CN102879795B - Application of KSr4(BO3)3:Ce3+ in Preparation of Electron Paramagnetic Resonance Dosimeter - Google Patents
Application of KSr4(BO3)3:Ce3+ in Preparation of Electron Paramagnetic Resonance Dosimeter Download PDFInfo
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- 238000004435 EPR spectroscopy Methods 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 44
- 238000001514 detection method Methods 0.000 claims abstract description 22
- 229910052684 Cerium Inorganic materials 0.000 abstract description 28
- 230000005855 radiation Effects 0.000 abstract description 19
- 238000001362 electron spin resonance spectrum Methods 0.000 abstract description 12
- 230000004044 response Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 229910052712 strontium Inorganic materials 0.000 abstract description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 abstract 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 abstract 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 18
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- 229910052593 corundum Inorganic materials 0.000 description 12
- 239000010431 corundum Substances 0.000 description 12
- 229910000420 cerium oxide Inorganic materials 0.000 description 11
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 11
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 11
- 229910000018 strontium carbonate Inorganic materials 0.000 description 11
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 9
- 239000004327 boric acid Substances 0.000 description 9
- 230000005298 paramagnetic effect Effects 0.000 description 9
- 229910000027 potassium carbonate Inorganic materials 0.000 description 9
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 description 8
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- 229910052799 carbon Inorganic materials 0.000 description 5
- 229910052810 boron oxide Inorganic materials 0.000 description 4
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 4
- 230000005865 ionizing radiation Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000004980 dosimetry Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
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Abstract
Description
技术领域 technical field
本发明涉及电子顺磁共振探测器技术领域，尤其涉及KSr4(BO3)3:Ce3+在制备电子顺磁共振剂量计中的应用。 The invention relates to the technical field of electron paramagnetic resonance detectors, in particular to the application of KSr 4 (BO 3 ) 3 : Ce 3+ in the preparation of electron paramagnetic resonance dosimeters.
背景技术 Background technique
电子顺磁共振是直接检测和研究含有未成对电子的顺磁性物质的现代分析方法。目前，电子顺磁共振已广泛应用于化学、物理、材料、环境、生命科学和医学等诸多领域。 Electron paramagnetic resonance is a modern analytical method for the direct detection and study of paramagnetic substances containing unpaired electrons. At present, electron paramagnetic resonance has been widely used in many fields such as chemistry, physics, materials, environment, life science and medicine. the
电子顺磁共振剂量测量方法是Bradshaw等人于1962年提出的（W.W.Bradshaw,D.G.Cadena,G.W.Crawford,H.A.W.Spetzler,The use of alanine as a solid dosimeter，Radiation Research，1962，17,11-21），它是利用特定样品在辐射后形成的稳定顺磁中心与辐射剂量成比例的关系对辐射剂量进行测量；并提出将丙氨酸作为电子顺磁共振剂量计中的探测器材料。之后研究人员对丙氨酸电子顺磁共振剂量计进行了大量的系统的研究。到1985年，基于丙氨酸的电子顺磁剂量测量方法已经成功的应用于工业范围内的辐射剂量测量中，并且这种方法在大剂量范围内的精确度很高，可以用做不同实验室的比对实验。 