JP2019163246A - イットリア含有量の異なる多層構造ジルコニア - Google Patents
イットリア含有量の異なる多層構造ジルコニア Download PDFInfo
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- JP2019163246A JP2019163246A JP2019048083A JP2019048083A JP2019163246A JP 2019163246 A JP2019163246 A JP 2019163246A JP 2019048083 A JP2019048083 A JP 2019048083A JP 2019048083 A JP2019048083 A JP 2019048083A JP 2019163246 A JP2019163246 A JP 2019163246A
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- layer
- ceramic
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- dental zirconia
- zirconia blank
- Prior art date
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 160
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 title 1
- 239000000919 ceramic Substances 0.000 claims abstract description 95
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 41
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims description 43
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 36
- 230000035699 permeability Effects 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 15
- 239000011164 primary particle Substances 0.000 claims description 12
- 230000005484 gravity Effects 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims 1
- 229910052726 zirconium Inorganic materials 0.000 claims 1
- 238000003475 lamination Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 103
- 238000005452 bending Methods 0.000 description 17
- 235000019646 color tone Nutrition 0.000 description 14
- 239000003086 colorant Substances 0.000 description 14
- 238000000034 method Methods 0.000 description 12
- 238000005245 sintering Methods 0.000 description 11
- 238000005520 cutting process Methods 0.000 description 10
- 238000004040 coloring Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 210000003298 dental enamel Anatomy 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000010304 firing Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000000465 moulding Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 210000000214 mouth Anatomy 0.000 description 4
- 229910052573 porcelain Inorganic materials 0.000 description 4
