CN104775162B - 光激发光剂量检测晶体制备方法 - Google Patents
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- 238000001514 detection method Methods 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims description 15
- 230000001443 photoexcitation Effects 0.000 title 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 71
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 17
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- 238000004020 luminiscence type Methods 0.000 claims description 26
- 229910052593 corundum Inorganic materials 0.000 claims description 15
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 15
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- 238000000034 method Methods 0.000 claims description 13
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- 239000004411 aluminium Substances 0.000 claims 1
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- 238000006243 chemical reaction Methods 0.000 abstract 1
- 238000005424 photoluminescence Methods 0.000 abstract 1
- 238000000904 thermoluminescence Methods 0.000 description 9
- 229910052594 sapphire Inorganic materials 0.000 description 8
- 230000005855 radiation Effects 0.000 description 7
- 230000012010 growth Effects 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000005231 Edge Defined Film Fed Growth Methods 0.000 description 3
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- 238000004980 dosimetry Methods 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
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- 238000003763 carbonization Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
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- 239000000843 powder Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
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Abstract
一种光激发光剂量检测晶体制备方法，该方法是先将氧化铝（Al2O3）以碳包覆起来，在真空下经过扩散（Diffusion）后，使碳原子扩散进入氧化铝晶格内，再于大气下进行退火（Annealing），使氧与碳原子反应，透过C+O转换成CO，或C+O2转换成CO2，使氧化铝晶体产生氧空缺（Oxygen Vacancy），而可简易制得碳分布均匀的检测晶体（C:Al2O3）结构，具有光激发光剂量响应灵敏度高，且线性剂量响应范围宽的特性。
Description
技术领域
本发明有关于一种光激发光剂量检测晶体制备方法，尤指涉及一种光激发光剂学，特别是指以碳包覆氧化铝结构经过真空扩散与大气退火后，使氧化铝晶体产生氧空缺（Oxygen Vacancy）缺陷的检测晶体（C:Al2O3）结构的制备方法。
背景技术
材料的热激发光（Thermoluminescence, TL）与光激发光（Optically StimulatedLuminescence, OSL）特性，广泛应用于辐射剂量学（Radiation Dosimetry），作为环境与个人辐射剂量之的测定。其中热激发光是指材料在吸收辐射能之后的热释光，而光激发光是指材料在吸收辐射能之后的光释光。光激发光与热激发光相比，光激发光剂量计使用过程中不用加热，可以有效避免发光中心之热淬灭，具有灵敏度高，使用相对简单的优点。然而，光激发光剂量学因为缺少有对辐射敏感、光激发光效率高、有效原子数较小、及光衰退性能好之的发光材料，因此长期没有得到重视与发展。
蓝宝石（Al2O3）晶体具有优良的热激发旋光性能，目前Al2O3晶体的生长方法常使用的包括提拉法（Czochralski, Cz）与泡生法（Kyropoulos, KY）两种，其中KY法仅能生长纯的Al2O3晶体，但纯的Al2O3晶体对射线的热激发光灵敏度很低。为了改善Al2O3晶体的热激发旋光性能，于20世纪90年代，Landauer公司的M.S. Akselrod研究小组采用Cz法在有石墨存在的强还原气氛条件下，生长得到α-Al2O3:C晶体（M. S. Akselrod et. al. Highlysensitive thermoluminescent anion-defective 0t-Al2O3: C single crystaldetectors, Radiation Protection Dosimetry, 1990， 32: 15-20)。经过一系列的研究表明，α-Al2O3:C晶体具有灵敏度高；热激发光峰单一且温度适中；背底与剂量阈值低；线性剂量响应范围宽；热激发光与光激发旋光性能衰减速度慢；低剂量下重复使用性能好；对辐射敏感；及光激发光效率高等诸多优点。因此α-Al2O3:C晶体是极具应用潜力的热激发光与光激发光材料。然而，目前α-Al2O3:C晶体的生长与剂量计的制造主要被美国Landauer公司所垄断，该公司研制生产的α-Al2O3:C热激发光与光激发光剂量计已经在欧美广泛使用，普遍应用于环境与个人剂量监测，但其采用Cz法长晶过程复杂，而导致碳在Al2O3晶体中分布不均匀，难以获得品质均一的α-Al2O3:C晶体；同时，晶体生长工艺还需要昂贵的设备、生产周期长且成本高。国内关于α-Al2O3:C晶体生长以及α-Al2O3:C剂量计的研制则有杨新波等人于文献（杨新波等人.硅酸盐学报,2008, 36(5)：678-682.；杨新波等人.无机材料学报,2009, 24(2)：255-258.）中提出采用导模法（Edge-defined Film-fed Growth, EFG）生长蓝宝石晶体，其过程中使用石墨加热体，导致生长得到的蓝宝石晶体表面附着有碳与碳化物，晶体质量较差。故，一般无法符合使用者于实际使用时所需。
