CN112500863A - 海关安检系统核壳型发光材料隐蔽标识的制备及应用 - Google Patents
海关安检系统核壳型发光材料隐蔽标识的制备及应用 Download PDFInfo
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Abstract
本发明公开了海关安检系统核壳型发光材料隐蔽标识的制备及应用,涉及标记技术领域,针对现有的隐蔽标签中发光标记不够清晰,无法识别所标记异常行李的问题,现提出如下方案:步骤一、制备TiO2;步骤二、制备Ag@TiO2复合纳米粒子;步骤三、制备Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光粒子;步骤四、制备隐蔽行李标签。本发明提供的Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光粒子发光强度比纯NaYF4:Yb3+,Er3+有了显著提高,该发光材料能较好的分散在乙醇、甲醇等有机试剂中,用于制备隐蔽标签,标记可疑行李,为无感通关、智能通关、安全通关的研究提供了方向。
Description
技术领域
本发明涉及标记技术领域,尤其涉及海关安检系统核壳型发光材料隐蔽标识的制备及应用。
背景技术
随着经济的高速发展,海关出入境人流量也在逐渐攀升,通关检查任务量也在逐步增加,安全隐患也愈发显著。走私以逃避监管、偷税漏税、牟取暴利为目的,扰乱经济秩序,对国家经济造成极大危害,必须对此行为进行严厉打击。在巨大利益的驱使下走私方式不断更新,走私方法更加隐秘,查私查毒过程中证据收集及认证的难度日益增加。例如在走私违禁物品犯罪中,嫌疑人往往会将物品藏匿于行李企图抽身。当嫌疑人察觉行李异常时往往会放弃行李,逃之夭夭,因此海关需要在发现可疑行李时,做隐蔽标签使其不易被察觉,待嫌疑人领取行李,确认抓捕目标后立即展开行动,人赃并获。
目前红外发光材料尚未应用于无感通关领域,且现有的红外发光材料吸收截面小,上转换发光强度低,会导致发光标记不够清晰,无法识别所标记的异常行李。
发明内容
本发明的目的是为了解决上述背景技术中提出的目前红外发光材料尚未应用于无感通关领域,且现有的红外发光材料吸收截面小,上转换发光强度低,会导致发光标记不够清晰,无法识别所标记异常行李的问题,而提出的海关安检系统核壳型发光材料隐蔽标识的制备及应用。
为了实现上述目的,本发明采用了如下技术方案:
海关安检系统核壳型发光材料隐蔽标识的制备及应用,包括如下步骤:
步骤一、制备TiO2:将TiCl4滴入去离子水中,形成混合液,将含有硫酸铵和浓盐酸的溶液滴入混合液中,然后在15℃条件下进行搅拌,其中离子浓度比为Ti4+:H+:SO4 2-=15:1:30,充分搅拌溶解后将混合物以10℃/min的速度加热到95℃,保持1h,加入适量NH4OH溶液,调节pH值至5~7,冷却至室温,4500r/min离心10min,沉淀物用去离子水和乙醇清洗三次后放入80℃真空干燥箱中干燥10h;
步骤二、制备Ag@TiO2复合纳米粒子:将制备的TiO2浸入0.001~0.005mol/L浓度硝酸银溶液中,并在高压汞灯(100W)下照射3~9h,用高纯水以及乙醇洗涤3次,干燥后在450℃马弗炉中煅烧3h后备用。
步骤三、制备Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光粒子:取稀土硝酸盐溶液Y(NO3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2O进行搅拌,掺杂的镧系离子浓度摩尔比配比为Y3+:Yb3 +:Er3+=80:18:2,在搅拌情况下加入Ag@TiO2复合纳米粒子,混合后加入定量NaF,放到磁力搅拌器上搅拌25min后,水浴加热至90℃并保持2h,冷却后8000r/min离心10min,沉淀物用去离子水和乙醇清洗三次,将沉降的原料放入60℃真空干燥箱中干燥12h,得到Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光粒子。
