JP2015127294A - 加工性ジルコニア及び加工性ジルコニアの製造方法 - Google Patents
加工性ジルコニア及び加工性ジルコニアの製造方法 Download PDFInfo
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- JP2015127294A JP2015127294A JP2014266166A JP2014266166A JP2015127294A JP 2015127294 A JP2015127294 A JP 2015127294A JP 2014266166 A JP2014266166 A JP 2014266166A JP 2014266166 A JP2014266166 A JP 2014266166A JP 2015127294 A JP2015127294 A JP 2015127294A
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- zirconia
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- workable
- temperature
- sintered body
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 280
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 37
- 239000002131 composite material Substances 0.000 claims abstract description 26
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims description 63
- 238000000034 method Methods 0.000 claims description 36
- 230000008569 process Effects 0.000 claims description 27
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 26
- 238000001513 hot isostatic pressing Methods 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 7
- 239000008187 granular material Substances 0.000 claims description 6
- 239000011858 nanopowder Substances 0.000 claims description 5
- 238000001694 spray drying Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 description 27
- 238000012423 maintenance Methods 0.000 description 19
- 230000008859 change Effects 0.000 description 15
- 238000012360 testing method Methods 0.000 description 13
- 239000000919 ceramic Substances 0.000 description 9
- 230000007423 decrease Effects 0.000 description 9
- 239000000654 additive Substances 0.000 description 8
- 230000000996 additive effect Effects 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- 230000000704 physical effect Effects 0.000 description 8
- 230000003247 decreasing effect Effects 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 230000007704 transition Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 239000011351 dental ceramic Substances 0.000 description 5
- 238000007373 indentation Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 210000000214 mouth Anatomy 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000004814 ceramic processing Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 238000002054 transplantation Methods 0.000 description 2
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
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- 230000000711 cancerogenic effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000010730 cutting oil Substances 0.000 description 1
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- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000004053 dental implant Substances 0.000 description 1
- 239000005548 dental material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000006355 external stress Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
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- 238000005728 strengthening Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 1
Classifications
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
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- 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
- A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
- A61K6/818—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising zirconium oxide
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Abstract
Description