Electron paramagnetic resonance dose measurement method was proposed by Bradshaw et al. in 1962 (W.W.Bradshaw, D.G.Cadena, G.W.Crawford, H.A.W.Spetzler, The use of alanine as a solid dosimeter, Radiation Research, 1962, 17, 11-21), It uses the proportional relationship between the stable paramagnetic center formed by a specific sample after radiation and the radiation dose to measure the radiation dose; and proposes to use alanine as the detector material in the electron paramagnetic resonance dosimeter. After that, the researchers conducted a lot of systematic research on the alanine electron paramagnetic resonance dosimeter. By 1985, the electronic paramagnetic dosimetry method based on alanine had been successfully applied to the radiation dosimetry on an industrial scale, and the accuracy of this method in the large dose range was very high, and it could be used in different laboratories comparison experiment. the
丙氨酸电子顺磁共振剂量计具有如下优点：1、组织等效性好；2、体积小，使用起来方便灵活；3、辐照后信号稳定；4、读取信号不具有破坏性，能够反复多次测量，也可以将信号累计起来测量；5、它对于光子和电子束的剂量率和能量依赖性非常小（M.Lin,T.Garcia,V.Lourenco,Y.Cui,Y.Z.Chen,F.Wang，Bilateral comparison of an alanine/ESR dosimetry system at radiotherapy dose levels,Radiation Measurements,2010,45,789-796）。鉴于这些优点，丙氨酸电子顺磁共振剂量计被认为是一种经典的测量高剂量0.1~100kGy电离辐射的剂量计而广泛的使用。但是丙氨酸电子顺磁共振剂量计在测量辐射治疗级或个人防护级等低剂量电离辐射时却不适用。因此，提 高电子顺磁共振剂量计的灵敏度，将电子顺磁共振剂量计测量电离辐射剂量的范围延伸至低剂量范围是目前很多研究人员的目标。 The alanine electronic paramagnetic resonance dosimeter has the following advantages: 1. Good tissue equivalence; 2. Small size, convenient and flexible to use; 3. The signal is stable after irradiation; 4. The read signal is not destructive and can Repeated measurements can also be accumulated to measure the signal; 5. Its dose rate and energy dependence on photons and electron beams is very small (M.Lin, T.Garcia, V.Lourenco, Y.Cui, Y.Z.Chen, F. Wang, Bilateral comparison of an alanine/ESR dosimetry system at radiotherapy dose levels, Radiation Measurements, 2010, 45, 789-796). In view of these advantages, the alanine electron paramagnetic resonance dosimeter is considered as a classic dosimeter for measuring high doses of ionizing radiation ranging from 0.1 to 100 kGy and is widely used. However, alanine electron paramagnetic resonance dosimeters are not suitable for measuring low doses of ionizing radiation such as radiation therapy grades or personal protection grades. Therefore, improving the sensitivity of the electron paramagnetic resonance dosimeter and extending the range of the electron paramagnetic resonance dosimeter to measure the ionizing radiation dose to the low dose range are the goals of many researchers. the
发明内容 Contents of the invention
有鉴于此，本发明所要解决的技术问题在于提供KSr4(BO3)3:Ce3+在制备电子顺磁共振剂量计中的应用，以KSr4(BO3)3:Ce3+作为电子顺磁剂量计中的探测材料，能够实现对低剂量范围电离辐射进行测量。 In view of this, the technical problem to be solved by the present invention is to provide the application of KSr 4 (BO 3 ) 3 : Ce 3+ in the preparation of electron paramagnetic resonance dosimeter, with KSr 4 (BO 3 ) 3 : Ce 3+ as electron The detection material in the paramagnetic dosimeter can realize the measurement of ionizing radiation in the low dose range.
本发明提供了一种KSr4(BO3)3:Ce3+在制备电子顺磁共振剂量计中的应用，其中，KSr4(BO3)3:Ce3+中Ce与Sr的摩尔比为0.0001~0.1：1。 The present invention provides a kind of application of KSr 4 (BO 3 ) 3 :Ce 3+ in the preparation of electron paramagnetic resonance dosimeter, wherein, the molar ratio of Ce and Sr in KSr 4 (BO 3 ) 3 :Ce 3+ is 0.0001~0.1:1.
优选的，所述Ce与Sr的摩尔比为0.0005～0.09：1。 Preferably, the molar ratio of Ce to Sr is 0.0005˜0.09:1. the
优选的，所述Ce与Sr的摩尔比为0.002～0.08：1。 Preferably, the molar ratio of Ce to Sr is 0.002˜0.08:1. the
本发明还提供了一种电子顺磁共振剂量计，其电子顺磁共振探测材料为KSr4(BO3)3:Ce3+，其中，Ce与Sr的摩尔比为0.0001～0.1：1。 The present invention also provides an electron paramagnetic resonance dosimeter, the electron paramagnetic resonance detection material is KSr 4 (BO 3 ) 3 :Ce 3+ , wherein the molar ratio of Ce to Sr is 0.0001-0.1:1.
