JP2020533449A - 放射線硬化性組成物及び積層造形プロセスを使用して作製された複合材物品 - Google Patents
放射線硬化性組成物及び積層造形プロセスを使用して作製された複合材物品 Download PDFInfo
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- JP2020533449A JP2020533449A JP2020514195A JP2020514195A JP2020533449A JP 2020533449 A JP2020533449 A JP 2020533449A JP 2020514195 A JP2020514195 A JP 2020514195A JP 2020514195 A JP2020514195 A JP 2020514195A JP 2020533449 A JP2020533449 A JP 2020533449A
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Images
Classifications
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Abstract
Description
1. 放射線硬化性組成物であって、少なくとも1つの放射線硬質化性成分と、光開始剤と、50重量%以上の量のプリント可能な組成物の微粒子の集合を含む充填材料と、を含み、この微粒子の集合は、粒径試験方法を使用して判定したときに体積平均基準で0.3マイクロメートル以上のメジアン径(D50)を呈し、更に、この放射線硬化性組成物は、粘度試験方法を使用して測定したときに150Pa・s以下の粘度を呈し、任意に、この放射線硬化性組成物は、有機溶媒を実質的に含まない、放射線硬化性組成物。
ある特定の用語が、本明細書及び特許請求の範囲の全体を通して使用されており、これらの大部分については周知であるが、何らかの説明が必要とされる場合もある。本明細書において使用される場合、以下の通りであることが理解されるべきである。
本開示は、以下に更に記載されるように、積層造形装置プロセス(例えば、ステレオフォトリソグラフィ)を使用して、ニアネットシェイプ(コ)ポリマー−セラミック複合歯科用修復物を製造するのに有用な放射線硬化性組成物について記載している。したがって、一例示的実施形態では、本開示は、少なくとも1つの放射線硬質化性成分と、光開始剤と、50重量%以上の量のプリント可能な組成物の微粒子の集合を有する充填材料と、を含む放射線硬化性組成物について記載している。微粒子の集合は、粒径試験方法を使用して判定したときに体積平均基準で0.3マイクロメートルより大きいメジアン径(D50)を呈し、放射線硬化性組成物は、粘度試験方法を使用して測定したときに150Pa・s未満の粘度を呈する。
本開示の放射線硬化性組成物は、少なくとも1つの放射線硬質化性成分又は放射線硬化性成分を含む。例えば、いくつかの実施形態では、放射線硬化は、(共)重合又は架橋反応を開始するために十分なエネルギーを有する化学線源を放射線硬質化性成分に選択的に照射することを含む。例えば、いくつかの実施形態では、紫外線(UV)、電子ビーム線、又はこれらの両方を、化学線源として使用することができる。他の実施形態では、ガンマ線を放射線源として使用してもよい。
本明細書に記載の放射線硬化性組成物は、1つ以上の光開始剤を更に含む。好ましくは、光開始剤は、カチオン性光開始剤ではない。より好ましくは、光開始剤は、光ラジカル光開始剤である。光開始剤は、典型的には、0.1〜5重量%、又は0.2〜4重量%、又は0.5〜3重量%の量で存在する。
・200〜500nm、又は300〜450nmの範囲内の放射線吸収バンドを示すこと。
・わずかに黄色がかった色を有すること。
(R9)2−P(=O)−C(=O)−R10