步骤四、制备行李隐蔽标签:将制备好的Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光材料溶解在乙醇溶剂中,用喷枪喷涂在行李标签上,形成特定图案;数秒后溶剂挥发,行李标签表面不会留下痕迹,形成隐蔽标签。
优选的,海关安检系统核壳型发光材料隐蔽标识的应用,具体步骤如下:
步骤一、将制备好的Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光材料溶解在乙醇溶剂中,用喷枪喷涂在行李标签上,形成特定图案;
步骤二、数秒后溶剂挥发,行李标签表面不会留下痕迹,形成隐蔽标签;
步骤三、安检系统扫描托运行李的标签信息,锁定行李主人的身份信息;
步骤四、通过监控系统的人脸识别搜索对应的行李主人的位置动向,并实时监控;
步骤五、嫌疑人在提取行李时无法察觉,放松警惕,该标签通过装有980nm激光器的安检门时,表面红外发光材料吸收近红外光,发出特定图案的可见光;
步骤六、安检门识别异常并自动报警,安检人员将嫌疑人及可疑行李共同带入安检室,进行安全检查。
优选的,所述步骤一中喷枪内置于行李安检机的内部隐藏设置,通过喷枪将发光材料快速喷在行李的标签上,或者直接喷在行李的表面形成隐蔽标签。
优选的,对于需要托运的行李,在进入行李安检机前,安检人员先在行李上贴上对应个人信息的标签,然后在进入安检机进行行李检查,当行李安检机中检测到违禁行李,在喷涂隐蔽标签的同时,安检系统通过扫描行李上对应个人信息的标签,快速锁定嫌疑人信息;对于随身行李过安检机时,检测到可疑行李后直接在行李表面喷涂隐蔽标签。
优选的,根据安检系统锁定的嫌疑人信息,通过海关或车站内的监控系统,进行全方位的人脸识别,锁定嫌疑人位置,与最终提取行李的嫌疑人作对比,双向核查。
优选的,所述隐蔽标签的图案按照危险品的种类分类,同时对于同类危险品的危险等级制定不同的图案特征,形成具有等级提示分级显示的隐蔽标签。
优选的,所述步骤三中根据安检门照射出隐蔽标签的图案特征,直接观察到行李中危险品的等级,辅助下一步行李检查中对检察人员的分配及预备案的快速制定。
与现有技术相比,本发明的有益效果是:
1.本发明提供的海关安检系统核壳型发光材料隐蔽标识的制备及应用,通过将发光材料喷涂在行李上形成隐蔽标签,通过安检系统的行李扫描以及人脸识别,全面锁定相关人员,能够避免相关人员冒名顶替等,有助于全方位的安检核查。
2.所制作的材料以贵金属Ag纳米粒子为核,采用水解法制备的TiO2为隔离层,以NaYF4:Yb3+,Er3+为壳的核壳结构上转换发光纳米材料,将贵金属的等离子体共振效应和稀土离子的上转换发光的优良性质相结合,该方法合成的发光材料不仅改善了水溶性,还能较好地分散在乙醇、甲醇等有机试剂中,形成隐蔽标签,用于标记可疑行李,为无感通关、智能通关、安全通关的研究提供了方向。
附图说明
图1为本发明海关安检系统核壳型发光材料隐蔽标识应用的流程框图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合具体实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
参照图1所示,本发明采用如下方案:
实施例1
海关安检系统核壳型发光材料隐蔽标识的制备,包括如下步骤:
步骤一、制备TiO2:将TiCl4滴入去离子水中,形成混合液,将含有硫酸铵和浓盐酸的溶液滴入混合液中,然后在15℃条件下进行搅拌,其中离子浓度比为Ti4+:H+:SO4 2-=15:1:30,充分搅拌溶解后将混合物以10℃/min的速度加热到95℃,保持1h,加入适量NH4OH溶液,调节pH值至5,冷却至室温,4500r/min离心10min,沉淀物用去离子水和乙醇清洗三次后放入80℃真空干燥箱中干燥10h;
步骤二、制备Ag@TiO2复合纳米粒子:将制备的TiO2浸入0.001mol/L硝酸银溶液中,并在高压汞灯(100W)下照射3h后,用高纯水以及乙醇洗涤3次,干燥后在450℃马弗炉中煅烧3h后备用;
