JPWO2019093334A1 - 靭性を向上させた歯科用製品 - Google Patents
靭性を向上させた歯科用製品 Download PDFInfo
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- JPWO2019093334A1 JPWO2019093334A1 JP2019552815A JP2019552815A JPWO2019093334A1 JP WO2019093334 A1 JPWO2019093334 A1 JP WO2019093334A1 JP 2019552815 A JP2019552815 A JP 2019552815A JP 2019552815 A JP2019552815 A JP 2019552815A JP WO2019093334 A1 JPWO2019093334 A1 JP WO2019093334A1
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- porcelain
- zirconia
- oxide
- dental
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- A61C8/0013—Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools characterised by the material or composition, e.g. ceramics, surface layer, metal alloy with a surface layer, coating
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Abstract
Description
[1]ジルコニア焼結体からなる基材と陶材層を含む歯科用製品であって、前記陶材の適正焼成温度が900℃以上であり、且つ前記陶材層の破壊靭性値が1.20MPa・m0.5以上である、歯科用製品;
[2]前記陶材層の厚さが10〜500μmである、前記[1]に記載の歯科用製品;
[3]前記ジルコニア焼結体からなる基材が安定化剤を含む、前記[1]又は[2]に記載の歯科用製品;
[4]前記安定化剤が、酸化イットリウム、酸化チタン、酸化カルシウム、酸化マグネシウム、酸化セリウム、酸化アルミニウム、酸化スカンジウム、酸化ランタン、酸化エルビウム、酸化プラセオジム、酸化サマリウム、酸化ユウロピウム及び酸化ツリウムからなる群から選ばれる少なくとも1種である、前記[3]に記載の歯科用製品;
[5]前記陶材の適正焼成温度が1100℃以上である、前記[1]〜[4]のいずれかに記載の歯科用製品;
[6]以下の関係式を満たす、前記[1]〜[5]のいずれかに記載の歯科用製品;
0<{(前記陶材の熱膨張係数)/(前記ジルコニア焼結体の熱膨張係数)}<1.0
[7]以下の関係式を満たす、前記[6]に記載の歯科用製品;
1.0×10−6K−1≦(前記ジルコニア焼結体の熱膨張係数)−(前記陶材の熱膨張係数)≦4.5×10−6K−1
[8]ジルコニア焼結体上に陶材層を成形し、1350℃以上の温度にて焼成する工程を含む、前記[1]〜[7]のいずれかに記載の歯科用製品の製造方法;
[9]ジルコニア仮焼体上に陶材層を成形し、前記ジルコニア仮焼体の適正焼成温度以上の温度にて、ジルコニア仮焼体を焼成し且つ陶材を焼成する工程を含む、[1]〜[7]のいずれかに記載の歯科用製品の製造方法;
[10]歯科用補綴物、歯列矯正用製品、及び歯科インプラント用製品からなる群から選ばれる少なくとも1種である、[1]〜[7]のいずれかに記載の歯科用製品;
(1)ジルコニア焼結体の上に陶材層を成形し、1350℃以上の温度にて焼成する工程を含む製造方法;
(2)ジルコニア仮焼体の上に陶材層を成形し、前記ジルコニア仮焼体の適正焼成温度以上の温度にて、ジルコニア仮焼体を焼成し且つ陶材を焼成する工程を含む製造方法、
