用する。
場合によっては、硬化性組成物は、他の溶媒、共溶媒(例えば、アルコール)、または希釈剤を含有することができる。必要に応じて、本発明の硬化性組成物は、指示剤、染料、顔料、阻害剤、促進剤、粘度調整剤、湿潤剤、酒石酸、キレート化剤、界面活性剤、緩衝剤、安定剤、および当業者に自明である他の同様な材料などの添加剤を含有することができる。さらに、医薬品または他の治療物質を、歯科用組成物に場合によっては添加することができる。例としては、歯科用組成物でしばしば使用されるタイプのフッ化物供給源、ホワイトニング剤、抗カリエス剤(例えば、キシリトール)、再石灰化剤(例えば、リン酸カルシウム化合物)、酵素、ブレスフレッシュナー、麻酔剤、凝固剤、酸中和剤、化学療法剤、免疫応答調節剤、チキソトロープ剤、ポリオール、抗炎症剤、抗菌剤、抗真菌剤、口内乾燥症の治療剤、減感剤などが挙げられるが、これらに限定されない。上記の添加剤のいずれの組合せでも使用することができる。いずれか1つのこのような添加剤の選択および量は、過度の実験なしに所望の結果が実現されるように当業者によって選択される。
本発明の硬化性歯科用組成物は、通常の混合技法を使用して様々な成分をすべて組み合わせることによって調製することができる。上述のように、酸反応性フィラーとポリ酸のイオン反応により、組成物を部分または完全硬化させることができる。場合によっては、組成物は、重合性成分および光開始剤を含有し、光開始反応により硬化することができ、あるいは組成物が例えば酸化剤および還元剤を含めてラジカル開始剤系を含むレドックスキュア系などの化学重合により部分または完全硬化することができる。あるいは、硬化性組成物は、様々な開始剤系を含有することができ、したがって組成物を、光重合性組成物と化学重合性組成物、ならびにイオン性硬化性組成物となり得る。屈折率を整合させる系は、共に2004年5月17日に出願された「ナノフィラーを含有する歯科用組成物および関連方法(Dental Compositions Containing Nanofillers and Related Methods)」という名称の(特許文献52)および「ナノジルコニアフィラーを含有する歯科用組成物(Dental Compositions Containing Nanozirconia Fillers)」という名称の(特許文献53)に記載のものなど歯科用組成物の配合でも使用することができる。
TEM(透過型電子顕微鏡)試験方法による平均粒径
厚さ約80nmの試料を、炭素で安定化されたホルムバール基材の200メッシュの銅グリッド(ストラクチャー・プローブ・インクの1つのディビジョンであるSPIサプライズ、米国ペンシルベニア州ウェストチェスター(SPI Supplies,a division of Structure Probe,Inc.,West Chester,PA))上に配置した。JEOL 200CX装置(JEOL,Ltd.、日本 昭島(Akishima,Japan)およびJEOL USA,Inc.販売)を200Kvで使用して、透過電子顕微鏡写真(TEM)を撮った。約50〜100個の粒子の集団の大きさを測定し、平均粒径を決定した。
液体組成物の屈折率値は、ボシュロム(Bausch and Lomb)製のアッベ(Abbe)−3L屈折計を利用して室温で測定した。測定を、製造者の推奨および良好な実験室の慣行に従って実施した。
固体材料(例えば、ガラスフィラー)の屈折率値は、固体試験試料を様々な知られている比屈折率を有する光学液体に分散することによって室温で測定した。較正された光学液体を含むキットは、カーギル研究所(Cargille Laboratories)(米国ニュージャージー州シーダーグローブ(Cedar Grove,NJ))から市販されている。分散液の観察は、光学顕微鏡で行われた。顕微鏡を用いた調査で分散粒子の外縁に沿って現れる光の帯としてベッケ線を使用することによって、固体材料の屈折率を決定した。ベッケ線は、固体材料と光学液体の屈折率が相対的に異なる、または等しいことを示唆する。
混合試験試料を、水が底部に存在しているが試料と接触していないシール容器中、37℃で1時間反応させ、硬化させることによって、円盤形状の(厚さ1mm×直径20mm)試験試料を調製した。硬化した試料について、マクベス(MacBeth)(マクベス、米国ニューヨーク州ニューバーグ(MacBeth,Newburgh,NY))から入手可能な、可視光フィルターを装備したマクベス(MacBeth)透過濃度計モデルTD−903を使用して、円盤の厚さを通り抜ける光の透過率を測定することによって、直接光透過率を測定した。マクベス値が低いほど、視覚不透明性が低く透光性が高い材料であることを示唆している。報告された値は、3個の測定値の平均である。