优选的，所述Ce与Sr的摩尔比为0.0005～0.09：1。 Preferably, the molar ratio of Ce to Sr is 0.0005˜0.09:1. the
优选的，所述Ce与Sr的摩尔比为0.002～0.08：1。 Preferably, the molar ratio of Ce to Sr is 0.002˜0.08:1. the
与现有技术相比，本发明将KSr4(BO3)3:Ce3+用作电子顺磁共振剂量计中的探测材料，其中，KSr4(BO3)3:Ce3+中Ce与Sr的摩尔比为0.0001~0.1：1。KSr4(BO3)3:Ce3+经辐照后，得到的电子顺磁共振谱由六个信号组成；以最强的信号作为电子顺磁共振探测信号，可实现在辐射剂量为0.89~90.30Gy范围内的测量。实验表明，以上述较强的信号作为电磁共振探测信号，在辐射剂量为0.89~90.30Gy范围内，所述探测材料在所测剂量范围内有响应，且呈线性响应，线性相关系数为0.9997~0.9999，说明本发明所述探测材料可以用于低剂量范围内辐射剂量的测量，且灵敏度高。此外，KSr4(BO3)3:Ce3+材料的制备工艺简单，原料便宜易得，生产成本低廉。 Compared with the prior art, the present invention uses KSr 4 (BO 3 ) 3 :Ce 3+ as the detection material in the electron paramagnetic resonance dosimeter, wherein, Ce in KSr 4 (BO 3 ) 3 :Ce 3+ and The molar ratio of Sr is 0.0001~0.1:1. After KSr 4 (BO 3 ) 3 :Ce 3+ is irradiated, the electron paramagnetic resonance spectrum obtained consists of six signals; the strongest signal is used as the electron paramagnetic resonance detection signal, which can be achieved at a radiation dose of 0.89~ Measurements in the range of 90.30Gy. Experiments show that when the above strong signal is used as the electromagnetic resonance detection signal, within the radiation dose range of 0.89~90.30Gy, the detection material has a response within the measured dose range, and the response is linear, and the linear correlation coefficient is 0.9997~ 0.9999, indicating that the detection material of the present invention can be used for the measurement of radiation dose in the low dose range, and has high sensitivity. In addition, the preparation process of the KSr 4 (BO 3 ) 3 :Ce 3+ material is simple, the raw materials are cheap and easy to obtain, and the production cost is low.
附图说明 Description of drawings
图1为本发明实施例2制备的KSr4(BO3)3:0.2%Ce3+材料被γ射线辐照后的电子顺磁共振谱； Fig. 1 is the electron paramagnetic resonance spectrum of the KSr 4 (BO 3 ) 3 :0.2%Ce 3+ material prepared in Example 2 of the present invention after being irradiated by gamma rays;
图2为本发明实施例2制备的KSr4(BO3)3:0.2%Ce3+材料对γ射线的剂量响应曲线。 Fig. 2 is the dose-response curve of the KSr 4 (BO 3 ) 3 :0.2%Ce 3+ material prepared in Example 2 of the present invention to γ-rays.
具体实施方式 Detailed ways
本发明提供了一种KSr4(BO3)3:Ce3+在制备电子顺磁共振剂量计中的应用，其中，KSr4(BO3)3:Ce3+中Ce与Sr的摩尔比为0.0001~0.1：1，优选为0.0005～0.09：1，更优选为0.002～0.08：1。本发明还提供了一种电子顺磁共振剂量计，其电子顺磁共振探测材料为KSr4(BO3)3:Ce3+，其中，Ce与Sr的摩尔比为0.0001～0.1：1，优选为0.0005～0.09：1，更优选为0.002～0.08：1。 The present invention provides a kind of application of KSr 4 (BO 3 ) 3 :Ce 3+ in the preparation of electron paramagnetic resonance dosimeter, wherein, the molar ratio of Ce and Sr in KSr 4 (BO 3 ) 3 :Ce 3+ is 0.0001-0.1:1, preferably 0.0005-0.09:1, more preferably 0.002-0.08:1. The present invention also provides an electron paramagnetic resonance dosimeter, the electron paramagnetic resonance detection material is KSr 4 (BO 3 ) 3 :Ce 3+ , wherein the molar ratio of Ce to Sr is 0.0001-0.1:1, preferably 0.0005-0.09:1, more preferably 0.002-0.08:1.