緻密化と微細粒径のために、本発明においては、2つの段階で加工性ジルコニアの焼結を施した。すなわち、第1の段階の温度に上昇させた後、維持温度で一定時間維持した後、再び第2の段階の温度に上昇させて焼結を施した。
<a.TiO2が添加された加工性ジルコニア>
ZrO2粉末(KZ−0Y、Kyoritsu)と、Y2O3(Uranos Chem.)と、Nb2O5とを前述した組成比で混合し、24時間の間、ボールミルを施した。得られた混合粉末を乾燥させた後、混合粉末をか焼させ、後に、ジルコニアのボールで3時間の間、アトリションミルを施して、焼成工程中に大きくなった粉末をおろし、微細な化合物を得た。粉末を再度乾燥させた後、125メッシュの篩でふるい分けを施して、加工性ジルコニア粉末((Y、Nb)−TZP)を準備した。
加工性ジルコニア粉末に対し、水熱合成法により合成したCeO2を添加し、前述した実施例と同様の方法で成形及び焼結を施した後、物性の変化を観察した。CeO2の添加量を1〜7質量%で変化させた試験片のそれぞれについて、密度及び硬度の変化を図8A及び図8Bに示した。密度の値は、CeO2の添加量を2質量%まで増加させることで99.5%に達し、これ以上の添加量では変化がなかった。一方、強度は、約3質量%の添加量までの範囲で徐々に増加していき、これ以上では、CeO2の添加量に応じて直線的に減少した。これは、安定化剤としてCeO2が破折時に正方晶相から単斜晶相への相転移を抑制させることにより靭性が低下し、その結果、線形破壊力学に基づいて、これに比例して強度が減少したと推測される。また、CeO2の添加は、ジルコニアの粒径を大きくすることで、この場合にも、粒径の粗大化に伴う強度が低下することを予想することができる。この硬度は、8.7GPaから4質量%添加時の9.4GPaまで一定に増加し、これ以上の添加では、緩やかな減少を示した。これは、4質量%までCeO2の添加が、圧痕時の変形を減少させる効果があることを意味する。一方、3質量%以上のCeO2の添加の場合、この強度が低下し、添加量が3質量%以上に増加すればするほど、試験片の色がますます濃くなることを確認した。
加工性ジルコニア粉末へのTiO2の添加量を2質量%で固定した状態で、CeO2の添加量を1.5〜5質量%まで変化させた試験片を準備し、得られた試験片の物性の変化を観察した。この添加量に応じた密度の変化と、強度及び硬度の変化を、図9A及び図9Bにそれぞれ示した。TiO2の添加量を固定し、CeO2の添加量を変化させる場合には、密度の変化と、強度及び硬度の変化の両方が、CeO2の添加量と反比例して減少する傾向を示した。
TiO2とCeO2の同時添加の実験で硬度が低くなる場合には、密度と強度は低下しているので、これを補償するために、加工性ジルコニア粉末に対しSiO2を少量添加し、全体的な密度及び硬度の変化を観察した。TiO2とCeO2が添加されたジルコニアの密度は、0.02質量%のSiO2の添加により増加し、0.08質量%のSiO2を添加するまで概ね増加する密度を維持した。
400MPa以上の強度と低い硬度を有する、1〜2質量%のTiO2が添加されたジルコニア粉末を、1650℃で40時間の間焼結することにより、加工性実験用ジルコニアブロックを製造した。加工装置(製品名:Mynx400、メーカー:Daewoo、Korea)に、直径3mmのダイヤモンドドリルを装着し、切削油を給油しながら加工を施した。この加工装置のドリルは、回転速度が5000rpm、フィード速度が18mm/sec、切込み量が0.15mmになるように固定した。加工性は、このドリルが試験片を歯の表面から6mmの深さまで加工して到達するのにかかる時間を測定することにより判断した。表5は、3mmのドリルが6mmの深さまで加工するのにかかる平均加工時間を示している。
セラミックの透光性(translucency)は、歯科治療の修復用のセラミックとして使用する上での機械的な特性に加えて、重要な要件の一つである。図12に示すように、本発明に係るジルコニアの透光性は、空気中で通常の焼結を施した場合よりも、焼結後に追加で熱間等方加圧(hot isostatic press、HIP)処理を施した場合に顕著に向上した。すなわち、本発明に係る組成の一つである、90.6mol%ZrO2、5.3mol%Y2O3、4.1mol%Nb2O5の組成を有するジルコニアを、空気中、1650℃で5時間の間焼結した試験片(as−sintered)の透光度よりも、焼結後に追加で、1500℃でHIP処理を施す場合の透光度が、約40%まで増加した。透光度は、HIP温度に比例して増加し、1450℃よりも高い温度でHIP処理を施した後の透光度は、現在の歯科治療の修復材として使用される歯科用のジルコニア(3Y−TZP)の透光度よりも高かった。
Claims (8)
- 79.8〜92mol%のZrO2及び4.5〜10.2mol%のY2O3と、3.5〜7.5mol%のNb2O5又は5.5〜10.0mol%のTa2O5と、を含む正方晶ジルコニア複合粉末と、
前記ジルコニア複合粉末に対する質量比が0質量%超過2.5質量%以下であるTiO2ナノ粉末と、
を含むように形成された焼結体であり、
焼結密度が99%以上であり、
前記焼結体の粒子の平均粒径が、2μm以上であり、
前記焼結体の硬度が、4〜10GPaであり、
前記焼結体の破壊靱性が、9〜14MPa・m1/2であり、
前記焼結体の強度が、400〜1000MPaである、加工性ジルコニア。 - 前記焼結体は、前記ジルコニア複合粉末に対する質量比が0.5〜3質量%であるCeO2を更に含有する、請求項1に記載の加工性ジルコニア。
- 前記焼結体は、前記ジルコニア複合粉末に対する質量比が0.2〜0.8質量%であるSiO2を更に含有する、請求項1又は2に記載の加工性ジルコニア。
- 前記焼結体は、前記ジルコニア複合粉末に対する質量比が0.005〜5質量%であるF2O3、Er2O3、Tb4O7、Pr2O3、又は、これらの混合物を更に含有する、請求項1〜3の何れか1項に記載の加工性ジルコニア。
- 79.8〜92mol%のZrO2及び4.5〜10.2mol%のY2O3と、3.5〜7.5mol%のNb2O5又は5.5〜10.0mol%のTa2O5と、を含む正方晶ジルコニア複合粉末と、前記ジルコニア複合粉末に対する質量比が0質量%超過2.5質量%以上であるTiO2ナノ粉末と、を含む原料物質を準備する段階と、
前記原料物質を含むスラリーを噴霧乾燥して、複合顆粒を形成する段階と、
前記複合顆粒を成形した後、焼結を施す焼結段階と、
を含み、
前記焼結は、1500〜1700℃の温度で2〜40時間実施される、加工性ジルコニアの製造方法。 - 前記焼結段階は、
1400〜1600℃の温度まで温度を上昇させる第1の段階と、
前記温度を所定時間維持する維持段階と、
1500〜1700℃の温度まで温度を上昇させる第2の段階と、
を含む、請求項5に記載の加工性ジルコニアの製造方法。 - 前記維持段階では、1300〜1500℃の温度が20〜30時間維持される、請求項6に記載の加工性ジルコニアの製造方法。
- 前記焼結後、1300〜1700℃の温度、10000〜50000psiの圧力で熱間等方加圧処理を施す、請求項6又は7に記載の加工性ジルコニアの製造方法。
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US9545363B2 (en) | 2017-01-17 |
KR101639708B1 (ko) | 2016-07-14 |
EP2889279A1 (en) | 2015-07-01 |
JP5973546B2 (ja) | 2016-08-23 |
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EP2889279B1 (en) | 2022-08-24 |
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