步骤三、制备Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光粒子:取稀土硝酸盐溶液Y(NO3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2O进行搅拌,掺杂的镧系离子浓度摩尔比配比为Y3+:Yb3 +:Er3+=80:18:2,在搅拌情况下加入Ag@TiO2复合纳米粒子,混合后加入定量NaF,放到磁力搅拌器上搅拌25min后,水浴加热至90℃并保持2h,冷却后8000r/min离心10min,沉淀物用去离子水和乙醇清洗三次,将沉降的原料放入60℃真空干燥箱中干燥12h,得到Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光粒子。
步骤四、制备行李隐蔽标签:将制备好的Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光材料溶解在乙醇溶剂中,用喷枪喷涂在行李标签上,形成特定图案;数秒后溶剂挥发,行李标签表面不会留下痕迹,形成隐蔽标签。
海关安检系统核壳型发光材料隐蔽标识的应用,具体步骤如下:
步骤一、将制备好的Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光材料溶解在乙醇溶剂中,用喷枪喷涂在行李标签上,形成特定图案;
步骤二、数秒后溶剂挥发,行李标签表面不会留下痕迹,形成隐蔽标签;
步骤三、安检系统扫描托运行李的标签信息,锁定行李主人的身份信息;
步骤四、通过监控系统的人脸识别搜索对应的行李主人的位置动向,并实时监控;
步骤五、嫌疑人在提取行李时无法察觉,放松警惕,该标签通过装有980nm激光器的安检门时,表面红外发光材料吸收近红外光,发出特定图案的可见光;
步骤六、安检门识别异常并自动报警,安检人员将嫌疑人及可疑行李共同带入安检室,进行安全检查。
在具体实施例中,所述步骤一中喷枪内置于行李安检机的内部隐藏设置,通过喷枪将发光材料快速喷在行李的标签上,或者直接喷在行李的表面形成隐蔽标签。
对于需要托运的行李,在进入行李安检机前,安检人员先在行李上贴上对应个人信息的标签,然后在进入安检机进行行李检查,当行李安检机中检测到违禁行李,在喷涂隐蔽标签的同时,安检系统通过扫描行李上对应个人信息的标签,快速锁定嫌疑人信息;对于随身行李过安检机时,检测到可疑行李后直接在行李表面喷涂隐蔽标签。
根据安检系统锁定的嫌疑人信息,通过海关或车站内的监控系统,进行全方位的人脸识别,锁定嫌疑人位置,与最终提取行李的嫌疑人作对比,双向核查。
所述隐蔽标签的图案按照危险品的种类分类,同时对于同类危险品的危险等级制定不同的图案特征,形成具有等级提示分级显示的隐蔽标签。
所述步骤三中根据安检门照射出隐蔽标签的图案特征,直接观察到行李中危险品的等级,辅助下一步行李检查中对检察人员的分配及预备案的快速制定。
实施例2
海关安检系统核壳型发光材料隐蔽标识的制备,包括如下步骤:
步骤一、制备TiO2:将TiCl4滴入去离子水中,形成混合液,将含有硫酸铵和浓盐酸的溶液滴入混合液中,然后在15℃条件下进行搅拌,其中离子浓度比为Ti4+:H+:SO4 2-=15:1:30,充分搅拌溶解后将混合物以10℃/min的速度加热到95℃,保持1h,加入适量NH4OH溶液,调节pH值至6,冷却至室温,4500r/min离心10min,沉淀物用去离子水和乙醇清洗三次后放入80℃真空干燥箱中干燥10h;
步骤二、制备Ag@TiO2复合纳米粒子:将制备的TiO2浸入0.003mol/L硝酸银溶液中,并在高压汞灯(100W)下照射6h后,用高纯水以及乙醇洗涤3次,干燥后在450℃马弗炉中煅烧3h后备用;
步骤三、制备Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光粒子:取稀土硝酸盐溶液Y(NO3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2O进行搅拌,掺杂的镧系离子浓度摩尔比配比为Y3+:Yb3 +:Er3+=80:18:2,在搅拌情况下加入Ag@TiO2复合纳米粒子,混合后加入定量NaF,放到磁力搅拌器上搅拌25min后,水浴加热至90℃并保持2h,冷却后8000r/min离心10min,沉淀物用去离子水和乙醇清洗三次,将沉降的原料放入60℃真空干燥箱中干燥12h,得到Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光粒子。