本发明所述KSr4(BO3)3:Ce3+经辐照后，得到的电子顺磁共振谱由六个信号组成；将最强的信号作为电子顺磁共振探测信号，通过测量探测材料KSr4(BO3)3:Ce3+在辐射剂量为0.89-90.30Gy范围内的响应情况，实验结果呈现较好的线性，线性相关系数为0.9997~0.9999。 After the KSr 4 (BO 3 ) 3 :Ce 3+ in the present invention is irradiated, the electron paramagnetic resonance spectrum obtained is composed of six signals; the strongest signal is used as the electron paramagnetic resonance detection signal, and the detection material is measured The response of KSr 4 (BO 3 ) 3 :Ce 3+ in the radiation dose range of 0.89-90.30Gy, the experimental results show a good linearity, and the linear correlation coefficient is 0.9997~0.9999.
在本发明中，所述KSr4(BO3)3:Ce3+为Ce掺杂的KSr4(BO3)3，其可以按照以下步骤制备获得： In the present invention, the KSr 4 (BO 3 ) 3 :Ce 3+ is Ce-doped KSr 4 (BO 3 ) 3 , which can be prepared according to the following steps:
将碳酸钾、碳酸锶、硼酸或氧化硼和氧化铈混合，预烧，所述氧化铈和所述碳酸锶的摩尔比为0.0001～0.1：1； Potassium carbonate, strontium carbonate, boric acid or boron oxide and cerium oxide are mixed and calcined, and the molar ratio of the cerium oxide to the strontium carbonate is 0.0001-0.1:1;
将预烧后的混合物研磨，在还原气体气氛中烧结，得到KSr4(BO3)3:Ce3+。 The pre-fired mixture is ground and sintered in a reducing gas atmosphere to obtain KSr 4 (BO 3 ) 3 :Ce 3+ .
按照本发明，将碳酸钾、碳酸锶、硼酸或氧化硼和氧化铈在研钵中充分研磨混合，在刚玉坩埚中进行预烧。所述碳酸钾优选为分析纯的碳酸钾，所述碳酸锶优选为分析纯的碳酸锶，所述硼酸或氧化硼优选为分析纯的硼酸或氧化硼，所述氧化铈优选为纯度为99.99%的氧化铈；所述氧化铈和所述碳酸锶的摩尔比为0.0001～0.1：1，优选为0.0005～0.09：1，更优选为0.002～0.08： 1。 According to the present invention, potassium carbonate, strontium carbonate, boric acid or boron oxide and cerium oxide are thoroughly ground and mixed in a mortar, and pre-fired in a corundum crucible. The potassium carbonate is preferably analytically pure potassium carbonate, the strontium carbonate is preferably analytically pure strontium carbonate, the boric acid or boron oxide is preferably analytically pure boric acid or boron oxide, and the cerium oxide preferably has a purity of 99.99%. cerium oxide; the molar ratio of the cerium oxide to the strontium carbonate is 0.0001-0.1:1, preferably 0.0005-0.09:1, more preferably 0.002-0.08: 1 .
本发明所述预烧是在空气气氛中进行的。所述预烧的时间优选为2~5小时，更优选为2.5~4.5小时；所述预烧的温度优选为300℃~650℃，更优选为350℃~550℃。 The pre-firing in the present invention is carried out in an air atmosphere. The pre-calcination time is preferably 2-5 hours, more preferably 2.5-4.5 hours; the pre-calcination temperature is preferably 300°C-650°C, more preferably 350°C-550°C. the
按照本发明，将预烧得到的混合物在研钵中进行研磨，在刚玉坩埚中于还原气体气氛中烧结，使各原料充分发生反应，得到KSr4(BO3)3:Ce3+。所述还原气体优选为CO、H2或N2和H2的混合气；所述烧结的时间优选为8~20小时，更优选为10~18小时；所述烧结的温度优选为650℃~1000℃，更优选为700℃~900℃。 According to the present invention, the pre-calcined mixture is ground in a mortar and sintered in a corundum crucible in a reducing gas atmosphere to fully react each raw material to obtain KSr 4 (BO 3 ) 3 :Ce 3+ . The reducing gas is preferably CO, H 2 or a mixture of N 2 and H 2 ; the sintering time is preferably 8 to 20 hours, more preferably 10 to 18 hours; the sintering temperature is preferably 650° C. to 1000°C, more preferably 700°C to 900°C.