(式中、各R9は個々に、アルキル、シクロアルキル、アリール、及びアラルキル等のヒドロカルビル基であってもよく、そのいずれもがハロ−、アルキル−、若しくはアルコキシ基で置換されていてもよく、又は2つのR9基が結合してリン原子と共に環を形成することができ、R10はヒドロカルビル基、S−、O−、若しくはN−含有5若しくは6員複素環基、又は−Z−C(=O)−P(=O)−(R9)2基であり、式中、Zは2〜6個の炭素原子を有するアルキレン又はフェニレン等の二価のヒドロカルビル基を表す)のものである。
−下限量:少なくとも0.01、又は少なくとも0.05、又は少なくとも0.1重量%;
−上限量:最大で3、又は最大で2、又は最大で1.5重量%;
−範囲:0.01〜3、又は0.05〜2重量%、又は0.1〜1.5重量%;
ここでの重量%は組成物全体の重量に対する重量%である。
本明細書に記載の放射線硬化性組成物は、50重量%以上の量のプリント可能な組成物の微粒子の集合を含む充填材料を更に含む。微粒子の集合は、本明細書で以下に記載されるように、レーザ回折粒径分析を使用して判定される体積平均基準で1マイクロメートル以上のメジアン径(D50)を呈する。放射線硬化性組成物中に使用される充填剤の量及びメジアン径は、硬化性組成物の粘度、硬化組成物の耐摩耗性、又はその両方に影響を及ぼし得る。
−下限量:プリント可能な組成物の少なくとも50重量%、55重量%、60重量%、又は更には70重量%;
−上限量:プリント可能な組成物の最大で80重量%、75重量%、70重量%、又は更には65重量%、又は55重量%;
−範囲:プリント可能な組成物の50重量%〜80重量%(両端値を含む)、50重量%〜75重量%(両端値を含む)、又は50重量%〜65重量%。
−下限量:少なくとも0.5、又は少なくとも1、又は少なくとも1.5重量%;
−上限量:最大8、又は最大7、又は最大5重量%;
−範囲:0.5〜8、又は1〜7、又は1.5〜5重量%;
ここでの重量%は、硬化性組成物全体の重量に対する重量%である。
−比表面積:30〜400、又は60〜300、又は80〜250m2/gであること、
−SiO2、ZrO2、Al2O3、及びこれらの混合物の粒子を含むこと、のうちの少なくとも1つ又は全てによって、特徴付けることができる。
−下限量:少なくとも5、又は少なくとも10、又は少なくとも15重量%;
−上限量:最大40、又は最大38、又は最大35重量%;
−範囲:5〜40、又は10〜38、又は15〜35重量%;
ここでの重量%は、硬化性組成物全体の重量に対する重量%である。
放射線硬化性組成物には、様々な追加成分を任意に含んでもよい。したがって、いくつかの例示的実施形態では、放射線硬化性組成物は、溶媒、モノマー、(コ)ポリマー、乳化剤、重合阻害剤、吸収調整剤、光増感剤、着色剤、繊維強化材料、又はこれらの組み合わせからなる群から選択される少なくとも1種の添加剤を含む。
ここでは好ましくないが、本開示の放射線硬化性組成物は、任意に、少なくとも1種の溶媒、好ましくは非反応性有機溶媒を含んでもよい。放射線硬質化性成分の粘度は、非反応性の溶媒などの溶媒中で成分を希釈することにより大幅に低下させることができる。本開示で有用な非反応性の溶媒を、本明細書では一時的溶媒と称する。
ここでは好ましくないが、1つ以上のモノマーを任意にこのようなフリーラジカル(共)重合性材料に組み込んでもよく、このようなフリーラジカル(共)重合性材料としては、メチルアクリレート、メチルメタクリレート、アクリル酸エチル、イソプロピルメタクリレート、n−アクリル酸ヘキシル、ステアリルアクリレート、アリルアクリレート、グリセロールジアクリレート、2−ヒドロキシエチルメタクリレート(HEMA)と2,2,4−トリメチルヘキサメチレンジイソシアネート(TMDI)との反応生成物であるUDMA(例えば、Rohm Plex 