JP6393328B2 - 酸化物セラミックの焼結動力学の制御 - Google Patents
酸化物セラミックの焼結動力学の制御 Download PDFInfo
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- JP6393328B2 JP6393328B2 JP2016528477A JP2016528477A JP6393328B2 JP 6393328 B2 JP6393328 B2 JP 6393328B2 JP 2016528477 A JP2016528477 A JP 2016528477A JP 2016528477 A JP2016528477 A JP 2016528477A JP 6393328 B2 JP6393328 B2 JP 6393328B2
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- oxide ceramic
- ceramic material
- sintering
- oxide
- process according
- Prior art date
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- 238000005245 sintering Methods 0.000 title claims description 110
- 229910052574 oxide ceramic Inorganic materials 0.000 title claims description 106
- 239000011224 oxide ceramic Substances 0.000 title claims description 50
- 238000000034 method Methods 0.000 claims description 46
- 239000000919 ceramic Substances 0.000 claims description 42
- 230000008569 process Effects 0.000 claims description 37
- 239000002019 doping agent Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 15
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000003086 colorant Substances 0.000 claims description 11
- 239000003112 inhibitor Substances 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 238000000280 densification Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 239000011164 primary particle Substances 0.000 claims description 6
- 239000011163 secondary particle Substances 0.000 claims description 6
- 238000003754 machining Methods 0.000 claims description 3
- 238000007493 shaping process Methods 0.000 claims 1
- 239000000843 powder Substances 0.000 description 71
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 48
- 238000010438 heat treatment Methods 0.000 description 25
- 238000005259 measurement Methods 0.000 description 14
- 229910010293 ceramic material Inorganic materials 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 238000004040 coloring Methods 0.000 description 10
- 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 description 9
- 238000012423 maintenance Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
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- 238000013459 approach Methods 0.000 description 5
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- 150000003839 salts Chemical class 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
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- 238000005520 cutting process Methods 0.000 description 3
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- 239000007788 liquid Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 229910000314 transition metal oxide Inorganic materials 0.000 description 3
- 238000004438 BET method Methods 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000009770 conventional sintering Methods 0.000 description 2
- 239000011351 dental ceramic Substances 0.000 description 2
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- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 101100465385 Arabidopsis thaliana PAF2 gene Proteins 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
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- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
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- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