本发明将KSr4(BO3)3:Ce3+用作电子顺磁共振剂量计中的探测材料，其中，KSr4(BO3)3:Ce3+中Ce与Sr的摩尔比为0.0001~0.1：1。KSr4(BO3)3:Ce3+经辐照 后，得到的电子顺磁共振谱由六个信号组成；以最强的信号作为电子顺磁共振探测信号，可实现在辐射剂量为0.89~90.30Gy范围内的测量。实验表明，以较强的信号作为电磁共振探测信号，在辐射剂量为0.89~90.30Gy范围内，所述探测材料在所测剂量范围内有响应，且呈线性响应，说明本发明所述探测材料可以用作低剂量范围内辐射剂量的测量，且灵敏度高。此外，KSr4(BO3)3:Ce3+材料的制备工艺简单，原料便宜易得，生产成本低廉。 The present invention uses KSr 4 (BO 3 ) 3 :Ce 3+ as the detection material in the electron paramagnetic resonance dosimeter, wherein the molar ratio of Ce to Sr in KSr 4 (BO 3 ) 3 :Ce 3+ is 0.0001~ 0.1:1. After KSr 4 (BO 3 ) 3 :Ce 3+ is irradiated, the electron paramagnetic resonance spectrum obtained consists of six signals; the strongest signal is used as the electron paramagnetic resonance detection signal, which can be achieved at a radiation dose of 0.89~ Measurements in the range of 90.30Gy. Experiments have shown that using a stronger signal as the electromagnetic resonance detection signal, within the range of 0.89 to 90.30Gy of radiation dose, the detection material has a response within the measured dose range, and a linear response, indicating that the detection material of the present invention It can be used to measure the radiation dose in the low dose range with high sensitivity. In addition, the preparation process of the KSr 4 (BO 3 ) 3 :Ce 3+ material is simple, the raw materials are cheap and easy to obtain, and the production cost is low.
为了进一步理解本发明，下面结合实施例对本发明提供的KSr4(BO3)3:Ce3+在制备电子顺磁共振剂量计中的应用进行详细描述。 In order to further understand the present invention, the application of KSr 4 (BO 3 ) 3 :Ce 3+ provided by the present invention in the preparation of electron paramagnetic resonance dosimeters will be described in detail below in conjunction with examples.
实施例1 Example 1
取1mol分析纯的碳酸钾、8mol分析纯的碳酸锶、6mol分析纯的硼酸和0.004mol纯度为99.9%的氧化铈在研钵中充分研磨均匀并烘干后放入刚玉坩埚中，在空气气氛中，在550℃的温度下预烧2.5h，将预烧得到的混合物冷却至室温，再次在研钵中充分研磨并混合均匀，放入刚玉坩埚中，在周围填充碳棒的条件下，在750℃的温度下焙烧12个小时，自然冷却到室温，在研钵中研磨后得到KSr4(BO3)3:0.05%Ce3+。 Take 1 mol of analytically pure potassium carbonate, 8 mol of analytically pure strontium carbonate, 6 mol of analytically pure boric acid and 0.004 mol of cerium oxide with a purity of 99.9%, fully grind them evenly in a mortar, dry them, put them into a corundum crucible, and place them in an air atmosphere , pre-fired at a temperature of 550°C for 2.5 hours, cooled the pre-fired mixture to room temperature, thoroughly ground it again in a mortar and mixed it evenly, put it into a corundum crucible, and filled it with carbon rods around it. Calcined at 750°C for 12 hours, cooled naturally to room temperature, and ground in a mortar to obtain KSr 4 (BO 3 ) 3 :0.05%Ce 3+ .
KSr4(BO3)3:0.05%Ce3+被1000Gy 60Co γ射线辐照后得到的电子顺磁共振谱由六个信号组成。 The electron paramagnetic resonance spectrum of KSr 4 (BO 3 ) 3 :0.05%Ce 3+ irradiated by 1000Gy 60 Co γ-rays consists of six signals.
KSr4(BO3)3:0.05%Ce3+材料分别被0.89Gy、9.03Gy、18.06Gy、45.15Gy和90.30Gy的60Coγ射线辐照，得到相应的电子顺磁信号强度，获得的电子顺磁信号强度与所受辐照剂量作图，即剂量响应曲线图，结果表明，本发明提供的KSr4(BO3)3:0.05%Ce3+材料在低剂量范围内呈现较好的线性，说明本发明的材料可用作电子顺磁共振剂量计材料，且灵敏度高。 The KSr 4 (BO 3 ) 3 :0.05%Ce 3+ material was irradiated by 0.89Gy, 9.03Gy, 18.06Gy, 45.15Gy and 90.30Gy 60Coγ -rays respectively, and the corresponding electronic paramagnetic signal intensity was obtained. The magnetic signal intensity is plotted against the received radiation dose, that is, the dose-response curve, and the results show that the KSr 4 (BO 3 ) 3 :0.05%Ce 3+ material provided by the present invention exhibits better linearity in the low dose range, It shows that the material of the present invention can be used as electron paramagnetic resonance dosimeter material, and has high sensitivity.