6661−0などの異性体の混合物)と呼ばれるジウレタンジメタクリレート、グリセロールトリアクリレート、エチレングリコールジアクリレート、ジエチレングリコールジアクリレート、トリエチレングリコールジメタクリレート、1,3−プロパンジオールジアクリレート、1,3−プロパンジオールジメタクリレート、トリメチロールプロパントリアクリレート、1,2,4−ブタントリオールトリメタクリレート、1,4−シクロヘキサンジオールジアクリレート、ペンタエリスリトールトリアクリレート、ペンタエリスリトールテトラアクリレート、ペンタエリスリトールテトラメタクリレート、ソルビトールヘキサクリレート、ビス[1−(2−アクリルオキシ)]−p−エトキシフェニルジメチルメタン、ビス[1−(3−アクリルオキシ−2−ヒドロキシ)]−p−プロポキシフェニルジメチルメタン、及びトリスヒドロキシエチル−イソシアヌレートトリメタクリレートなどのモノ−、ジ−、トリ−、又は他のポリアクリレート及びメタクリレート;分子量200〜500のポリエチレングリコールのビスアクリレート及びビスメタクリレート、米国特許第4,652,274号(Boettcherら)におけるものなどのアクリル化モノマーの共(共)重合可能な混合物、並びに米国特許第4,642,126号(Zadorら)におけるものなどのアクリレート化オリゴマー;欧州特許第2008636号(Hechtら)のものなどの、ウレタン、尿素又はアミド基を含む多官能性(メタ)アクリレートが挙げられる。放射線硬質化性成分が、任意に、ウレタン基、エポキシ基、又はその両方を含む。放射線硬質化性成分は、シリコーンアクリレートオリゴマー、エポキシ(メタ)アクリレートオリゴマー、ポリエステル(メタ)アクリレートオリゴマー又は塩素化ポリエステル(メタ)アクリレート、アリル系オリゴマー及び(メタ)アクリルオリゴマーを更に含んでもよい。所望により、これらのフリーラジカル(共)重合性材料のうちの2つ以上の混合物を使用することができる。
ここでは好ましくないが、本開示の放射線硬化性組成物は、任意に、少なくとも1つの(コ)ポリマーを含んでもよい。少なくとも1つの(コ)ポリマーは、最終(コ)ポリマー−セラミック複合修復物に可撓性を提供する(例えば、少なくとも最小破断伸度)。いくつかの実施形態では、(コ)ポリマーが、非架橋性(コ)ポリマーを含む。非架橋性(コ)ポリマーを含めることは、放射線硬化性組成物が化学線に曝露されて放射線硬質化性成分を(共)重合させたときに、(コ)ポリマーは架橋せずその伸長能力を低下させないため、有利であり得る。
ある特定の実施形態では、エマルジョンは、放射線硬質化性成分及びいずれかの任意による成分を含有する形態であってもよい。
加えて、本明細書に記載の放射線硬化性組成物は、1つ以上の増感剤を更に含んでよく、同様に存在し得る1つ以上の光開始剤の有効性を増加させ得る。いくつかの実施形態では、増感剤は、イソプロピルチオキサントン(isopropylthioxanthone、ITX)又は2−クロロチオキサントン(chlorothioxanthone、CTX)を含む。他の増感剤もまた使用されてよい。放射線硬化性組成物中で使用する場合、増感剤は、放射線硬化性組成物の総重量に基づいて、約0.01重量%又は約1重量%の範囲の量で存在することができる。
本明細書に記載の放射線硬化性組成物はまた、任意に1つ以上の(共)重合阻害剤又は安定剤を含む。(共)重合阻害剤は、多くの場合、組成物に更なる熱安定性を加えるために放射線硬化性組成物に含まれる。いくつかの例では、安定剤は1種以上の酸化防止剤を含む。本開示の目的に反しない任意の酸化防止剤を使用してよい。例えば、いくつかの実施形態では、好適な酸化防止剤として様々なアリール化合物が挙げられ、これにはブチル化ヒドロキシトルエン(BHT)(butylated hydroxytoluene)が含まれ、これは、本明細書に記載の実施形態で(共)重合阻害剤としてもまた使用することができる。追加的に又は代替的に、(共)重合阻害剤は、メトキシヒドロキノン(MEHQ)(methoxyhydroquinone)を含む。
