JP2009525359A - 焼結された立方晶ハロゲン化物のシンチレーター物質、およびこれを作製する方法 - Google Patents
焼結された立方晶ハロゲン化物のシンチレーター物質、およびこれを作製する方法 Download PDFInfo
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- G01T1/16—Measuring radiation intensity
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Abstract
【選択図】
図1
Description
本出願は、2006年1月30日に出願された米国仮特許出願第60/763249号に基づく優先権を主張し、この出願を援用することにより総ての内容が本明細書の一部として取り入れられる。
周囲で散乱され、そして吸収されて、ガンマ線を発生させるので、これにより井戸試掘孔の周囲の物理的な特性が得られることになる。
御パラメーターが必要である。他のハロゲン化アルカリ結晶のなかには一般に、ヨウ化ナトリウム結晶を作製するための方法を開示する幾つかの出版物がある。例えば、米国特許第5,178,719号公報は、結晶の長さに交差した方向で、残余の不純物およびドーパントの濃度を制御する方法を開示する。しかし、シンチレーター結晶を作製するための品質管理解決法の多くは、企業秘密として保持されている。
用される。シンチレーター本体は、シンチレーター物質の圧粉によって製造される、密度が高く、機械的に安定な部品である。
径を有する。第三の実施態様において、NaI粉末は、75μm(米国ふるい200)から200μm(米国ふるい70)の平均一次粒径を有する。第四の実施態様において、異なる平均粒径をもつ粒子の最適な混合物は、充填密度を最大化し、そして熱処理される圧粉体の細孔容積、孔径および分布を最小化するために使用される。
記載するように、あらかじめ選択された一連の焼結順序で鋳型の中に異なる位置で充填してよい。そのような方法でシンチレーター本体を製作することは、単結晶製作によっては容易に果たしえない本発明の特色である。
る。一軸圧縮は、冷温一軸圧縮(cold uniaxial pressing;CUP)、中温一軸圧縮(warm uniaxial pressing;WUP)、もしくは高温圧縮(hot pressing)でよい。WUPでは、CUP鋳型は、圧力の印加前に、そして印加中に加熱する。
わたって加わり、複雑な形が製作されることになり、そして部品内の圧力勾配が減少する。この段階では、粉末の圧粉体もしくは粉末は、カプセル化するか、もしくは密閉容器に入れ、そして理論密度の>93%に密度を増加するために、約50,000と100,000psiの間で等方的に印加してよい。このプロセスは、冷温等方圧縮(cold isostatic pressing)、中温等方圧縮(warm isostatic
pressing)、もしくは高温等方圧縮(hot isostatic pressing)(CIP、WIPもしくはHIP)のいずれかでよい。
シンチレーター本体は、理論密度の少なくとも99.9%の密度を有する、本来の形状に近い形状の素材片(a near net shape blank)である。発明の一つの実施態様において、焼結されたNaIシンチレーター本体は、本来の形状に近い形状の素材片(4x4x16)である。一つの実施態様において、シンチレーター本体は、3.67g/cm3の密度、415nmにおける最大の放出、0.23msの崩壊定数、1.85の屈折率、そして100の変換効率を有する。
これらの実施例では、シグマアルドリッチ社(Sigma Aldrich)から得た純度99.999%のヨウ化ナトリウム粉末の20gの試料は、粉末を乾燥することによ
り前処理し、水分と揮発性不純物を除去し、以下に述べる手順のあいだ乾燥雰囲気下に保った。試料の粒径分布は、下の表1に記載した。試料はタリウムを含まなかった。試料を金型に入れ、真空ホットプレスで高温圧縮し、そして次の実験計画にしたがった圧力下で焼結した。最初は周囲温度の試料を6.6℃/分の加熱上昇速度で、300℃の加工第一温度まで加熱し、表1に示したような第一滞留時間のあいだ、第一温度で保持した。次に、試料を焼鈍のために、240℃の第二温度まで4℃/分の冷却下降速度で冷却させ、そして15分の第二滞留時間のあいだ第二温度に保った。最後に、試料を6.6℃/分の冷却下降速度で冷却し、周囲温度に戻した。初期昇温の最後の15分間に表1に示したように焼結圧力に至るまで圧力をかけ、そして第一温度および滞留時間の条件のあいだ維持し、その後圧力を常圧に下げた。生成したシンチレーター本体を光学的な透明性と色とを目視で評価し、結果を下の表1にまとめた。実施例1〜5の生成したシンチレーター本体の写真は、表1に示したように、図2から6にそれぞれ表わした。
この実施例では、0.2%のヨウ化タリウムを含み、約10マイクロメートルから約592マイクロメートルの粒径を有するヨウ化ナトリウム20gを周囲温度、110,000psiで、5分間、冷温圧縮した。生成したシンチレーター本体は図7に示すが、これは半透明、黄色であった。
要であることを示す。
Claims (24)
- 下記を含有する焼結された立方晶ハロゲン化物のシンチレーターを作製する方法:
662keVで約7%から約20%までのパルス波高分解能を有する多結晶性の焼結された立方晶ハロゲン化物のシンチレーターを生成するのに効果的な、圧力、温度、滞留時間および粒径の加工条件下で、立方晶ハロゲン化物および少なくとも一つの活性化剤の粉末混合物を圧縮する;その際、前記加工温度が、およそ周囲温度からセ氏度で立方晶ハロゲン化物の融点の約90%に至るまで、圧力が、約30,000psiから約200,000psiまで、圧縮滞留時間が、約5分から約120分まで、そして平均立方晶ハロゲン化物粒径が、約60マイクロメートルから約2000マイクロメートルまでの範囲である。 - 前記立方晶ハロゲン化物が、ナトリウム、カリウム、セシウム、ルビジウムのハロゲン化物から選択される二成分系の立方晶ハロゲン化物である、請求項1に記載の方法。