实施例2 Example 2
取1mol分析纯的碳酸钾、8mol分析纯的碳酸锶、6mol分析纯的硼酸和0.016mol纯度为99.9%的氧化铈在研钵中充分研磨均匀并烘干后放入刚玉坩埚中，在空气气氛中，在500℃的温度下预烧3h，将预烧得到的混合物冷却至室温，再次在研钵中充分研磨并混合均匀，放入刚玉坩埚中，在周围填充碳棒的条件下，在700℃的温度下焙烧10个小时，自然冷却到室温，在研钵中研磨后得到KSr4(BO3)3:0.2%Ce3+。 Take 1 mol of analytically pure potassium carbonate, 8 mol of analytically pure strontium carbonate, 6 mol of analytically pure boric acid and 0.016 mol of cerium oxide with a purity of 99.9%, fully grind them evenly in a mortar, dry them, put them into a corundum crucible, and place them in an air atmosphere , pre-fired at a temperature of 500°C for 3 hours, cooled the pre-fired mixture to room temperature, thoroughly ground it again in a mortar and mixed it evenly, put it into a corundum crucible, and filled it with carbon rods around it. Calcined at ℃ for 10 hours, cooled naturally to room temperature, and ground in a mortar to obtain KSr 4 (BO 3 ) 3 :0.2%Ce 3+ .
KSr4(BO3)3:0.2%Ce3+被1000Gy 60Coγ射线辐照后得到的电子顺磁共振谱参见图1。图1为本发明实施例2制备的KSr4(BO3)3:0.2%Ce3+材料被γ射线辐照后的电子顺磁共振谱。由图1可知，KSr4(BO3)3:0.2%Ce3+材料的电子顺磁共振谱由六个信号组成。 See Figure 1 for the electron paramagnetic resonance spectrum obtained after KSr 4 (BO 3 ) 3 :0.2%Ce 3+ was irradiated by 1000Gy 60 Coγ-rays. Fig. 1 is the electron paramagnetic resonance spectrum of the KSr 4 (BO 3 ) 3 :0.2%Ce 3+ material prepared in Example 2 of the present invention after being irradiated by γ-rays. It can be seen from Fig. 1 that the electron paramagnetic resonance spectrum of KSr 4 (BO 3 ) 3 :0.2%Ce 3+ material consists of six signals.
KSr4(BO3)3:0.2%Ce3+材料分别被0.89Gy、9.03Gy、18.06Gy、45.15Gy和90.30Gy的60Coγ射线辐照，得到相应的电子顺磁信号强度，获得的电子顺磁信号强度与所受辐照剂量作图，即剂量响应曲线图，结果参见图2，图2为本发明实施例2制备的KSr4(BO3)3:0.2%Ce3+材料对γ射线的剂量响应曲线。由图2可知，本发明提供的KSr4(BO3)3:0.2%Ce3+材料在低剂量范围内呈现较好的线性，线性相关系数为0.9998，说明本发明的材料可用作电子顺磁共振剂量计材料，且灵敏度高。 The KSr 4 (BO 3 ) 3 :0.2%Ce 3+ material was irradiated by 0.89Gy, 9.03Gy, 18.06Gy, 45.15Gy and 90.30Gy 60Coγ -rays respectively, and the corresponding electronic paramagnetic signal intensity was obtained. The magnetic signal intensity is plotted against the received radiation dose, that is, the dose-response curve, and the results are shown in Figure 2. Figure 2 shows the response of the KSr 4 (BO 3 ) 3 :0.2%Ce 3+ material to γ-rays prepared in Example 2 of the present invention. dose-response curve. It can be seen from Figure 2 that the KSr 4 (BO 3 ) 3 :0.2%Ce 3+ material provided by the present invention exhibits good linearity in the low dose range, and the linear correlation coefficient is 0.9998, indicating that the material of the present invention can be used as a Magnetic resonance dosimeter material with high sensitivity.