- 238000013001 point bending Methods 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 239000005354 aluminosilicate glass Substances 0.000 description 2
- 150000001869 cobalt compounds Chemical class 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 229910052602 gypsum Inorganic materials 0.000 description 2
- 239000010440 gypsum Substances 0.000 description 2
- 150000002506 iron compounds Chemical class 0.000 description 2
- 239000003103 lithium disilicate glass Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 150000001845 chromium compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 201000005299 metal allergy Diseases 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000003114 praseodymium compounds Chemical class 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 150000003682 vanadium compounds Chemical class 0.000 description 1
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Abstract
Description
しかし、単冠において曲げ強度500MPaは十分な強度であると言えるが、ブリッジ等の複数ユニットの補綴装置の場合、500MPaでは十分な強度を有しているとは言えない。特に、連結部には、咬合等により大きな力が加わることとなり、より高い曲げ強度を有していることが求められる。
本発明の目的は、高透過で天然歯に近い色調再現が可能であり口腔内で耐えられる強度を有する歯科用ジルコニアブランクを提供する。さらに、高い強度を有した、4ユニット以上の補綴装置も作製可能な歯科用ジルコニアブランクを提供することである。
本発明においては、第1の層は、高透過性セラミックスにおける酸化ジルコニウムの含有率及び/又は酸化イットリウムの含有率が互いに異なる複数の高透過性層状領域を有することが好ましい。
本発明においては、少なくとも一つの高透過性層状領域が、酸化エルビウムを0.0001〜0.30 mol%含有することが好ましい。
本発明においては、第2の層は、組成が互いに異なる複数の低透過性層状領域から構成されていることが好ましい。
本発明においては、第2の層は、低透過性セラミックスにおける酸化ジルコニウムの含有率及び/又は酸化イットリウムの含有率が互いに異なる複数の低透過性層状領域を有することが好ましい。
本発明においては、少なくとも一つの低透過性層状領域が、酸化エルビウムを0.0001〜0.30 mol%含有することが好ましい。
本発明においては、高透過性セラミックスは、組成の異なる複数のセラミックス粉末の仮焼体であることが好ましい。
本発明においては、低透過性セラミックスは、組成の異なる複数のセラミックス粉末の仮焼体であることが好ましい。
本発明においては、第1の層は、第1の層が位置する歯科用ジルコニアブランクの積層方向の一端側の表面の重心からの垂線上における、一端側の表面と対向する他端側の表面までの寸法の5〜40%の範囲まで位置していることが好ましい。
本発明においては、高透過性セラミックスを構成するセラミックス粉末及び低透過性セラミックスを構成するセラミックス粉末は、BET比表面積の差が2m2/gの範囲であり、かつ、平均1次粒子径の差が20nmの範囲であることが好ましい。
本発明においては、少なくとも1つの高透過性層状領域の透明性が、第2の層の透明性よりも高く、第1の層のL*a*b*表色系による色度をLE、aE、bEで表した時、LEが65.0以上82.0以下であり、aEが-4.0以上2.0以下であり、bEが0.0以上20.0以下であることが好ましい。
本発明においては、第1の層の透明性が、第2の層の透明性よりも高く、第1の層のL*a*b*表色系による色度をLE、aE、bEで表した時、LEが65.0以上82.0以下であり、aEが-4.0以上2.0以下であり、bEが0.0以上20.0以下であることが好ましい。
本発明においては、第1の層が、酸化エルビウムを0.0001〜.00 mol%含有することが好ましい。
本発明においては、第2の層が、酸化エルビウムを0.0001〜1.00 mol%含有することが好ましい。