が挙げられる。図1を参照しながら製造方法について説明する。
各実施例及び比較例に用いる陶材の製造方法として、まず、表1に記載の組成を有するように、Si元素、Al元素、Li元素、Na元素、K元素、Ca元素、Mg元素、Zn元素、B元素、Ce元素をそれぞれ含有する、SiO2、Al2O3、Li2O、Na2O、K2O、CaO、MgO、ZnO、B2O3、CeO2を用いて、各化合物を混合し原料混合物とした。次に、得られた原料混合物(組成物)を加熱して熔融し、得られた熔融体を冷却したうえでカレット化し、さらに得られたカレットを、ボールミルを用いて粉砕した。その後、得られた粉砕物を#200メッシュの篩を通過させ、ふるい分けすることによって、粉末状の陶材を作製した。前記熔融温度は1500℃とし、また、熔融時間は120分とした。
まず、前述の製造例1〜5により得られた粉末状の陶材に対して、精製水を使用しスラリーを作製した。次に、各陶材のスラリーを直径約13mm、厚さ約1.5mmの金型に流し込み、乾燥させることで円柱状の固形物の試料を作製した。作製した固形物の試料をSKメディカル電子株式会社製の焼成炉「セラフュージョンBX」を使用して焼成を行った。円柱状の焼成後の各陶材の外観を、株式会社ハイロックス製「デジタルマイクロスコープKH−7700」を用いて観察した。焼成後の各陶材の表面の粗さと透明度に基づき、以下の基準により各陶材の適正焼成温度を決定した。図2の左側の陶材のように、表面が滑沢で、透明度が高く背景が透過する状態は、陶材が十分に焼成されているとみなすことができる。一方、図2の右側の陶材のように、表面が粗造で透明度の低い状態は、焼成不足と判断できる。本発明において、図2の左側の陶材のように十分に焼成されているとみなすことができる最低の温度を陶材の適正焼成温度と判断した。製造例1〜5における陶材の適正焼成温度を表1に示す。
ISO 6872:2015に準拠して熱膨張係数を測定した。まず、前述の製造例1〜5により得られた粉末状の陶材に対して、精製水を使用しスラリーを作製した。次に、各スラリーを前記ISO規格に従ったサイズの金型に流し込み、乾燥させることで角柱状試料を作製した。作製した角柱状試料をSKメディカル電子株式会社製の焼成炉「セラフュージョンBX」を使用して、表1に示す各適正焼成温度で1分間の条件の下で焼成を行った。焼成後の角柱状試料を前記ISO規格に従い寸法調整をし、熱膨張係数測定の試料とした。熱膨張係数の解析温度範囲は25℃〜500℃とした。測定は、10K/分の昇温させて行った。測定装置は、熱機械分析装置(商品名:Thermo plus TMA8310、株式会社リガク製)を使用した。製造例1〜5における各陶材の熱膨張係数を表1に示す。
ジルコニア仮焼体を、厚さが約1.5mmの試料に切り出し、SKメディカル電子株式会社製の焼成炉「ノリタケ カタナ(登録商標) F−1N」を使用して焼成を行った。試料の形状は、四角形でも円形でもよい。焼成後の厚さが約1.2mmになるように、各ジルコニア仮焼体からなる試料を製造した。得られた試料の外観を目視にて観察し、試料の透明度に基づき以下の基準により各ジルコニア仮焼体の適正焼成温度を決定した。図3の左側の試料のように、透明度が高く背景が透過する状態は、ジルコニア仮焼体が十分に焼成されているとみなすことができる。一方、図3の右側の試料のように、透明度の低い状態あるいは白濁した状態は、焼成不足と判断できる。本発明において、図3の左側の試料のように十分に焼成されているとみなすことができる最低の温度をジルコニア仮焼体の適正焼成温度と判断した。本実施例及び比較例で用いたジルコニア仮焼体と、その適正焼成温度はそれぞれ、クラレノリタケデンタル株式会社製「ノリタケ カタナ(登録商標) ジルコニア」KT(適正焼成温度:1375℃)、「ノリタケ カタナ(登録商標) ジルコニア」HT/ML(適正焼成温度:1500℃)、「ノリタケ カタナ(登録商標) ジルコニア」STML(適正焼成温度:1550℃)、「ノリタケ カタナ(登録商標) ジルコニア」UTML(適正焼成温度:1550℃)、株式会社ニッシン製「ベレッツァ ハイトランス ジルコニア」(適正焼成温度:1450℃)である。