实施例3 Example 3
取1mol分析纯的碳酸钾、8mol分析纯的碳酸锶、6mol分析纯的硼酸和0.16mol纯度为99.9%的氧化铈在研钵中充分研磨均匀并烘干后放入刚玉坩埚中，在空气气氛中，在450℃的温度下预烧4.5h，将预烧得到的混合物冷却至室温，再次在研钵中充分研磨并混合均匀，放入刚玉坩埚中，在周围填充碳棒的条件下，在800℃的温度下焙烧15个小时，自然冷却到室温，在研钵中研磨后得到KSr4(BO3)3:2%Ce3+。 Take 1 mol of analytically pure potassium carbonate, 8 mol of analytically pure strontium carbonate, 6 mol of analytically pure boric acid, and 0.16 mol of cerium oxide with a purity of 99.9%, fully grind them in a mortar and put them into a corundum crucible after drying. , pre-fired at 450°C for 4.5 hours, cooled the mixture obtained by pre-fired to room temperature, thoroughly ground it again in a mortar and mixed it evenly, put it into a corundum crucible, and filled it with carbon rods around it. Calcined at 800°C for 15 hours, cooled naturally to room temperature, and ground in a mortar to obtain KSr 4 (BO 3 ) 3 :2%Ce 3+ .
KSr4(BO3)3:2%Ce3+被1000Gy 60Coγ射线辐照后得到的电子顺磁共振谱由六个信号组成。 The electron paramagnetic resonance spectrum of KSr 4 (BO 3 ) 3 :2%Ce 3+ irradiated by 1000Gy 60 Coγ-rays consists of six signals.
KSr4(BO3)3:2%Ce3+材料分别被0.89Gy、9.03Gy、18.06Gy、45.15Gy和90.30Gy的60Coγ射线辐照，得到相应的电子顺磁信号强度，获得的电子顺磁信号强度与所受辐照剂量作图，即剂量响应曲线图，结果表明，本发明提供的KSr4(BO3)3:2%Ce3+材料在低剂量范围内呈现较好的线性，说明本发明的材料可用作电子顺磁共振剂量计材料，且灵敏度高。 KSr 4 (BO 3 ) 3 : 2%Ce 3+ material was irradiated by 0.89Gy, 9.03Gy, 18.06Gy, 45.15Gy and 90.30Gy 60Coγ -rays respectively, and the corresponding electronic paramagnetic signal intensity was obtained. The magnetic signal intensity is plotted against the received radiation dose, that is, the dose-response curve, and the results show that the KSr 4 (BO 3 ) 3 :2%Ce 3+ material provided by the present invention presents better linearity in the low dose range, It shows that the material of the present invention can be used as electron paramagnetic resonance dosimeter material, and has high sensitivity.
实施例4 Example 4
取1mol分析纯的碳酸钾、8mol分析纯的碳酸锶、6mol分析纯的硼酸和0.32mol纯度为99.9%的氧化铈在研钵中充分研磨均匀并烘干后放入刚玉坩埚中，在空气气氛中，在400℃的温度下预烧3h，将预烧得到的混合物冷却至室温，再次在研钵中充分研磨并混合均匀，放入刚玉坩埚中，在周围填充碳 棒的条件下，在850℃的温度下焙烧16个小时，自然冷却到室温，在研钵中研磨后得到KSr4(BO3)3:4%Ce3+。 Take 1 mol of analytically pure potassium carbonate, 8 mol of analytically pure strontium carbonate, 6 mol of analytically pure boric acid and 0.32 mol of cerium oxide with a purity of 99.9%, fully grind them evenly in a mortar, dry them, put them into a corundum crucible, and place them in an air atmosphere , pre-fired at a temperature of 400°C for 3 hours, cooled the pre-fired mixture to room temperature, thoroughly ground it again in a mortar and mixed it evenly, put it into a corundum crucible, and filled it with carbon rods around it. Calcined at ℃ for 16 hours, cooled naturally to room temperature, and ground in a mortar to obtain KSr 4 (BO 3 ) 3 :4%Ce 3+ .
KSr4(BO3)3:4%Ce3+被1000Gy 60Coγ射线辐照后得到的电子顺磁共振谱由六个信号组成。 The electron paramagnetic resonance spectrum of KSr 4 (BO 3 ) 3 :4%Ce 3+ irradiated by 1000Gy 60 Coγ-rays consists of six signals.