发明内容
本发明的主要目的在于，克服已知技术所遭遇的上述问题，并提供一种可简易制得碳分布均匀的光激发光剂量检测晶体（C:Al2O3）的制备方法。
本发明的次要目的在于，提供一种具有光激发光剂量响应灵敏度高，且线性剂量响应范围宽等特性的检测晶体（C:Al2O3）结构。
为达以上目的，本发明所用的技术方案是：一种光激发光剂量检测晶体制备方法，该方法至少包含下列步骤：
（A）于一氧化铝（Al2O3）外面涂覆一层碳膜，以碳将氧化铝包覆形成碳包覆氧化铝结构；其中，碳膜选自石墨碳材、碳粉、碳纸或人造石墨粉中的一种或几种。
（B）将该碳包覆氧化铝结构置于一高温炉中，在抽真空无氧环境下，以1500℃-1900℃的加热处理进行扩散程序，使碳原子扩散进入氧化铝晶格内；其中，加热处理时间为10min-2hr。
（C）在大气下的开放式高温炉中，以1400℃-1800℃的加热处理进行退火程序，使氧化铝内部晶格氧与碳原子反应而形成氧空缺缺陷，以制成检测晶体C:Al2O3结构；其中，加热处理时间为10min-2hr。
如此，可简易制得碳分布均匀的检测晶体（C:Al2O3）结构，具有光激发光剂量响应灵敏度高，且线性剂量响应范围宽的特性。
附图说明
图1是本发明的制备流程示意图。
标号说明：
步骤（A）碳包覆氧化铝11 步骤（B）加热扩散12
步骤（C）加热退火13。
具体实施方式
请参阅图1所示，为本发明的制备流程示意图。如图所示：本发明为一种光激发光剂量检测晶体制备方法，其至少包含下列步骤：
（A）碳包覆氧化铝步骤11：于一氧化铝（Al2O3）外面涂覆一层碳膜（Carbon Film），以碳将氧化铝包覆形成碳包覆氧化铝结构，其中该碳膜选自石墨碳材、碳粉（C2 powder）、碳纸（C-paper）、或人造石墨粉中的一种或几种组合；
（B）加热扩散步骤12：将该碳包覆氧化铝结构置于一高温炉中，在抽真空无氧环境下进行扩散程序（Diffusion Process），以1500℃-1900℃加热处理10min-2hr，使碳原子扩散进入氧化铝晶格内；以及
（C）加热退火步骤13：接着在大气下的开放式高温炉中进行退火程序（AnnealingProcess），以1400℃-1800℃加热处理10min-2hr，使氧化铝内部晶格氧与碳原子反应而形成氧空缺（Oxygen Vacancy）缺陷，以制成检测晶体（C:Al2O3）结构。
如是，藉由上述揭露的流程构成一全新的光激发光剂量检测晶体制备方法。
藉此，本发明所提的光激发光剂量检测晶体制备方法，是先将氧化铝以碳包覆起来，在真空下经过扩散后，使碳原子扩散进入氧化铝晶格内，再于大气下进行退火，使氧与碳原子反应，透过C+O转换成CO，或C+O2转换成CO2，使氧化铝晶体产生氧空缺（OxygenVacancy）缺陷，而可简易制得碳分布均匀的检测晶体（C:Al2O3）结构，具有光激发光剂量响应灵敏度高，且线性剂量响应范围宽的特性。
综上所述，本发明为一种光激发光剂量检测晶体制备方法，可有效改善现有技术的种种缺点，是先将氧化铝以碳包覆起来，在真空下经过扩散后，使碳原子扩散进入氧化铝晶格内，再于大气下进行退火，使氧化铝晶格内的氧与碳原子反应而形成氧空缺（OxygenVacancy）缺陷，以制成检测晶体（C:Al2O3）结构，进而使本发明的产生能更进步、更实用、更符合使用者所须，确已符合发明专利申请的要件，依法提出专利申请。
惟以上所述，仅为本发明的较佳实施例而已，当不能以此限定本发明实施的范围。故，凡依本发明申请专利范围及发明说明书内容所作的简单的等效变化与修饰，皆应仍属本发明专利涵盖的范围内。
Claims (3)
1.一种光激发光剂量检测晶体制备方法，其特征在于，该方法至少包含下列步骤：
(A)于一氧化铝外面涂覆一层碳膜，以碳将氧化铝包覆形成碳包覆氧化铝结构；其中，碳膜选自碳粉、碳纸或人造石墨粉中的一种或几种；
(B)将该碳包覆氧化铝结构置于一高温炉中，在抽真空无氧环境下，以1500℃-1900℃的加热处理进行扩散程序，使碳原子扩散进入氧化铝晶格内；
(C)在大气下的开放式高温炉中，以1400℃-1800℃的加热处理进行退火程序，使氧化铝内部晶格氧与碳原子反应而形成氧空缺缺陷，以制成检测晶体C:Al2O3结构。
2.如权利要求1所述的光激发光剂量检测晶体制备方法，其特征在于，所述步骤(B)中的加热处理时间为10min-2h。
3.如权利要求1所述的光激发光剂量检测晶体制备方法，其特征在于，所述步骤(C)中的加热处理时间为10min-2h。
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| WO2001035398A1 (en) * | 1999-11-10 | 2001-05-17 | Georgetown University | Near-field crystal optical memory |
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| US6846434B2 (en) * | 2001-12-04 | 2005-01-25 | Landauer, Inc. | Aluminum oxide material for optical data storage |
| WO2010114002A1 (ja) * | 2009-04-01 | 2010-10-07 | 国立大学法人 広島大学 | アルミニウム酸化物蛍光体及びその製造方法 |
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| TW201527739A (zh) | 2015-07-16 |
| US20150198530A1 (en) | 2015-07-16 |
| CN104775162A (zh) | 2015-07-15 |
| US9322781B2 (en) | 2016-04-26 |
| TWI507673B (zh) | 2015-11-11 |
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