ジルコニア焼結体について、ISO 6872:2015に準拠して熱膨張係数を測定した。熱膨張係数の解析温度範囲は25℃〜500℃とした。以下に、試料の作製方法を説明する。ジルコニアの仮焼体として、ジルコニアディスクであるクラレノリタケデンタル株式会社製「ノリタケ カタナ(登録商標) ジルコニア」HT/ML、「ノリタケ カタナ(登録商標) ジルコニア」STML、「ノリタケ カタナ(登録商標) ジルコニア」UTML、及び株式会社ニッシン製「ベレッツァ ハイトランス ジルコニア」、また、ジルコニアブロックであるクラレノリタケデンタル株式会社製「ノリタケ カタナ(登録商標) ジルコニア」KT(20.0mm×40.0mm×75.0mm)を準備した。各ジルコニアの仮焼体をそれぞれの適正焼成温度で120分焼成してジルコニア焼結体を作製し、熱膨張係数測定の試料とした。熱膨張係数の測定は、上記した陶材の熱膨張係数の測定と同様に行った。測定結果を表2に示す。
陶材層の破壊靭性値の測定は、本発明の歯科用製品に相当する、ジルコニア焼結体からなる基材と陶材層を含む複合体の試料を作製して行った。まず、安定化剤としてイットリアを含有する市販製品のジルコニア仮焼体として、クラレノリタケデンタル株式会社製「ノリタケ カタナ(登録商標) ジルコニア」HT/MLを用いて、平板状(縦:約20mm、横:約20mm、厚さ:約1.5mm)に切り出した。次に、SKメディカル電子株式会社製の焼成炉「ノリタケ カタナ(登録商標) F−1N」を使用して室温より昇温し、各ジルコニア仮焼体の適正焼成温度で120分間焼成をして、各ジルコニア焼結体を作製した。次に、50μmのアルミナ粒子を用いて0.2MPaの圧力で、得られたジルコニア焼結体の一方の面をサンドブラスト処理して、ジルコニア焼結体上に陶材層を形成するための前準備を行った。このサンドブラスト処理によって、処理面はつや消し状態となった。次に、アセトン中で基材を超音波洗浄した後、乾燥させた。
次に審美性及びクラック発生有無の評価用ジルコニア焼結体フレームを作製した。まず、印象材と呼ばれる型取り材を用い、支台歯、その対合歯及び支台歯周囲の歯列のメス型を採った。次に、そこへ石膏を流し込みオス型の石膏模型を作製し、支台歯、その対合歯及び支台歯周囲の歯列を再現した。次に、ワックスを用いて、石膏模型の支台歯上に、噛み合わせ、形状、寸法等を合わせたワックス冠を形成した。このワックス冠は、フレーム形成の基礎となるものである。次に、ワックス冠において、フレームに陶材を塗布する領域の表面を深さ約0.2mm削り落とした。次に、石膏模型の支台歯及びワックス冠を、クラレノリタケデンタル株式会社製「カタナ(登録商標) デンタルスキャナー D750」を用いて光学スキャンして、支台歯及びワックス冠のデジタル化した3次元データを得た。なお、本実施例では、石膏模型を光学スキャンしたが、口腔内スキャナにより直接口腔内を光学スキャンしてもよい。また、ワックス冠を用いずに、石膏模型を光学スキャンした後、3次元CADソフトを用いて仮想的なフレーム形状に基づく3次元データを作製してもよい。
陶材層の破壊靭性値の測定は、本発明の歯科用製品に相当する、ジルコニア焼結体からなる基材と陶材層を含む複合体の試料を作製して行った。まず、安定化剤としてイットリアを含有する市販製品のジルコニア仮焼体として、クラレノリタケデンタル株式会社製「ノリタケ カタナ(登録商標) ジルコニア」KT、「ノリタケ カタナ(登録商標) ジルコニア」HT/ML、「ノリタケ カタナ(登録商標) ジルコニア」STML、「ノリタケ カタナ(登録商標) ジルコニア」UTML、及び株式会社ニッシン製「ベレッツァ ハイトランス ジルコニア」を用いて、平板状(縦:約20mm、横:約20mm、厚さ:約1.5mm)に切り出した。