本明細書に記載の放射線硬化性組成物はまた、化学線の透過度を制御するために、1つ以上の吸収調整剤(例えば、染料、光学的増白剤、顔料、微粒子充填剤など)を含むことができる。特に好適な吸収調整剤の1つは、BASF Corporation(Florham Park,NJ)から入手可能なTinopal OB(ベンゾオキサゾール,2,2’−(2,5−チオフェンジイル)ビス[5−(1,1−ジメチルエチル)])である。吸収調整剤を使用する場合、吸収調整剤は、放射線硬化性組成物の総重量に基づいて、約0.001重量%〜5重量%、約0.01重量%〜1重量%、0.1重量%〜3重量%、又は約0.1重量%〜1重量%の量で存在し得る。
本明細書に記載の放射線硬化性組成物はまた、染料、顔料、及び顔料染料などの1つ以上の着色剤を含んでもよい。好適な着色剤は、米国特許第5,981,621号(Clarkら)に記載され、例としては、1−ヒドロキシ−4−[4−メチルフェニルアミノ]−9,10−アントラセンジオン(FD&C紫色2号)、6−ヒドロキシ−5−[(4−スルホフェニル)オキソ]−2−ナフタレンスルホン酸の二ナトリウム塩(FD&C黄色6号)、9−(o−カルボキシフェニル)−6−ヒドロキシ−2,4,5,7−テトラヨード−3H−キサンテン−3−オン、二ナトリウム塩、一水和物(FD&C赤色3号)などが挙げられる。
本明細書に記載の放射線硬化性組成物はまた、1つ以上の繊維性強化材を含むことができ、好適な繊維性強化材の例としては、米国特許第6,183,593号(Narangら)に記載されているようなPGAマイクロ繊維、コラーゲンマイクロ繊維、及びその他のものが挙げられる。不連続繊維もまた、炭素、セラミック、ガラス、又はこれらの組み合わせを含む繊維などの好適な充填剤でもある。好適な不連続繊維は、セラミック繊維などの様々な組成物を有することができる。セラミック繊維は連続長で製造され得、これらが細断又は剪断されて、不連続なセラミック繊維が得られる。セラミック繊維は、様々な市販のセラミックフィラメントから製造され得る。
所望の場合、本開示の組成物は、他の添加剤、例えば、指示薬、促進剤、界面活性剤、湿潤剤、酸化防止剤、酒石酸、キレート化剤、緩衝剤、及び当業者に明らかである他の類似成分を含有してもよい。加えて、医薬又は他の治療用物質を、プリントされた組成物に任意に添加することができる。例としては、フッ化物供給源、増白剤類、抗カリエス剤類(例えば、キシリトール)、無機成分補給剤類(例えば、リン酸カルシウム化合物、並びにその他のカルシウム供給源及びホスフェート供給源)、酵素類、口臭清涼剤類、麻酔剤類、凝固剤類、酸中和剤類、化学療法剤類、免疫反応調整剤類、チキソトロープ類、ポリオール類、抗炎症剤類、抗菌剤類、抗カビ剤類、口内乾燥処理剤、減感剤類などの、多くの場合、歯科用組成物に使用されるタイプのものが挙げられるが、これらに限定されない。
本開示はまた、放射線硬化性組成物を、ニアネットシェイプ(コ)ポリマー−セラミック複合歯科用修復物に加工するのに有用な積層造形プロセスについても記載している。したがって、更なる例示的実施形態では、本開示は、複合材物品の製造方法について記載しており、この方法が、(a)放射線硬化性組成物が、少なくとも1つの放射線硬化性(例えば、放射線硬質化性)成分と、光開始剤と、50重量%以上の量のプリント可能な組成物の微粒子の集合を有する充填材料と、を含み、この微粒子の集合は、粒径試験方法を使用して判定したときに体積平均基準で0.3マイクロメートルより大きいメジアン径(D50)を呈し、更に、この放射線硬化性組成物は、粘度試験方法を使用して測定したときに150Pa・s未満の粘度を呈し、任意に、この放射線硬化性組成物は、有機溶媒を実質的に含まない、放射線硬化性組成物を提供するステップと、(b)この放射線硬化性組成物の一部分を化学線源に選択的に曝露して、この放射線硬化性組成物のこの曝露部分を少なくとも部分的に硬化させ、それによって硬質化された層を形成するステップと、を含み、ステップ(a)及び(b)が繰り返されて、ニアネットシェイプ複合材物品を形成する。