本発明においては、低透過性セラミックスは、酸化ジルコニウム及び酸化イットリウムからなることが好ましい。
本発明においては、第1の層は高透過性セラミックスからなることが好ましい。
本発明においては、第2の層は低透過性セラミックスからなることが好ましい。
本発明においては、歯科用ジルコニアブランクは、第1の層及び第2の層からなることが好ましい。
歯科用ジルコニアブランクは、CAD/CAM技術による切削加工に使用される。歯科用ジルコニアブランクは焼結体もしくは半焼結体で提供される。より好ましくは半焼結体で提供される。半焼結体で提供された歯科用ジルコニアブランクはCAD/CAM技術による切削加工後に再焼成され、焼結体として、口腔内で用いられる。
歯科用ジルコニアブランクの形状は、円柱体であるディスクタイプでも、立方体もしくは直方体であるブロックタイプでも良い。
高透過性セラミックスを構成するセラミックス粉末と低透過性セラミックスを構成するセラミックス粉末はBET比表面積の差が2m2/gの範囲で且つ、平均1次粒子径の差が20nmの範囲であることが好ましい。さらに、BET比表面積の差が1m2/gの範囲であり、且つ平均1次粒子径の差が10nmの範囲であることが好ましい。
これらのBET比表面積や平均1次粒子径の差が大きいセラミックス粉末を積層成型して焼結した場合、ジルコニアブランク成型体の歪みが生じることとなる。特に、半焼結体のジルコニアブランクから削り出す場合、ブランク自体が歪んで反りが発生する、最終焼結時に補綴装置が割れる、適合が合わない、等の不具合が生じる。
(各層におけるセラミックス粉末の調合)
それぞれの平均1次粒子径が40-90nm、BET比表面積は7-13m2/gである市販のジルコニア粉末、酸化イットリウム含有ジルコニア粉末、酸化エルビウム含有ジルコニア粉末及び着色材含有ジルコニア粉末を用いた。
ジルコニア粉末、酸化イットリウム含有ジルコニア粉末、酸化エルビウム含有ジルコニア粉末及び着色剤含有ジルコニア粉末を用いて、表に示す組成となる様に調合し、第1の層及び第2の層に用いるセラミックス粉末を得た。セラミックス粉末は目的とする色に合わせて微量の鉄化合物、コバルト化合物の着色剤が配合されている。
(歯科用ジルコニアブランクの成型方法)
各セラミックス粉末を直径100mmの金型に、表に記載の順番に第1の層側から必要な量を充填後、10kNの圧力で1分間プレス成型を行った。試験体の形状を図1に示す。図1の上部が第1の層であり、下部が第2の層である。
プレス成型を行った後200MPaの圧力で1分間CIP成型を行った。プレス成型体の脱脂は、50℃/hの昇温速度で500℃まで昇温し、2時間係留後、100℃/hの降温速度で室温まで冷却した。脱脂後、100℃/hの昇温速度で1000〜1200℃まで昇温し、2時間係留後、炉内放冷をして予備焼結体であるジルコニアブランクを得た。
上記方法で成型した歯科用ジルコニアブランク(半焼結体)について、反りの有無を確認した。凸に変形した面を下にして設置した時、設置面から前記底面までの距離をデジタルマイクロスコープVHX-5000(KEYENCE社)を用いて測定した。10箇所測定して、最大距離が1mm以内である場合は○、1mmを越える場合は×として判定した。
前歯6本の支台歯形成を行った石こう模型に、6本ブリッジのワックスアップを行い、D2000(3shape社)のスキャナを用いて6本ブリッジのデータを取り込み、DWX-50(ローランド社製)の加工機を用いて、上記方法で成型した歯科用ジルコニアブランクから、データを取り込んだ6本ブリッジを加工し、5℃/minの昇温速度で1450℃まで昇温し、2時間係留後、室温まで炉内放冷して焼結体とし、適合性を確認した。焼結した6本ブリッジを石こう模型に戻した際に、ガタツキ無く適合する場合は○、ガタツキがあり適合しない場合は×として判定した。
上記方法で成型した歯科用ジルコニアブランクの第1の層及び第2の層の積層方向における45〜55%の部分から、試験体を加工し、5℃/minの昇温速度で1450℃まで昇温し、2時間係留後、室温まで炉内放冷して焼結体とし、さらに平面研磨により、幅4mm、厚さ1.2mm、長さ16mmの曲げ試験体を作製した。曲げ試験は、ISO 6872 : 7.3 Flexural strength に準じて行い、支点間距離は12mmとした。第1の層の曲げ強度は300MPa以上で臨床上使用可能とした。また第2の層の曲げ強度は、1000MPa以上で臨床上使用可能とした。
(色調及びコントラスト比測定)
上記方法で成型した歯科用ジルコニアブランクの各層から、試験体を加工し、5℃/minの昇温速度で1450℃まで昇温し、2時間係留後、室温まで炉内放冷して焼結体とし、さらに平面研磨により、直径14mm、厚さ1.2mmの丸板を作製した。色調の測定は分光測色計(CM-5:コニカミノルタ)を用いて、白バック測色の色度(L*、a*、b*)を測定した。また、白バック及び黒バック上において測色し、測定したそれぞれのY値(白バック上で測色したY値をYW、黒バック上で測色したY値をYBとする)を用いて、
