JP5685846B2 - 透明ジルコニア焼結体及びその製造方法、並びにその用途 - Google Patents
透明ジルコニア焼結体及びその製造方法、並びにその用途 Download PDFInfo
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Description
平均結晶粒径は焼結体の研磨エッチング面の走査電子顕微鏡観察から測定される値であり、具体的には、J.Am.Ceram.Soc.、52[8]443−6(1969)に記載されている方法に従い、(1)式により求めた。
D:平均結晶粒径(μm)
L:任意の直線を横切る粒子の平均長さ(μm)
なお、Lの値は100本以上の実測長さの平均値とした。
直線透過率及び全光線透過率はダブルビーム方式の分光光度計(日本分光株式会社製、V−650型)で測定された。測定試料としては焼結体厚みを1mmに加工し、表面粗さRa=0.02μm以下に両面鏡面研磨したものが用いられた。測定波長領域200nmから800nmの領域で測定し、可視光線領域の600nmの測定波長での透過率を直線透過率及び全光線透過率とした。
Tt:全光線透過率(%)
Td:拡散透過率(%)
Ti:直線透過率(%)
なお、本発明のジルコニア焼結体の透過率はランベルト・ベールの法則に従うため、試料が厚くなると透過率は低下する。
曲げ試験はJISR1601「ファインセラミックスの曲げ強さ試験方法」に基づき3点曲げ試験により実施され、10本の測定値の平均値を平均曲げ強度として採用した。
東ソー株式会社製のジルコニア粉末TZ−8Y(酸化イットリウム8mol%、比表面積13.5m2/g)を用い、一軸プレス(500kgf/cm2)、CIP(2ton/cm2)により加圧成形し、成形体を得た。
一次焼結体の焼結条件を、昇温速度10℃/時で1100℃から1250℃まで加熱し、保持を1250℃で4時間とした以外は実施例1と同様にして一次焼結体(試料番号:No.2)を得た。1200℃以上での保持時間は9時間であった。結果を表1に示した。
一次焼結体の焼結条件として、昇温速度400℃/時で室温から1260℃まで加熱し、1260℃で20時間保持した以外は実施例1と同様な方法で一次焼結体(試料番号:No.3)を得た。1200℃以上での保持時間は20.2時間であった。
昇温速度1000℃/時で室温から1400℃まで加熱し、保持せずに加熱を中止し放冷した以外は実施例1と同様の方法で一次焼結体(試料番号:No.4)を得た。
昇温速度1000℃/時で室温から1430℃まで加熱し、保持せずに加熱を中止し放冷した以外は実施例1と同様の方法で一次焼結体(試料番号:No.6)を得た。
昇温速度100℃/時で1100℃から1400℃まで加熱し、1400℃で2時間保持した以外は実施例1と同様に処理して一次焼結体(試料番号:No.5)を得た。
比較例1と同様の一次焼結体を特許文献1に準じてHIP処理した(処理温度1750℃、圧力150MPa、保持時間1時間)。HIP処理後の焼結体は大気中1100℃で2時間アニールしてジルコニア焼結体を得た。
Claims (9)
- イットリアを7mol%以上30mol%以下含有し、平均結晶粒径が8μm以下、試料厚さ1mmにおける測定波長600nmの可視光に対する直線透過率が50%以上であり、結晶相が立方晶蛍石型構造であり、フッ素元素を含有しないことを特徴とするジルコニア焼結体。
- 平均結晶粒径が5μm以下であることを特徴とする請求項1に記載のジルコニア焼結体。
- 試料厚さ1mmにおける測定波長600nmの可視光に対する直線透過率が55%以上であることを特徴とする請求項1又は2に記載のジルコニア焼結体。
- 試料厚さ1mmにおける測定波長600nmの可視光に対する直線透過率が60%以上であることを特徴とする請求項1乃至3のいずれかに記載のジルコニア焼結体。
- 平均曲げ強度が300MPa以上であることを特徴とする請求項1乃至4のいずれかに記載のジルコニア焼結体。
- 平均曲げ強度が350MPa以上であることを特徴とする請求項1乃至5のいずれかに記載のジルコニア焼結体。
- ジルコニア粉末を成型し、これを焼結した一次焼結体を熱間静水圧プレス処理する方法において、一次焼結体が1200℃以上1300℃以下で5時間以上保持されたものであり、熱間静水圧プレス処理に供する一次焼結体の平均結晶粒径が1μm以下、相対密度が92%以上、結晶相が立方晶のみからなることを特徴とするジルコニア焼結体の製造方法。
- ジルコニア粉末を成型し、これを焼結した一次焼結体を熱間静水圧プレス処理する方法において、一次焼結体が昇温速度500℃/時以上、焼結温度1350℃以上1500℃以下とし、焼結温度での保持をせずに焼結されたものでり、熱間静水圧プレス処理に供する一次焼結体の平均結晶粒径が1μm以下、相対密度が92%以上、結晶相が立方晶のみからなることを特徴とするジルコニア焼結体の製造方法。
- 熱間静水圧プレス処理を1250℃以上1600℃未満、50MPa以上で行うことを特徴とする請求項7又は8に記載のジルコニア焼結体の製造方法。
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EP2380851B1 (en) * | 2008-12-16 | 2013-09-04 | Nissan Chemical Industries, Ltd. | Method for producing yttrium oxide-stabilized zirconium oxide sol |
WO2011111624A1 (ja) | 2010-03-09 | 2011-09-15 | 東ソー株式会社 | 赤色透光性ジルコニア焼結体、その製造方法、その焼結体からなる部材、及びその部材を用いる宝飾品及び外装部品 |
CN103270000B (zh) | 2010-12-20 | 2016-02-03 | 东曹株式会社 | 氮化镓烧结体或氮化镓成形物以及它们的制造方法 |
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US11660172B2 (en) | 2016-11-07 | 2023-05-30 | Shofu Inc. | Dental zirconia blank having high relative density |
JP6962657B2 (ja) * | 2016-11-07 | 2021-11-05 | 株式会社松風 | 高い相対密度を有する多層の歯科用ジルコニアブランク |
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