步骤四、制备行李隐蔽标签:将制备好的Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光材料溶解在乙醇溶剂中,用喷枪喷涂在行李标签上,形成特定图案;数秒后溶剂挥发,行李标签表面不会留下痕迹,形成隐蔽标签;嫌疑人在提取行李时无法察觉,放松警惕,该标签通过装有980nm激光器的安检门时,表面红外发光材料吸收近红外光,发出特定图案的可见光;安检门识别异常并自动报警,安检人员将嫌疑人及可疑行李共同带入安检室,进行安全检查。
实施例3
海关安检系统核壳型发光材料隐蔽标识的制备,包括如下步骤:
步骤一、制备TiO2:将TiCl4滴入去离子水中,形成混合液,将含有硫酸铵和浓盐酸的溶液滴入混合液中,然后在15℃条件下进行搅拌,其中离子浓度比为Ti4+:H+:SO4 2-=15:1:30,充分搅拌溶解后将混合物以10℃/min的速度加热到95℃,保持1h,加入适量NH4OH溶液,调节pH值至7,冷却至室温,4500r/min离心10min,沉淀物用去离子水和乙醇清洗三次后放入80℃真空干燥箱中干燥10h;
步骤二、制备Ag@TiO2复合纳米粒子:将制备的TiO2浸入0.005mol/L硝酸银溶液中,并在高压汞灯(100W)下照射9h后,用高纯水以及乙醇洗涤3次,干燥后在450℃马弗炉中煅烧3h后备用;
步骤三、制备Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光粒子:取稀土硝酸盐溶液Y(NO3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2O进行搅拌,掺杂的镧系离子浓度摩尔比配比为Y3+:Yb3 +:Er3+=80:18:2,在搅拌情况下加入Ag@TiO2复合纳米粒子,混合后加入定量NaF,放到磁力搅拌器上搅拌25min后,水浴加热至90℃并保持2h,冷却后8000r/min离心10min,沉淀物用去离子水和乙醇清洗三次,将沉降的原料放入60℃真空干燥箱中干燥12h,得到Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光粒子。
步骤四、制备行李隐蔽标签:将制备好的Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光材料溶解在乙醇溶剂中,用喷枪喷涂在行李标签上,形成特定图案;数秒后溶剂挥发,行李标签表面不会留下痕迹,形成隐蔽标签;嫌疑人在提取行李时无法察觉,放松警惕,该标签通过装有980nm激光器的安检门时,表面红外发光材料吸收近红外光,发出特定图案的可见光;安检门识别异常并自动报警,安检人员将嫌疑人及可疑行李共同带入安检室,进行安全检查。
综上,将实施例1,实施例2,实施例3得到的样品进行荧光图谱分析,结果显示980mm激光下,调节步骤一中pH值分别为5,6,7,在镧系离子浓度摩尔比配比为Y3+:Yb3+:Er3+=80:18:2条件下生成的Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光粒子荧光强度大,均可发出肉眼可见强烈的绿色可见光,具有有效的上转换发光效果。将实施例1,实施例2,实施例3得到的样品置于比色管中,加水至100ml,盖紧塞子,摇匀,经30min后取出比色管与另一只加入同等质量NaYF4:Yb3+,Er3+纳米发光粒子后加水至100ml的比色管一起放在黑色背景上,结果显示本发明制备的Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光粒子水溶性更好。同样方法测得在乙醇、甲醇中分散效果也较好。
本发明所提出的海关安检系统核壳型隐蔽发光材料的制备方法所得到的纳米发光粒子发光前水溶性较好,溶剂蒸发后隐形无感,不易察觉,且在经近红外光照射后有优秀的发光效果,用于标记可疑行李,为无感通关、智能通关、安全通关的研究提供了方向。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (7)