混合試験試料を、36℃および少なくとも95%の相対湿度で1時間反応および硬化させることによって、円盤形状の(厚さ1.5mm×直径15mm)試験試料を調製した。硬化した試料について、反射率測定法を用い、かつハンターラブ(HunterLab)測色装置(ラブスキャン(Labscan)−2 0/45 SN−14014;ハンターラブ、米国バージニア州レストン(HunterLab,Reston,VA))を使用することによって、不透明性を測定した。この試験における不透明性は、黒色で裏打ちされた試料の反射率と白色で裏打ちされた試料の反射率の比と定義する。第1の測定を1時間不透明性値と指定する。その後に、試料を直ちにバイアルに移し、36℃の水にさらに23時間貯蔵し、その後に、不透明性を上述のように測定した(24時間不透明性)。ハンターラブ(HunterLab)不透明性値が低くなれば、材料の視覚不透明性は低くなり、透過性は高くなることが示唆される。
混合試験試料を、水が底部に存在しているが試料と接触していないシール容器中、36℃で1時間反応させ、硬化させることによって、圧縮強さを評価した。硬化させた円盤形状の試料(直径4mm×厚さ6mm)を水中に36℃でさらに23時間貯蔵した。次いで、ISO規格9917−1(1991)に従って、1ミリメートル/分(mm/分)のクロスヘッド速度で操作したツビック(Zwick)万能試験機(ツビック、ドイツ ウルム(Zwick GmbH&Co.KG,Ulm,Germany))を使用して、圧縮強さを決定した。結果は、6回の反復実験の平均として報告した。
試験試料の曲げ強さは、長方形の形状の試料(長さ25mm×幅2mm×厚さ2mm)を使用した点以外は上記のCS試験方法について記載されているように評価し、曲げ強さは、ISO規格9917−2(1998)に従って、1ミリメートル/分(mm/分)のクロスヘッド速度で操作したツビック(Zwick)万能試験機(ツビック、ドイツ ウルム(Zwick GmbH&Co.KG,Ulm,Germany))を使用して決定した。結果は、6回の反復実験の平均として報告した。
ポリ酸A:
アクリル酸およびマレイン酸のコポリマー
アクリル酸およびマレイン酸ナトリウム塩(モル比1:1.2)に過酸化水素開始剤(アクリル酸に対して5倍モル過剰)を添加した水溶液を、90〜100℃で5時間加熱した。室温に冷却した後、溶液を硫酸でpH約1に酸性化した。得られたポリ酸沈殿物を膜濾過で精製し、スプレー乾燥で単離して、10,000〜12,000g/molの平均分子量(MW)を有するポリ(アクリル/マレイン)酸として特徴付けられた粉末を得た。
アクリル酸およびマレイン酸のコポリマー
アクリル酸およびマレイン酸ナトリウム塩(モル比1:1.2)に過酸化水素開始剤(アクリル酸に対して0.1モル比)を添加した水溶液を、90〜100℃で5時間加熱した。室温に冷却した後、溶液を硫酸でpH約1に酸性化した。得られたポリ酸沈殿物を膜濾過で精製し、スプレー乾燥で単離し、28,000〜32,000g/molの平均分子量(MW)を有するポリ(アクリル/マレイン)酸として特徴付けられた粉末を得た。
シラン処理したナノチタニア(「高レベル」)
OPTILAKE 3チタニアゾル(200g)をシルクエスト(SILQUEST)A−1230(12.026g)と組み合わせ、得られた溶液を、シール容器中80℃で16時間加熱した。得られた溶液を粉末(ナノフィラーAと称される)になるまで乾燥した。これは、わずかな熱および撹拌(ホットプレートで60〜80℃)で非常に効果的に水に分散して、光学的に透明な溶液を形成することが判明した。
シラン処理したナノチタニア(「低レベル」)
OPTILAKE 3チタニアゾル(100g)をシルクエスト(SILQUEST)A−1230(3g)と組み合わせ、得られた溶液を、シール容器中80℃で16時間加熱した。得られた溶液を粉末(ナノフィラーBと称される)になるまで乾燥した。これは、わずかな熱および撹拌(ホットプレートで60〜80℃)で非常に効果的に水に分散して、光学的に透明な溶液を形成することが判明した。
シラン処理したナノチタニア(「より低いレベル」)
OPTILAKE 3チタニアゾル(25g)をシルクエスト(SILQUEST)A−1230(0.625g)と組み合わせ、得られた溶液を、シール容器中80℃で16時間加熱した。得られた溶液を粉末(ナノフィラーCと称される)になるまで乾燥した。これは、わずかな熱および撹拌(ホットプレートで60〜80℃)で非常に効果的に水に分散して、光学的に透明な溶液を形成することが判明した。
シラン処理したナノチタニアゾル(「高レベル」)
OPTILAKE 3チタニアゾル(15g)を、シルクエスト(SILQUEST)A−1230(0.375g)と組み合わせ、得られた溶液を、シール容器中80℃で16時間加熱し、次いで室温に冷却した。得られたチタニアゾル(約10重量%のシラン処理したナノチタニアフィラー)をチタニアゾルA1230−A(TS A1230−A)と称した。
シラン処理したナノチタニアゾル(「低レベル」)