- 前記立方晶ハロゲン化物が、ヨウ化ナトリウムである、請求項1に記載の方法。
- 前記活性化剤が、タリウム、セシウム、およびナトリウムのハロゲン化物から選択される、請求項1に記載の方法。
- 前記活性化剤が、ヨウ化タリウムである、請求項1に記載の方法。
- 前記活性化剤の濃度が、重量で約0.005%から5.0%までの範囲である、請求項1に記載の方法。
- 前記加工温度が約20℃から約30℃までの範囲であり、前記圧力が約100,000psiから約200,000psiまでの範囲であり、前記滞留時間が約5分から約10分までの範囲であり、そして前記平均粒径が約60マイクロメートルから約90マイクロメートルまでの範囲である、請求項1に記載の方法。
- 前記温度が約90℃から約150℃までの範囲であり、前記圧力が約100,000psiから約150,000psiまでの範囲であり、前記滞留時間が約5分から約10分までの範囲であり、そして前記平均粒径が約90マイクロメートルから約120マイクロメートルまでの範囲である、請求項1に記載の方法。
- 前記温度が約250℃から約450℃までの範囲であり、前記圧力が約30,000psiから約60,000psiまでの範囲であり、前記滞留時間が約50分から約60分までの範囲であり、そして前記平均粒径が約200マイクロメートルから約275マイクロメートルまでの範囲である、請求項1に記載の方法。
- 前記圧縮が、冷温一軸圧縮、中温一軸圧縮、もしくは高温一軸圧縮によって行われる、請求項1に記載の方法。
- 前記一軸圧縮が、高温圧縮である、請求項10に記載の方法。
- 前記圧縮が、冷温等方圧縮、中温等方圧縮、もしくは高温等方圧縮によって行われる、請求項1に記載の方法。
- 前記活性化剤が、混合物の全体にわたって実質的に均一に分布する、請求項1に記載の方法。
- 前記活性化剤が、制御された勾配にしたがって混合物の全体にわたって変化する濃度百分率を有する、請求項1に記載の方法。
- 前記混合物が、第一および第二の異なった活性化剤濃度、および/もしくは、第一および第二の異なった粒径範囲分布を有する、少なくとも第一および第二のブレンドを含有し、この第一および第二のブレンドが、シンチレーターの寸法に沿って、活性化剤濃度および/もしくは結晶サイズの制御された勾配を有するシンチレーター本体を生成するために、あとに続く焼結用にあらかじめ選択された順序で圧縮鋳型に充填される、請求項1に記載の方法。
- 前記混合物が、比較的大きい第一の立方晶ハロゲン化物平均粒径を有する立方晶ハロゲン化物と活性化剤との第一ブレンド(25%から約75%まで)、および、第一の立方晶ハロゲン化物平均粒径の約30%に至るまでの比較的小さい第二の立方晶ハロゲン化物平均粒径を有する立方晶ハロゲン化物と活性化剤との第二ブレンド(約25%から約75%まで)を含むことができる、請求項1に記載の方法。
- 前記比較的大きい第一の立方晶ハロゲン化物平均粒径が、約200マイクロメートルから約250マイクロメートルまでの範囲であり、そして前記第二の比較的小さい平均立方晶ハロゲン化物粒径が、約30マイクロメートルから約50マイクロメートルまでの範囲である、請求項16に記載の方法。
- 水分および/もしくは他の揮発性不純物を除去するために、圧縮に先立って、前記混合物を前処理することをさらに含む、請求項1に記載の方法。
- 前記前処理が、不活性雰囲気下もしくは真空下で前記混合物をあらかじめ加熱することによって行われる、請求項18に記載の方法。
- シンチレーターにおける機械的な内部応力を減少させるのに充分な温度で、前記多結晶性の焼結された立方晶ハロゲン化物のシンチレーターを焼鈍することをさらに含む、請求項1に記載の方法。
- 請求項1に記載の方法にしたがって製造されたシンチレーター。
- 7%から約20%までのパルス波高分解能を有する、請求項21に記載のシンチレーター。
- 請求項1の方法にしたがって製造され、そして光学的に光検出器に接続したシンチレーターを含有する放射線検出器。
- 前記シンチレーターがヨウ化ナトリウムを含有し、そして前記活性化剤がヨウ化タリウムを含有する、請求項23に記載の放射線検出器。
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JP2014514368A (ja) * | 2011-02-24 | 2014-06-19 | 日東電工株式会社 | 蛍光体成分を有する発光複合材 |
JP2012207162A (ja) * | 2011-03-30 | 2012-10-25 | Canon Inc | 相分離構造を有するシンチレータ結晶体 |
JP5603461B1 (ja) * | 2013-07-02 | 2014-10-08 | 公立大学法人大阪府立大学 | アルカリハライド系シンチレータ粉末の製造方法及びシンチレータ材料の製造方法 |
JP6480648B1 (ja) * | 2018-04-09 | 2019-03-13 | 公立大学法人大阪府立大学 | 電磁放射線検出装置 |
US11194060B2 (en) | 2018-04-09 | 2021-12-07 | University Public Corporation Osaka | Electromagnetic radiation detector and method |
Also Published As
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WO2007089746A1 (en) | 2007-08-09 |
KR20080096529A (ko) | 2008-10-30 |
US20070237668A1 (en) | 2007-10-11 |
CN101410346A (zh) | 2009-04-15 |
CN101410346B (zh) | 2013-02-13 |
US7879284B2 (en) | 2011-02-01 |
EP1981828A1 (en) | 2008-10-22 |
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