JP5708050B2 - 赤色透光性ジルコニア焼結体及びその製造方法 - Google Patents
赤色透光性ジルコニア焼結体及びその製造方法 Download PDFInfo
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Description
色調は、JISZ8722に準拠し、D65光源、10°視野角の条件において色差計(カラーアナライザーTC−1800MK−II、東京電色社製)を用いて測定を行った。
透過率はJISK7105「プラスティックスの光学特性試験方法」およびJISK7361−1「プラスティック・透明材料の全光線透過率の試験方法」に基づいて測定した。測定試料は焼結体厚みを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を用いた。測定に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)を用い、光源(重水素ランプおよびハロゲンランプ)より発生した光を試料に透過および散乱させ積分球を用いて全光線透過量、拡散透過量を測定した。直線透過率は(2)式から導いた。測定波長領域は200nm〜800nmの領域とした。
Tt:全光線透過率(%)
Td:拡散透過率(%)
Ti:直線透過率(%)
焼結体の蛍光スペクトルを測定し、焼結体中の3価セリウムの有無を確認した。測定は日本分光(株)製FP−6500装置を用い、励起光源としてキセノンランプ(248nm)を用い、反射法によって波長300nm〜700nmの発光を測定した。測定試料は直線透過率の測定に用いたものを用いた。570〜600nm付近のピークの存在によって3価セリウムを確認した。
(原料粉末の調製)
ジルコニア粉末及び酸化セリウム粉末を所定量秤量し、エタノール溶媒中直径10mmのジルコニア製ボールで72時間ボールミル混合した後、乾燥しセリウム量の異なる原料粉末を調製した。
各原料粉末を金型プレスによって圧力50MPaで成形した後、冷間静水圧プレス装置を用い圧力200MPaで処理し、直径20mm、厚さ3mmの円柱状の成形体を得た。
試料番号1〜3の一次焼結体を用い、温度1650℃、圧力150MPa、保持時間1時間でHIP処理した。圧力媒体には純度99.9%のアルゴンガスを用いた。HIP装置はカーボンヒーター及びカーボン断熱材を備えた装置であった。また、試料を設置する容器として通気孔のあるアルミナ製蓋付きルツボを用いた。
試料番号1〜3の一次焼結体を用い、HIP処理温度を1500℃にした以外は実施例1〜3と同様にしてジルコニア焼結体を得た。得られたジルコニア焼結体の特性を表3に示した。
(粉末調製)
ジルコニア粉末、酸化セリウム粉末の他、酸化ネオジウム、酸化コバルトを、それぞれ所定量を秤量し、エタノール溶媒中直径10mmのジルコニア製ボールで72時間ボールミル混合し、乾燥した粉末を原料粉末とした。
(一次焼結)
原料粉末を金型プレスによって圧力50MPaで成形した後、冷間静水圧プレス装置を用い圧力200MPaで処理し、直径20mm、厚さ3mmの円柱成形体を得た。
試料番号7又は8の一次焼結体を用い、温度1650℃、圧力150MPa、保持時間1時間で、実施例1〜3と同様の方法でHIP処理した後、焼結体を大気中、昇温速度250℃/hで1000℃に1時間保持してアニールした。
実施例3及び6のジルコニア焼結体の蛍光スペクトルを測定した。いずれのジルコニア焼結体も3価セリウムに帰属される590nmにピークを有する発光が観察され、セリウム3価の存在が確認された。実施例3の蛍光スペクトルを図3に示した。
実施例3及び6と同様にして得られたジルコニア焼結体について、大気中、昇温速度250℃/h、温度1200℃で1時間保持するアニール処理した。いずれのジルコニア焼結体も、ごく薄い黄色味を帯びた透明体であった。
Claims (10)
- 6mol%〜30mol%のイットリア及びCeO2換算で0.1mol%〜5mol%のセリウム酸化物を含有し、該セリウム酸化物が3価セリウムの酸化物を含有し、なおかつ、結晶相が立方晶蛍石型構造であることを特徴とするジルコニア焼結体。
- 試料厚さ1mmにおいて、波長400nm〜500nmの可視光に対する直線透過率の最大値が3%以下であり、かつ、波長600nm〜800nmの可視光に対する直線透過率の最大値が40%以上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。
- 明度L*、色相a*およびb*が、20≦L*≦50、40≦a*≦60および30≦b*≦70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。
- 6mol%〜30mol%イットリア及びCeO2換算で0.1mol%〜5mol%のセリウム酸化物を含有するジルコニア粉末を成形し、一次焼結、熱間静水圧プレス処理およびアニールし、焼結体中に3価セリウムを生成させることを特徴するジルコニア焼結体の製造方法。
- 一次焼結体を通気性のある容器に配してHIP処理を行うことを特徴とする請求項4に記載の製造方法。
- アニールを800℃以上1000℃以下で行うことを特徴とする請求項4又は5に記載のジルコニア焼結体の製造方法。
- HIP処理に供する一次焼結体の平均粒径が5μm以下であることを特徴とする請求項4乃至6のいずれかに記載の製造方法。
- 請求項1乃至3のいずれかに記載のジルコニア焼結体からなる部材。
- 請求項8に記載の部材を用いることを特徴とする宝飾品。
- 請求項8に記載の部材を用いることを特徴とする外装部品。
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