OPTILAKE 3チタニアゾル(200g)をシルクエスト(SILQUEST)A−1230(1.16g)と組み合わせ、得られた溶液を、シール容器中80℃で16時間加熱し、次いで室温に冷却した。得られたチタニアゾル(約10重量%のシラン処理したナノチタニアフィラー)をチタニアゾルA1230−B(TS A1230−B)と称した。
シラン処理したナノジルコニア
ジルコニアゾル(100.0g;16.95gのジルコニア)を、16オンスのガラス製ジャーに加え、続いて撹拌しながら、1−メトキシ−2−プロパノール(100g;シグマ−アルドリッチ(Sigma−Aldrich))、シルクエスト(SILQUEST)A−174(3.45g)およびシルクエスト(SILQUEST)A−1230(2.4g)を添加した。得られた混合物を室温で10分間撹拌し、90℃に4.0時間加熱し、次いで内容物をロータリーエバポレーションで濃縮して、液体濃縮物(59g)を得た。
水性ポリ酸+シラン処理したナノチタニアフィラー
ナノフィラーAおよびBを様々なレベルで、30重量%のポリ酸A水溶液に添加し、本明細書に記載するRI試験方法Aに従って、得られた分散液の屈折率(RI)値を決定した。表1に、様々なナノフィラーレベルおよびRIの測定値を示す。
水性ポリ酸+シラン処理したナノチタニアフィラー+FASガラス
30重量%のポリ酸A水溶液を40重量%のナノフィラーA(実施例1/ラン5;「液体成分」)と組み合わせ、続いてFASフィラーA(「粉末成分」;RI 約1.508)を添加することによって、グラスアイオノマー(GI)組成物を調製した。2つの成分を、重量比2:1の粉末/液体で完全に混合して、実施例2と称したペーストを得た。それから、これを、水が底部に存在しているが試料と接触していないシール容器中、37℃で1時間硬化させた。
水性ポリ酸+シラン処理したナノチタニアフィラー+FASガラス
30重量%のポリ酸A水溶液を40重量%のナノフィラーB(「液体成分」;実施例1/ラン8)と組み合わせ、続いてFASフィラーA(「粉末成分」)を添加することによってグラスアイオノマー(GI)組成物を調製した。2つの成分を、重量比2.5:1の粉末/液体(すなわち、71.4%のFASフィラーAを充填)で完全に混合して、ペーストを得た。これを実施例4と称し、それから水が底部に存在しているが試料と接触していないシール容器中、37℃で1時間硬化させた。
グラスアイオノマー組成物
粉末パート(ポリ酸およびFASガラスフィラー成分を含有)を液体パート(水および任意選択的なナノフィラー成分を含有)と混合することによって、グラスアイオノマー(GI)組成物を調製し、得られたペースト(実施例7〜9および比較例2〜3)を、36℃および少なくとも95%の相対湿度で1時間硬化させた。ナノフィラー成分は、TS A1230−Aの形(約10重量%のシラン処理したナノチタニアを含有するチタニアゾル、または同じゾルのより濃縮した形(例えば、約20重量%))で導入した。表4に、粉末成分および液体成分の相対重量部、ペースト混合組成物中の成分の重量部、および利用する粉末/液体の重量比を示す。
グラスアイオノマー組成物
粉末パート(ポリ酸およびFASガラスフィラー成分を含有)を液体パート(水および任意選択的なナノフィラー成分を含有)と混合することによって、グラスアイオノマー(GI)組成物を調製し、得られたペースト(実施例10〜20および比較例4)を、36℃および少なくとも95%の相対湿度で1時間硬化させた。ナノフィラー成分は、TS A1230−B、OPTILAKE 3 TS、またはナノフィラーCの形で導入した。表5Aおよび5Bに、粉末成分および液体成分の相対重量部、ペースト混合組成物中の成分の重量部、および利用する粉末/液体の重量比を示す。
樹脂改質グラスアイオノマー組成物
表6Aに列挙する材料(重量部で示す)を組み合わせることによって、2個の第1のペースト組成物(ペーストA1およびA2と称される)を調製した。フィラーD(シラン処理したナノジルコニア)を、組成物に樹脂A(HEMA/PEGDMA−400−ナノフィラーDの出発材料調製を参照のこと)中70%のナノジルコニアからなる流体分散物の一部分として添加した。表6Bに列挙する材料(重量部で示す)を組み合わせることによって、1個の第2のペースト組成物(ペーストBと称される)を調製した。
Claims (5)
- 硬化性歯科用組成物であって、
(a)ポリ酸;
(b)酸反応性フィラー;
(c)ナノフィラー;
(d)水;および
(e)任意選択的な重合性成分を含み、
前記ポリ酸、前記ナノフィラー、前記水、および前記任意選択的な重合性成を組み合わせた混合物の屈折率が、前記酸反応性フィラーの屈折率の4パーセント以内である、組成物。 - 重合性成分を含む、請求項1に記載の組成物。
- 前記酸反応性フィラーが、フルオロアルミノケイ酸(FAS)ガラスを含む、請求項1に記載の組成物。
- 歯科用物品を調製する方法であって、
(a)請求項1に記載の歯科用組成物を提供するステップと、
