CN111548788A - 一种基于荧光法检测氧气的复合传感膜及其使用方法 - Google Patents
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Abstract
一种基于荧光法检测氧气的复合传感膜及其使用方法,传感膜包括有透明支撑基材层,所述透明支撑基材层表面结合有荧光材料镀层,所述荧光材料镀层表面结合有散射光镀层,所述散射光镀层表面结合有黑色镀层,采用以下步骤使用传感膜:S1、用红光作为参比光源,用绿光或蓝光作为激发光源,辐照传感膜的透明支撑层,利用荧光淬灭原理,通过氧气分子与荧光染料分子的相互作用,产生激发红光;S2、经光电二极管检测采集,将光信号转换为电信号,通过处理模块对数据进行非线性算法拟合处理,获得氧气浓度的变化。
Description
技术领域
本发明涉及传感器技术领域,具体涉及一种基于荧光法检测氧气的复合传感膜及其使用方法。
背景技术
水中溶解的氧气含量是衡量水质好坏重要指标之一,溶解氧对于水生动植物存活环境的重要性及水体健康程度的重要性犹如空气中的氧对人类的重要性一样。国际上水中溶解氧的检测技术到目前为止经历了三代(注:水中溶解氧的检测本质上仍然是检测氧分子浓度)。
第一代即传统的比色法和Winkler滴定法(1956年之前):比色法精度和测量范围有限,尤其是在检测低浓度时引入的误差较大;Winkler滴定法虽然精度有保证但操作复杂,人为引入的误差不可避免。
第二代即电化学检测方法(1956-2003年):通常检测系统由两部分组成,一是前端探头部分或传感单元,二是后端数字显示部分。电化学溶解氧传感器的传感单元通常由阴极和阳极构成,在一定的电解质溶液中当被检测样品中的氧气扩散到电极表面后,经由电化学反应产生对应的电流信号,溶解氧浓度经数据经处理后通过表端显示。电化学传感器性能不仅受制于流速的影响,而且此类传感器在废水和污水处理应用中,由于探头部分容易受污染而降低灵敏度从而影响传感器长期稳定性,且需定期添加化学试剂,因而维护成本高。
第三代即光学传感技术(2003-现在):采用荧光淬灭原理,通过氧气分子与荧光分子的相互作用,获得溶解氧浓度随荧光淬灭的变化曲线,通过一定算法来计算被测氧分子浓度。与电化学溶解氧传感器相比,安装维护非常简单,无需添加任何电解质溶液或化学试剂,不受制于流速的影响且可实现即插即用。
基于荧光检测技术的第三代氧气传感器,其检测精度和灵敏度取决于传感单元核心部件,也就是传感膜对荧光信号产生的光化反应感知灵敏度,因而功能化传感膜单元成为传感器核心部件。高性能传感单元能将环境被测信号转换为可定量表征的稳定的原始数据,从而使得传感膜对荧光信号产生的光化反应感知灵敏度十分重要,现有技术存在改进之处。
发明内容
为解决上述技术问题,本发明提出了一种基于荧光法检测氧气的复合传感膜,依次设置的透明支撑基材层、荧光材料镀层、散射光镀层、黑色镀层保证传感膜对光化反应感知灵敏度,从而保证对溶解氧浓度检测的精度。
为达到上述目的,本发明的技术方案如下:一种基于荧光法检测氧气的复合传感膜,其特征在于,包括有透明支撑基材层,所述透明支撑基材层表面结合有荧光材料镀层,所述荧光材料镀层表面结合有散射光镀层,所述散射光镀层表面结合有黑色镀层。
本发明进一步设置为:所述散射光镀层与所述黑色镀层之间设置有反光层。
本发明进一步设置为:反光层采用Ag或Pt或Pd金屈材料制成,所述反光层的厚度在0.0-100μm。
本发明进一步设置为:所述透明支撑基材层采用玻璃或塑料材质制成。
本发明进一步设置为:所述散射光镀层采用钛白粉、SiO2、六方氮化硼、ZrO2、TiO2、MgF2、Al2O3、MgO、ZnO中的多种纳米颗粒混合物制成,纳米颗粒的粒径在1nm-500nm范围.