(コントラスト比)=1-(1-YB/YW)
の式からコントラスト比を算出した。第1の層のコントラスト比は、着色材を含まない場合は0.71以下、着色材を含む場合は、0.75-0.85を臨床上使用可能とした。第2の層のコントラスト比は、着色材を含まない場合は0.70以上、着色材を含む場合は、0.80-0.90を臨床上使用可能とした。
比較例1は、第1の層における曲げ強度が不足していた。
比較例2は、仮焼成時の反りが1mmより大きく、本焼結時のガタツキがあり適合性は良くなかった。
比較例3は第1の層におけるコントラスト比が高く、十分な審美性が得られなかった。
比較例4は第1の層及び第2の層におけるコントラスト比に差がなく、十分な審美性が得られなかった。
比較例5は第2の層におけるコントラスト比が低く、十分な審美性が得られなかった。
比較例6は焼結体が崩壊してしまい、試験を行うことができなかった。
2 第2の層(ボディ層)
Claims (15)
- 複数の層を有する歯科用ジルコニアブランクであって、
酸化ジルコニウムを91.6-96.5mol%および酸化イットリウムを3.5〜8.4 mol%含有する高透過性セラミックスから構成される第1の層と、
酸化ジルコニウムを95.6-98.5mol%および酸化イットリウムを1.5〜4.4 mol%含有する低透過性セラミックスから構成される第2の層と、を含み、
低透過性セラミックスの酸化イットリウムの含有率は、高透過性セラミックスの酸化イットリウムの含有率より0.5-5.4 mol%少なく、
第1の層は、複数の層の積層方向の一端に位置することを特徴とする歯科用ジルコニアブランク。 - 第1の層は、組成が互いに異なる複数の高透過性層状領域から構成されていることを特徴とする請求項1の歯科用ジルコニアブランク。
- 第1の層は、高透過性セラミックスにおける酸化ジルコニウムの含有率及び/又は酸化イットリウムの含有率が互いに異なる複数の高透過性層状領域を有することを特徴とする請求項2の歯科用ジルコニアブランク。
- 少なくとも一つの高透過性層状領域が、酸化エルビウムを0.0001〜0.30 mol%含有することを特徴とする請求項2〜3のいずれかの歯科用ジルコニアブランク。
- 第2の層は、組成が互いに異なる複数の低透過性層状領域から構成されていることを特徴とする請求項1〜4のいずれかの歯科用ジルコニアブランク。
- 第2の層は、低透過性セラミックスにおける酸化ジルコニウムの含有率及び/又は酸化イットリウムの含有率が互いに異なる複数の低透過性層状領域を有することを特徴とする請求項5の歯科用ジルコニアブランク。
- 少なくとも一つの低透過性層状領域が、酸化エルビウムを0.0001〜0.30 mol%含有することを特徴とする請求項5〜6のいずれかの歯科用ジルコニアブランク。
- 高透過性セラミックスは、組成の異なる複数のセラミックス粉末の仮焼体であることを特徴とする請求項1〜7のいずれかの歯科用ジルコニアブランク。
- 低透過性セラミックスは、組成の異なる複数のセラミックス粉末の仮焼体であることを特徴とする請求項1〜8のいずれかの歯科用ジルコニアブランク。
- 第1の層は、第1の層が位置する歯科用ジルコニアブランクの積層方向の一端側の表面の重心からの垂線上における、一端側の表面と対向する他端側の表面までの寸法の5〜40%の範囲まで位置していることを特徴とする請求項1〜9のいずれかの歯科用ジルコニアブランク。
- 高透過性セラミックスを構成するセラミックス粉末及び低透過性セラミックスを構成するセラミックス粉末は、BET比表面積の差が2m2/gの範囲であり、かつ、平均1次粒子径の差が20nmの範囲であることを特徴とする請求項1〜10の歯科用ジルコニアブランク。
- 少なくとも1つの高透過性層状領域の透明性が、第2の層の透明性よりも高く、
前記少なくとも1つの高透過性層状領域のL*a*b*表色系による色度をLE、aE、bEで表した時、
LEが65.0以上82.0以下であり、
aEが-4.0以上2.0以下であり、
bEが0.0以上20.0以下であることを特徴とする請求項2〜4のいずれかの歯科用ジルコニアブランク。 - 第1の層の透明性が、第2の層の透明性よりも高く、
第1の層のL*a*b*表色系による色度をLE、aE、bEで表した時、
LEが65.0以上82.0以下であり、
aEが-4.0以上2.0以下であり、
bEが0.0以上20.0以下であることを特徴とする請求項1〜12のいずれかの歯科用ジルコニアブランク。 - 第1の層が、酸化エルビウムを0.0001〜0.30 mol%含有することを特徴とする請求項1〜13のいずれかの歯科用ジルコニアブランク。
- 第2の層が、酸化エルビウムを0.0001〜0.30 mol%含有することを特徴とする請求項1〜14のいずれかの歯科用ジルコニアブランク。
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