様々な歯科用修復物(例えば、図3〜図5に示されるような歯科用クラウン)は、上述の例示的な放射線硬化性組成物及び積層造形方法を使用して製造することができる。
更なる例示的実施形態では、本開示は、歯科用修復物の3Dモデルを表示するディスプレイと、ユーザーによって選択されたこの3Dモデルに応じて、積層造形方法を使用してニアネットシェイプ複合歯科用修復物を積層造形デバイスに作製させる、1つ以上のプロセッサと、を含む、システムについて記載している。積層造形方法は、(a)放射線硬化性組成物を提供するステップと、(b)この放射線硬化性組成物の一部分を化学線源に選択的に曝露して、この放射線硬化性組成物のこの曝露部分を少なくとも部分的に硬化させ、それによって硬質化された層を形成するステップと、を含む。ステップ(a)及び(b)は繰り返されて、ニアネットシェイプ複合歯科用修復物を形成する。放射線硬化性組成物は、少なくとも1つの放射線硬質化性(例えば、放射線硬質化性)成分と、光開始剤と、50重量%以上の量のプリント可能な組成物の微粒子の集合を有する充填材料と、を含み、この微粒子の集合は、粒径試験方法を使用して判定したときに体積平均基準で0.3マイクロメートルより大きいメジアン径(D50)を呈し、更に、この放射線硬化性組成物は、粘度試験方法を使用して測定したときに150Pa・s未満の粘度を呈する。
本明細書では、全ての部及びパーセンテージは、別途特定されない限り、重量(重量%)によるものとする。全ての水は脱イオン水であり、全ての分子量は、別途特定されない限り、平均分子量である。別途特定されない限り、材料は、Sigma−Aldrich(Milwaukee,WI)から得ることができる。別途特定されない限り、3Dプリントの実施例は全て、Asiga USA(Anaheim Hills,CA)から入手可能な液槽(共)重合3Dプリンタ、ASIGA PICO 2を用いた。
充填樹脂(すなわち、プリント用組成物)を、表3に示す配合に従って、Thinkyプラネタリーミキサー内にて2000rpmで1分間高速混合することにより調製した。混合は4回繰り返し、各混合サイクルの間にプリント用組成物を室温まで放冷した。
以下の試験方法を使用して、本開示の実施例のうちの一部を評価した。
充填樹脂の粒径分布を以下のように判定した。充填樹脂を、1−メトキシ−2−プロパノールで、1:1000の体積比に希釈してから、再循環プールに導入した。粒径分布は、Horiba粒径分布分析器モデルLA−950V2でのレーザ回折粒径分析を使用して測定した。各充填樹脂の体積平均D10値、D50値(メジアン)、及びD90値(マイクロメートル、μm)を表4に示す。
40℃にて0.1/秒の剪断速度で40mmコーンプレート測定システムを使用するTA Instruments AR−G2磁気ベアリングレオメーターを用いて、未充填樹脂及び充填樹脂の絶対粘度を測定した。2つの複製を測定し、平均値を粘度(Pa・s)として報告した。
充填樹脂を室温で透明なガラスバイアル瓶に入れ、室温で沈降/相分離を観察した。粒子沈降が検出されなかったので、全ての充填樹脂実施例F1〜F7を、室温(約22℃)で少なくとも1ヶ月間安定であると判定した。4ヶ月後、F1、F2、F7のバイアル瓶の底部でいくらかの沈殿物を検出した。充填樹脂実施例F3、F4、F5、及びF6では、沈降を検出しなかった。
比較例CE−1〜CE−6及び実施例EX−1〜EX−6