切り出した各ジルコニア仮焼体上に、各製造例で得られた粉末状の陶材をスラリー化し、焼成後の厚さが「表2に記載の陶材厚さ+100μm以上」となるように該スラリーを塗布して陶材層を成形し、SKメディカル電子株式会社製の焼成炉「ノリタケ カタナ(登録商標) F−1N」を使用して室温より昇温し、各ジルコニア仮焼体の適正焼成温度以上して表2に記載の温度で、いずれも120分間焼成をすることで、ジルコニア仮焼体を焼成させ、且つ陶材層も同時に焼成を行った。ジルコニア焼結体上で焼成した陶材層を表2に記載の厚さになるように寸法調整した後に、最終仕上げとして表面を2000番のサンドペーパーで研磨処理し、ジルコニア焼結体からなる基材と陶材層を含む複合体の試料を作製した。得られた試料を用いて、陶材層の破壊靭性値を、試験荷重を49Nとして、JIS R 1607:2015に準拠して圧子圧入法(IF法)によって測定した。陶材層の破壊靭性値を測定することにより、歯科用製品として十分な耐久性を有するかどうかを確認した。また、上記測定後の試料表面を目視にて観察し、チッピング発生の有無を評価した。結果を表2に示す。
審美性及びクラック発生有無の評価については、前述の実施例1〜9及び比較例1〜5の方法と同様にして、歯科用製品の下部構造となるジルコニア仮焼体のフレームを作製する。但し、この時点では焼成は行わず、該フレーム上に、各製造例で得られた粉末状の陶材をスラリー化し、焼成後の厚さが「表2に記載の陶材厚さ+100μm以上」となるように該スラリーをジルコニア仮焼体のフレーム上に塗布した。その後、SKメディカル電子株式会社製の焼成炉「ノリタケ カタナ(登録商標) F−1N」を使用して、表2に記載の試験時焼成温度、及び試験時係留時間の条件で、ジルコニア仮焼体を焼成し、且つ陶材層を焼成し、試料を作製した。試料表面を目視にて観察し、審美性とクラック発生の有無を評価した。なお、審美性は、焼成後の試料に白濁が見られないものを「良好」、明確な白濁が見られるものを「不良」と判断した。結果を表2に示す。
2 ジルコニア焼結体
3 陶材層
Claims (10)
- ジルコニア焼結体からなる基材と陶材層を含む歯科用製品であって、前記陶材の適正焼成温度が900℃以上であり、且つ前記陶材層の破壊靭性値が1.20MPa・m0.5以上である、歯科用製品。
- 前記陶材層の厚さが10〜500μmである、請求項1に記載の歯科用製品。
- 前記ジルコニア焼結体からなる基材が安定化剤を含む、請求項1又は2に記載の歯科用製品。
- 前記安定化剤が、酸化イットリウム、酸化チタン、酸化カルシウム、酸化マグネシウム、酸化セリウム、酸化アルミニウム、酸化スカンジウム、酸化ランタン、酸化エルビウム、酸化プラセオジム、酸化サマリウム、酸化ユウロピウム及び酸化ツリウムからなる群から選ばれる少なくとも1種である、請求項3に記載の歯科用製品。
- 前記陶材の適正焼成温度が1100℃以上である、請求項1〜4のいずれか1項に記載の歯科用製品。
- 以下の関係式を満たす、請求項1〜5のいずれか1項に記載の歯科用製品。
0<{(前記陶材の熱膨張係数)/(前記ジルコニア焼結体の熱膨張係数)}<1.0 - 以下の関係式を満たす、請求項6に記載の歯科用製品。
1.0×10−6K−1≦(前記ジルコニア焼結体の熱膨張係数)−(前記陶材の熱膨張係数)≦4.5×10−6K−1 - ジルコニア焼結体上に陶材層を成形し、1350℃以上の温度にて焼成する工程を含む、請求項1〜7のいずれか1項に記載の歯科用製品の製造方法。
- ジルコニア仮焼体上に陶材層を成形し、前記ジルコニア仮焼体の適正焼成温度以上の温度にて、ジルコニア仮焼体を焼成し且つ陶材を焼成する工程を含む、請求項1〜7のいずれか1項に記載の歯科用製品の製造方法。
- 歯科用補綴物、歯列矯正用製品、及び歯科インプラント用製品からなる群から選ばれる少なくとも1種である、請求項1〜7のいずれか1項に記載の歯科用製品。
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