KSr4(BO3)3:4%Ce3+材料分别被0.89Gy、9.03Gy、18.06Gy、45.15Gy和90.30Gy的60Coγ射线辐照，得到相应的电子顺磁信号强度，获得的电子顺磁信号强度与所受辐照剂量作图，即剂量响应曲线图，结果表明，本发明提供的KSr4(BO3)3:4%Ce3+材料在低剂量范围内呈现较好的线性，说明本发明的材料可用作电子顺磁共振剂量计材料，且灵敏度高。 The KSr 4 (BO 3 ) 3 : 4%Ce 3+ material was irradiated by 0.89Gy, 9.03Gy, 18.06Gy, 45.15Gy and 90.30Gy 60 Coγ-rays respectively, and the corresponding electron paramagnetic signal intensity was obtained. The magnetic signal intensity is plotted against the received radiation dose, that is, the dose-response curve, and the results show that the KSr 4 (BO 3 ) 3 :4%Ce 3+ material provided by the present invention presents better linearity in the low dose range, It shows that the material of the present invention can be used as electron paramagnetic resonance dosimeter material, and has high sensitivity.
实施例5 Example 5
取1mol分析纯的碳酸钾、8mol分析纯的碳酸锶、6mol分析纯的硼酸和0.64mol纯度为99.9%的氧化铈在研钵中充分研磨均匀并烘干后放入刚玉坩埚中，在空气气氛中，在350℃的温度下预烧4h，将预烧得到的混合物冷却至室温，再次在研钵中充分研磨并混合均匀，放入刚玉坩埚中，在周围填充碳棒的条件下，在900℃的温度下焙烧18个小时，自然冷却到室温，在研钵中研磨后得到KSr4(BO3)3:8%Ce3+。 Take 1 mol of analytically pure potassium carbonate, 8 mol of analytically pure strontium carbonate, 6 mol of analytically pure boric acid, and 0.64 mol of cerium oxide with a purity of 99.9%, fully grind them evenly in a mortar, dry them, put them into a corundum crucible, and place them in an air atmosphere , pre-fired at a temperature of 350°C for 4 hours, cooled the pre-fired mixture to room temperature, thoroughly ground it again in a mortar and mixed it evenly, put it into a corundum crucible, and filled it with carbon rods around it. Calcined at ℃ for 18 hours, cooled naturally to room temperature, and ground in a mortar to obtain KSr 4 (BO 3 ) 3 :8%Ce 3+ .
KSr4(BO3)3:8%Ce3+被1000Gy 60Coγ射线辐照后得到的电子顺磁共振谱由六个信号组成。 The electron paramagnetic resonance spectrum of KSr 4 (BO 3 ) 3 :8%Ce 3+ irradiated by 1000Gy 60 Coγ-rays consists of six signals.
KSr4(BO3)3:8%Ce3+材料分别被0.89Gy、9.03Gy、18.06Gy、45.15Gy和90.30Gy的60Coγ射线辐照，得到相应的电子顺磁信号强度，获得的电子顺磁信号强度与所受辐照剂量作图，即剂量响应曲线图，结果表明，本发明提供的KSr4(BO3)3:,8%Ce3+材料在低剂量范围内呈现较好的线性，说明本发明的材料可用作电子顺磁共振剂量计材料，且灵敏度高。 The KSr 4 (BO 3 ) 3 :8%Ce 3+ material was irradiated by 0.89Gy, 9.03Gy, 18.06Gy, 45.15Gy and 90.30Gy 60Coγ -rays respectively, and the corresponding electronic paramagnetic signal intensity was obtained. The magnetic signal intensity is plotted against the received radiation dose, that is, the dose response curve, and the results show that the KSr 4 (BO 3 ) 3 :, 8%Ce 3+ material provided by the present invention exhibits better linearity in the low dose range , indicating that the material of the present invention can be used as an electron paramagnetic resonance dosimeter material, and has high sensitivity.
以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以对本发明进行若干改进和修饰，这些改进和修饰也落入本发明权利要求的保护范围内。 The descriptions of the above embodiments are only used to help understand the method and core idea of the present invention. It should be pointed out that for those skilled in the art, without departing from the principle of the present invention, some improvements and modifications can be made to the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention. the
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