385nm及び約23mW/cm2の出力のLED光源を使用して、Asiga Pico 2プリンタで、未充填樹脂及び充填樹脂をプリントした。ISO−4049標準に従って調製した曲げ試験棒(2×2×25mm)を、2x2がビルドプレートに面した状態でプリントした。プリンタの樹脂浴を、プリントの前に35〜40℃に加熱し、プリントできるように粘度を低下させた。各配合物のプリント温度を表5に列挙する。使用した設定は、スライス厚さ=50μm、バーンイン層=3、分離速度=10mm/秒、1層当たりのスライド数=1、バーンイン露光時間=15.0秒、通常露光時間=1.5秒であった。次にプリントされた棒をイソプロピルアルコールで洗浄して過剰な未硬化の樹脂を除去した。次いで、試験棒を、融合ランプ下で、各側で90分間ずつ後硬化させた。次に、後硬化された試験棒を、ISO−4049標準に従う3点曲げ治具内で試験した。後硬化された試験棒の曲げ強度及び曲げ弾性率を、メガパスカル(MPa)及びギガパスカル(GPa)でそれぞれ報告する。
上記データは、歯科用クラウンなどの恒久修復材(restoratives)に望ましい良好な曲げ強度及び曲げ弾性率を得るために、より多い粒子充填量(>50重量%)が必要であることを示唆している。低粒子充填量を有する比較例CE−5は、低い強度及び弾性率を示すのに対して、EX−1及びEX−4は、約125MPaに迫る強度を示し、この強度は、恒久修復材(restoratives)に使用される市販品であるCE−1に近い。1層ずつ重ねてプリントされているが、EX−1〜EX−6は、恒久歯科用修復物に必要な範囲で許容可能な特性を示す。
実施例EX−7
以下の設定を用いるASIGA PICO 2プリンタ上で充填樹脂F4を使用して歯科用クラウンを3Dプリントした。プリントに使用した設定は、スライス厚さ=50μm、バーンイン層=2、分離速度=10mm/秒、1層当たりのスライド数=1、バーンイン露光時間=20.0秒、通常露光時間=1.5、液槽温度=35℃であった。このクラウンを生成するために、市販の小児用クラウン(3M Stainless Steel)で3Dスキャン(3M Lava Scan)を行い、表面メッシュファイルを生成した。このファイルをGeomagic Studioにインポートし、これを加工して、300マイクロメートル厚のシェルを得た。STLファイルをエクスポートし、後加工ソフトウェア(Asiga)に送信し、ここで、支持体を積層し、スライスを生成した。プリント後、歯科用クラウンをビルドプレートから除去し、イソプロピルアルコールですすぎ、ASIGA UVチャンバ内で90分間後硬化させた。
Claims (15)
- 放射線硬化性組成物であって、
少なくとも1つの放射線硬質化性成分と、
光開始剤と、
50重量%以上の量のプリント可能な組成物の微粒子の集合を含む充填材料と、を含み、前記微粒子の集合は、粒径試験方法を使用して判定したときに体積平均基準で0.3マイクロメートルより大きいメジアン径(D50)を呈し、更に、前記放射線硬化性組成物は、粘度試験方法を使用して測定したときに150Pa・s未満の粘度を呈し、任意に、前記放射線硬化性組成物は、有機溶媒を実質的に含まない、放射線硬化性組成物。 - 前記少なくとも1つの放射線硬質化性成分が、エチレン性不飽和である、請求項1に記載の放射線硬化性組成物。
- 前記少なくとも1つの放射線硬質化性成分が、二量体、三量体、オリゴマー、及びこれらの組み合わせからなる群から選択され、任意に、前記放射線硬化性組成物が、重合性モノマーを実質的に含まない、請求項2に記載の放射線硬化性組成物。
- 前記光開始剤が、カチオン性光開始剤ではない、請求項1に記載の放射線硬化性組成物。
- 前記光開始剤が、光ラジカル光開始剤である、請求項4に記載の放射線硬化性組成物。
- 前記充填材料が、無機微粒子を含む、請求項1に記載の放射線硬化性組成物。
- 前記無機微粒子が、金属、金属合金、金属酸化物、金属窒化物、金属炭化物、炭素、及びこれらの組み合わせを含む、請求項6に記載の放射線硬化性組成物。
- 前記無機微粒子が、表面処理されている、請求項7に記載の放射線硬化性組成物。
- 前記微粒子の集合が、ナノ充填剤を含み、任意に、前記ナノ充填剤が、ナノクラスターを含む、請求項1に記載の放射線硬化性組成物。