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- 210000004513 dentition Anatomy 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
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- IBIKHMZPHNKTHM-RDTXWAMCSA-N merck compound 25 Chemical compound C1C[C@@H](C(O)=O)[C@H](O)CN1C(C1=C(F)C=CC=C11)=NN1C(=O)C1=C(Cl)C=CC=C1C1CC1 IBIKHMZPHNKTHM-RDTXWAMCSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 150000003114 praseodymium compounds Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
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- 230000036346 tooth eruption Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000003826 uniaxial pressing Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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- 239000003232 water-soluble binding agent Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
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- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/008—Producing shaped prefabricated articles from the material made from two or more materials having different characteristics or properties
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Description
HV2.5が、ISO14705:2008に従って2.5kgf(24.517N)の荷重で測定されるビッカース硬さであり;
HVmaxが、HV2.5の測定値の最大値であり;
HVminが、HV2.5の測定値の最小値であり;
予備焼結済み多層酸化物セラミックブランクによって解決される。
本発明によるブランクは、最終的な焼結ステップ中に歪みを示さないか、または本質的に歪みを示さないことが意外にも判明した。特に、これらは、異なる層間の焼結動態または収縮挙動の著しい差異を欠点として持たない。さらに、標準的なISO14705:2008に従ったビッカース硬さの測定値は、予備焼結済み多層ブランク内の異なる位置の焼結挙動を特定および予測するのに適していることが予想外にも判明した。
Y2O3 2.0〜10.0wt.%、特に4.5〜6.0wt.%;
HfO2 最大で5.0wt.%;
Al2O3 最大で0.5wt.%;
SiO2 最大で0.1wt.%;および
Na2O 最大で0.1wt.%。
HV2.5が、ISO14705:2008に従って2.5kgf(24.517N)の荷重で測定されるビッカース硬さであり;
HVmaxが、HV2.5の測定値の最大値であり;
HVminが、HV2.5の測定値の最小値であり;
多層酸化物セラミック未焼結体も提供する。
(a)少なくとも第1の酸化物セラミック材料および第2の酸化物セラミック材料を準備するステップであり、第1の酸化物セラミック材料および第2の酸化物セラミック材料が、焼結挙動の観点において異なる、ステップと、
(b)第1の酸化物セラミック材料の焼結挙動を第2の酸化物セラミック材料の焼結挙動に対して調整するように酸化物セラミック材料の少なくとも1種を適応させるステップと
を含む。
(c)酸化物セラミック材料の層を形成し、互いの上に層を配列するステップ、または第1の酸化物セラミック材料から第2の酸化物セラミック材料への連続的な勾配を含む酸化物セラミック材料の層を形成するステップと;
(d)酸化物セラミック材料を、任意選択で締め固め、特に圧縮して、未焼結体を得るステップと;
(e)酸化物セラミック材料を、任意選択で予備焼結して、予備焼結済みセラミックブランクを得るステップ
を含む。
酸化物粉末上にコーティングされる元素の適当な量の水溶性塩および0.1〜2wt.%(コーティングされる粉末の量と比べて)のポリビニルアルコール(例えば、Zschimmer&Schwarz社製Optapix PAF2またはPAF35)などの水溶性結合剤を含有する水溶液を、約0.5時間撹拌することによって(例えば、磁気撹拌機を使用して)ホモジナイズした。得られた溶液を、流動床造粒機によって酸化物粉末上に完全に塗布した。このステップ中、粉末を、圧縮空気(0.15〜0.30バール、30〜80℃)によって流動床として懸濁液中に維持し、この流動床の上に配列されたノズルを通して2〜6バールの吹き付け圧力で吹き付けることによって、着色液を粉末に塗布した。加熱された圧縮空気は、プロセス中にコーティングされた粉末を同時に乾燥させた。
着色または無着色粉末にドーパント(すなわち、非着色焼結助剤または焼結阻害剤)を添加することによる収縮性の制御:
2)3wt.%のY2O3および0.25wt.%のAl2O3を含む
ドープされた酸化物セラミック粉末を使用する予備焼結済み多層酸化物セラミックブロック
最大で300℃まで0.25K/分、維持時間60分
最大で500℃まで0.25K/分
最大で1120℃まで1K/分、維持時間120分。
歪みの係数の決定
実施例2Aおよび2Bで得られたタイプAおよびBの予備焼結済みブロックの複数の測定点で、ビッカース硬さHV2.5(0.5〜1.0GPa)を測定した。測定点の位置を図3に概略的に示す。図中、zは、異なる層が配列されている次元である。結果を以下の表に示す。
ドープされた酸化物セラミック粉末を使用する完全に焼結された多層酸化物セラミックブロック
(比較)
二重層ブロック(29mm×4.6mm×5.8mm)を、一方が以下の表に示した一般的な手順を使用して着色元素でコーティングされた、2種の異なる原料ジルコニア粉末に由来する酸化物粉末から調製した。
2)0.05wt.%のAl2O3を含む、比表面積 約13m2/g
3)0.25wt.%のAl2O3を含む;比表面積 約7m2/g
最大で300℃まで0.25K/分、維持時間120分
最大で500℃まで0.25K/分
最大で700℃まで0.5K/分、維持時間120分
最大で1050℃まで1K/分、維持時間120分
二つの層を含み、白色の、濃淡を付けられた4ユニットモノリシックブリッジをシミュレートする四つの細長い矩形ブロック(46mm×7.5mm×5.8mm)を、以下の表のように配合されたY−TZPジルコニア粉末から製作した。粉末の二つの層を、層間の適度に平らな界面を保証するための振動台上の単純な鋼チャネル金型中に順次注ぎ、約18MPaの圧力を使用して一軸性に締め固めた。得られた一軸性に予備加圧成形された未焼結コンパクトを、ラテックスバッグ中に真空密封し、約345MPaでさらに冷間等方圧加圧成形し、1500℃で2時間最終的に焼結した。歪み/湾曲の非存在または存在についての目視観察を以下の表に要約する。