(b)前記歯科用組成物を硬化して、前記歯科用物品を形成するステップとを含む方法。 - 前記歯科用物品が、歯科用ミルブランク、歯冠、歯科用充填物、義歯、および歯科矯正用装置からなる群から選択される、請求項4に記載の方法。
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PCT/US2005/010404 WO2005117806A1 (en) | 2004-05-17 | 2005-03-29 | Use of nanoparticles to adjust refractive index of dental compositions |
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JP (1) | JP4851453B2 (ja) |
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AT (1) | ATE456948T1 (ja) |
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DE10026432A1 (de) | 2000-05-29 | 2002-02-14 | 3M Espe Ag | Präpolymere (Meth)acrylate mit polycyclischen oder aromatischen Segmenten |
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2004
- 2004-05-17 US US10/847,803 patent/US7090721B2/en not_active Expired - Lifetime
-
2005
- 2005-03-29 DE DE602005019235T patent/DE602005019235D1/de active Active
- 2005-03-29 WO PCT/US2005/010404 patent/WO2005117806A1/en active Application Filing
- 2005-03-29 JP JP2007527214A patent/JP4851453B2/ja active Active
- 2005-03-29 AT AT05744069T patent/ATE456948T1/de not_active IP Right Cessation
- 2005-03-29 EP EP05744069A patent/EP1750650B1/en active Active
- 2005-03-29 CN CN2005800239401A patent/CN1984632B/zh not_active Expired - Fee Related
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- 2005-03-29 AU AU2005249353A patent/AU2005249353B2/en active Active
- 2005-03-29 KR KR1020067026523A patent/KR101166940B1/ko not_active IP Right Cessation
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Also Published As
Publication number | Publication date |
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WO2005117806A1 (en) | 2005-12-15 |
KR20070013331A (ko) | 2007-01-30 |
ATE456948T1 (de) | 2010-02-15 |
AU2005249353A1 (en) | 2005-12-15 |
EP1750650A1 (en) | 2007-02-14 |
CN1984632B (zh) | 2012-06-06 |
CN1984632A (zh) | 2007-06-20 |
KR101166940B1 (ko) | 2012-07-19 |
CA2567034A1 (en) | 2005-12-15 |
EP1750650B1 (en) | 2010-02-03 |
US7090721B2 (en) | 2006-08-15 |
DE602005019235D1 (de) | 2010-03-25 |
CA2567034C (en) | 2013-10-01 |
AU2005249353B2 (en) | 2011-08-18 |
US20050252414A1 (en) | 2005-11-17 |
JP2007538072A (ja) | 2007-12-27 |
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