- 溶媒、モノマー、(コ)ポリマー、乳化剤、重合阻害剤、吸収調整剤、光増感剤、着色剤、繊維強化材料、又はこれらの組み合わせからなる群から選択される少なくとも1種の添加剤を更に含む、請求項1に記載の放射線硬化性組成物。
- 複合材物品の製造方法であって、前記方法が、
(a)放射線硬化性組成物が、
少なくとも1つの放射線硬質化性成分と、
光開始剤と、
50重量%以上の量のプリント可能な組成物の微粒子の集合を含む充填材料と、を含み、前記微粒子の集合は、粒径試験方法を使用して判定したときに体積平均基準で0.3マイクロメートルより大きいメジアン径(D50)を呈し、更に、前記放射線硬化性組成物は、粘度試験方法を使用して測定したときに150Pa・s未満の粘度を呈し、任意に、前記放射線硬化性組成物は、有機溶媒を実質的に含まない、放射線硬化性組成物を提供するステップと、
(b)前記放射線硬化性組成物の一部分を化学線源に選択的に曝露して、前記放射線硬化性組成物の前記曝露部分を少なくとも部分的に硬化させ、それによって硬質化された層を形成するステップと、を含み、ステップ(a)及び(b)が繰り返されて、ニアネットシェイプ複合材物品を形成する、複合材物品の製造方法。 - 前記放射線硬化性組成物を加熱するステップ、未硬化放射線硬化性組成物を前記ニアネットシェイプ複合材物品から除去するステップ、前記ニアネットシェイプ複合材物品を溶媒で洗浄するステップ、又は前記ニアネットシェイプ複合材物品を加熱するステップ、のうちの少なくとも1つを更に含む、請求項11に記載の方法。
- 歯科用修復物である、請求項11に記載の方法に従って調製された複合材物品。
- 前記歯科用修復物が、クラウン、ブリッジ、インレー、オンレー、べニア、ポンティック、又はこれらの組み合わせからなる群から選択される、請求項13に記載の複合材物品。
- システムであって、
歯科用修復物の3Dモデルを表示するディスプレイと、
ユーザーによって選択された前記3Dモデルに応じて、積層造形方法を使用してニアネットシェイプ複合歯科用修復物を積層造形デバイスに作製させる、1つ以上のプロセッサと、を備え、前記積層造形方法が、
(a)放射線硬化性組成物が、
少なくとも1つの放射線硬質化性成分と、
光開始剤と、
50重量%以上の量のプリント可能な組成物の微粒子の集合を含む充填材料と、を更に含み、前記微粒子の集合は、粒径試験方法を使用して判定したときに体積平均基準で0.3マイクロメートルより大きいメジアン径(D50)を呈し、更に、前記放射線硬化性組成物は、粘度試験方法を使用して測定したときに150Pa・s未満の粘度を呈し、任意に、前記放射線硬化性組成物は、有機溶媒を実質的に含まない、放射線硬化性組成物を提供するステップと、
(b)前記放射線硬化性組成物の一部分を化学線源に選択的に曝露して、前記放射線硬化性組成物の前記曝露部分を少なくとも部分的に硬化させ、それによって硬質化された層を形成するステップと、を含み、ステップ(a)及び(b)が逐次的に又は連続的に繰り返されて、前記ニアネットシェイプ複合歯科用修復物を形成する、システム。
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US11553996B2 (en) | 2023-01-17 |
EP3681434A4 (en) | 2021-04-07 |
CN111050694B (zh) | 2022-04-12 |
KR102588065B1 (ko) | 2023-10-13 |
US20200197138A1 (en) | 2020-06-25 |
WO2019048963A1 (en) | 2019-03-14 |
JP7398364B2 (ja) | 2023-12-14 |
EP3681434A1 (en) | 2020-07-22 |
KR20200051623A (ko) | 2020-05-13 |
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