1.海关安检系统核壳型发光材料隐蔽标识的制备,其特征在于,包括如下步骤:
步骤一、水溶法制备TiO2:将TiCl4滴入去离子水中,形成混合液,将含有硫酸铵和浓盐酸的溶液滴入混合液中,然后在15℃条件下进行搅拌,其中离子浓度比为Ti4+:H+:SO4 2-=15:1:30,充分搅拌溶解后将混合物以10℃/min的速度加热到95℃,保持1h,加入适量NH4OH溶液,调节pH值至5~7,冷却至室温,4500r/min离心10min,沉淀物用去离子水和乙醇清洗三次后放入80℃真空干燥箱中干燥10h;
步骤二、制备Ag@TiO2复合纳米粒子:将制备的TiO2浸入0.001~0.005mol/L浓度硝酸银溶液中,并在高压汞灯100W下照射3~9h,用高纯水以及乙醇洗涤3次,干燥后在450℃马弗炉中煅烧3h后备用;
步骤三、制备Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光粒子:取稀土硝酸盐溶液Y(NO3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2O进行搅拌,掺杂的镧系离子浓度摩尔比为Y3+:Yb3+:Er3 +=80:18:2,在搅拌情况下加入Ag@TiO2复合纳米粒子,混合后加入定量NaF,放到磁力搅拌器上搅拌25min后,水浴加热至90℃并保持2h,冷却后8000r/min离心10min,沉淀物用去离子水和乙醇清洗三次,将沉降的原料放入60℃真空干燥箱中干燥12h,得到Ag@TiO2@NaYF4:Yb3 +,Er3+纳米发光粒子;
步骤四、制备行李隐蔽标签:将制备好的Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光材料溶解在乙醇溶剂中,用喷枪喷涂在行李标签上,形成特定图案;数秒后溶剂挥发,行李标签表面不会留下痕迹,形成隐蔽标签。
2.根据权利要求1所述的海关安检系统核壳型发光材料隐蔽标识的应用,其特征在于,具体步骤如下:
步骤一、将制备好的Ag@TiO2@NaYF4:Yb3+,Er3+纳米发光材料溶解在乙醇溶剂中,用喷枪喷涂在行李标签上,形成特定图案;
步骤二、数秒后溶剂挥发,行李标签表面不会留下痕迹,形成隐蔽标签;
步骤三、安检系统扫描托运行李的标签信息,锁定行李主人的身份信息;
步骤四、通过监控系统的人脸识别搜索对应的行李主人的位置动向,并实时监控;
步骤五、嫌疑人在提取行李时无法察觉,放松警惕,该标签通过装有980nm激光器的安检门时,表面红外发光材料吸收近红外光,发出特定图案的可见光;
步骤六、安检门识别异常并自动报警,安检人员将嫌疑人及可疑行李共同带入安检室,进行安全检查。
3.根据权利要求2所述的海关安检系统核壳型发光材料隐蔽标识的应用,其特征在于,所述步骤一中喷枪内置于行李安检机的内部隐藏设置,通过喷枪将发光材料快速喷在行李的标签上,或者直接喷在行李的表面形成隐蔽标签。
4.根据权利要求3所述的海关安检系统核壳型发光材料隐蔽标识的应用,其特征在于,对于需要托运的行李,在进入行李安检机前,安检人员先在行李上贴上对应个人信息的标签,然后在进入安检机进行行李检查,当行李安检机中检测到违禁行李,在喷涂隐蔽标签的同时,安检系统通过扫描行李上对应个人信息的标签,快速锁定嫌疑人信息;对于随身行李过安检机时,检测到可疑行李后直接在行李表面喷涂隐蔽标签。
5.根据权利要求4所述的海关安检系统核壳型发光材料隐蔽标识的应用,其特征在于,根据安检系统锁定的嫌疑人信息,通过海关或车站内的监控系统,进行全方位的人脸识别,锁定嫌疑人位置,与最终提取行李的嫌疑人作对比,双向核查。
6.根据权利要求3所述的海关安检系统核壳型发光材料隐蔽标识的应用,其特征在于,所述隐蔽标签的图案按照危险品的种类分类,同时对于同类危险品的危险等级制定不同的图案特征,形成具有等级提示分级显示的隐蔽标签。
7.根据权利要求2所述的海关安检系统核壳型发光材料隐蔽标识的应用,其特征在于,所述步骤三中根据安检门照射出隐蔽标签的图案特征,直接观察到行李中危险品的等级,辅助下一步行李检查中对检察人员的分配及预备案的快速制定。
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