2)0wt.%のFe2O3を含む;比表面積 約7m2/g
3)0.14wt.%のFe2O3を含む;比表面積 約13m2/g
4)0.19wt.%のFe2O3を含む;比表面積 約7m2/g
異なる予備緻密化がなされた粉末の焼結挙動
ジルコニアセラミック粉末のサンプル(KCM KZ−3YF(SD)AC)を、100、150、200、および250MPaの圧力で冷間一軸加圧成形し、500℃で脱結合させた。得られた緻密化された粉末を、950〜1150℃の温度範囲にわたって、最大で900℃まで5K/分および最大で1150℃まで1K/分の加熱速度で熱処理に付した。温度の関数としての相対的な収縮のプロットを図7に示す。この図から分かるように、酸化物セラミック粉末の焼結挙動を、前記粉末を異なる程度の部分的な緻密化に付すことによって適応させることができる。異なる層中で使用される粉末を異なる程度の部分的な緻密化に付すことによって、所与の焼結温度でのこれらの線収縮を等しくすることができ、その結果、これらの粉末から作製される多層ブロックは、予備焼結状態または高密度焼結状態で歪みを示さない。
Claims (14)
- 歪みを伴うことなく焼結され得る、化学組成の観点において異なる少なくとも二つの異なる層を有する多層酸化物セラミック体を製造するためのプロセスであって、
(a)少なくとも第1の酸化物セラミック材料および第2の酸化物セラミック材料を準備するステップであって、前記第1の酸化物セラミック材料および前記第2の酸化物セラミック材料が、焼結挙動の観点において異なる、ステップと;
(b)前記第1の酸化物セラミック材料の焼結挙動を前記第2の酸化物セラミック材料の焼結挙動に対して調整するように前記酸化物セラミック材料の少なくとも1種を適応させるステップと
を含み、
ここで、前記酸化物セラミック材料の少なくとも1種を適応させるステップが、
(i)前記酸化物セラミック材料をドーパントでコーティングすることによって、前記酸化物セラミック材料中にドーパントを組み込むこと、および/または
(ii)前記酸化物セラミック材料を異なる程度の部分的な緻密化に付すこと
を含む、プロセス。 - 前記体が、マルチユニット歯科修復物の製造に適している、請求項1に記載のプロセス。
- 前記少なくとも二つの異なる層が、異なる色を有する、請求項1または2に記載のプロセス。
- 前記焼結挙動が、850〜1350℃の範囲内の温度での焼結の際の相対的な線収縮である、請求項1から3のいずれか一項に記載のプロセス。
- ステップ(a)において、前記第1の酸化物セラミック材料の焼結挙動および前記第2の酸化物セラミック材料の焼結挙動が、少なくとも0.15%異なる、請求項1から4のいずれか一項に記載のプロセス。
- ステップ(b)において、前記適応させるステップが、0.15%未満異なる、前記第1の酸化物セラミック材料の焼結挙動および前記第2の酸化物セラミック材料の焼結挙動をもたらす、請求項1から5のいずれか一項に記載のプロセス。
- (c)前記酸化物セラミック材料の層を形成し、互いの上に前記層を配列するステップ、または前記第1の酸化物セラミック材料から前記第2の酸化物セラミック材料への連続的な勾配を含む前記酸化物セラミック材料の層を形成するステップと;
(d)前記酸化物セラミック材料を、任意選択で締め固め、未焼結体を得るステップと;
(e)前記酸化物セラミック材料を、任意選択で予備焼結して、予備焼結済みセラミックブランクを得るステップと
をさらに含む、請求項1から6のいずれか一項に記載のプロセス。 - 前記ドーパントが、焼結助剤および焼結阻害剤から選択される、請求項1から7のいずれか一項に記載のプロセス。
- 前記ドーパントが、Al2O3およびY2O3から選択される、請求項1から8のいずれか一項に記載のプロセス。
- 前記酸化物セラミック材料の少なくとも1種を適応させるステップが、前記酸化物セラミック材料の少なくとも一部の一次および/もしくは二次粒子サイズならびに/または比表面積を変更することをさらに含む、請求項1から9のいずれか一項に記載のプロセス。
- 請求項1から10のいずれか一項に記載のプロセスによって多層酸化物セラミック体を調製するステップおよび成形セラミック製品を得るために、前記体を、所望の幾何形状に成形するステップを含む、歯科修復物を製造するためのプロセス。
- 前記成形ステップが、機械加工によって実施される、請求項11に記載のプロセス。
- 前記成形セラミック製品が、歯科用フレームワーク、アバットメント、またはモノリシック全輪郭歯科修復物の形状を有する、請求項11または12に記載のプロセス。
- 前記成形セラミック製品を高密度に焼結するステップをさらに含む、請求項11から13のいずれか一項に記載のプロセス。
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EP13177474.7A EP2829251B1 (en) | 2013-07-22 | 2013-07-22 | Controlling of sintering kinetics of oxide ceramics |
EP13177474.7 | 2013-07-22 | ||
PCT/EP2014/065595 WO2015011079A1 (en) | 2013-07-22 | 2014-07-21 | Controlling of sintering kinetics of oxide ceramics |
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EP (1) | EP2829251B1 (ja) |
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CA3084630C (en) | 2022-11-22 |
US20190099245A1 (en) | 2019-04-04 |
CA2952770C (en) | 2020-07-21 |
CA2952770A1 (en) | 2015-01-29 |
US11413122B2 (en) | 2022-08-16 |
CA2917378C (en) | 2017-07-11 |
US20160157971A1 (en) | 2016-06-09 |
JP2016527017A (ja) | 2016-09-08 |
KR20160033141A (ko) | 2016-03-25 |
CA2917378A1 (en) | 2015-01-29 |
EP2829251A1 (en) | 2015-01-28 |
WO2015011079A1 (en) | 2015-01-29 |
CN105392444A (zh) | 2016-03-09 |
KR101851881B1 (ko) | 2018-04-26 |
CA3084630A1 (en) | 2015-01-29 |
EP2829251B1 (en) | 2019-04-10 |
CN107573035B (zh) | 2020-12-01 |
CN105392444B (zh) | 2017-10-31 |
CN107573035A (zh) | 2018-01-12 |
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