本发明进一步设置为:所述荧光材镀层采用如式(1)所示卟吩系列的荧光染料分子:包括有金属离子M以及侧链基R,其中金属离子M为Zn、Cu、Cd、Fe、Pt、Pd、Ru中的一种,其中共轭侧链基R相同或不同,染料分子浓度控制在0.1μg-10g/L。
本发明进一步设置为:所述侧链基R还包括有相同或不同R1、R2、R3、R4,通过调节侧链基R获得拓展的π-共轭体系,获得发射波长570-780nm的稳定的荧光信号。
本发明进一步设置为:黑色镀层采用黑色石墨、碳粉、黑色金屈纳米颗粒中的一种或多种制成,黑色颗粒浓度控制在1-100g/L。
本发明还公开了一种传感膜的使用方法,通过光电二极管对荧光染料分子激发产生的红光进行采集,并将光信号转换成电信号,经过算法处理后获得氧气浓度。
为达到上述目的,本发明的技术方案如下:一种传感膜的使用方法,包括以下步骤:
S1、用红光作为参比光源,用绿光或蓝光作为激发光源,辐照传感膜的透明支撑层,利用荧光淬灭原理,通过氧气分子与荧光染料分子的相互作用,产生激发红光;
S2、经光电二极管检测采集,将光信号转换为电信号,通过处理模块对数据进行非线性算法拟合处理,获得氧气浓度的变化。
综上所述,本发明具有以下效果:
1、选用一种或多种上述荧光染料分子组合制造的荧光传感膜,可以获得荧光寿命为1nS-200uS的荧光淬灭时间,荧光寿命可调。
2、选用一种或多种上述荧光染料分子组合制造的荧光传感膜,可以获得稳定性高,响应时间快,如T90(达到最终读数的90%所用时间)可根据需要调节从1uS到60S。
附图说明
为了更清楚地说明本发明实施例中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍。
图1为传感膜的结构示意图;
图2为传感膜的检测原理示意图;
图3为传感膜使用流程示意图。
图中:1、传感膜;11、透明支撑基材层;12、荧光材料镀层;13、散射光镀层;14、黑色镀层;15、反光层;2、参比光源;3、激发光源;4、光电二极管;5、处理模块。
具体实施方式
下面结合附图对本发明作进一步详细的说明。
如图1所示,一种基于荧光法检测氧气的复合传感膜,传感膜包括有透明支撑基材层,所述透明支撑基材层表面结合有荧光材料镀层,所述荧光材料镀层表面结合有散射光镀层,所述散射光镀层表面结合有黑色镀层,所述散射光镀层与所述黑色镀层之间设置有反光层。
本方案中,反光层采用Ag或Pt或Pd金屈材料制成,所述反光层的厚度在0.0-100μm,通过调节光电二极管检测到的荧光信号不出现过饱和现象为宜。
本方案中,所述透明支撑基材层采用玻璃或塑料材质制成。
本方案中,所述散射光镀层采用钛白粉(TiO2)、SiO2、六方氮化硼、ZrO2、TiO2、MgF2、Al2O3、MgO、ZnO中的多种纳米颗粒混合物制成,其中纳米颗粒的粒径在1nm-500nm范围,其中配方一:SiO2、ZrO2、TiO2颗粒物总浓度控制但不仅限于在0.1mg-5g/L;配方二:MgF2、Al2O3、MgO、ZnO纳米颗粒浓度控制但不仅限于在1-100g/L之间。
本方案中,黑色镀层采用黑色石墨、碳粉、黑色金屈纳米颗粒中的一种或多种制成,黑色颗粒浓度控制在1-100g/L,黑色镀层可以有效防止外部光透过使得荧光材料镀层寿命的衰减以及荧光材料镀层内荧光信号的干扰影响检测灵敏度和稳定性。
本方案中,所述荧光材镀层采用如式(1)所示卟吩系列的荧光染料分子:
进一步的,所述侧链基R还包括有相同或不同R1、R2、R3、R4,通过调节侧链基R获得拓展的π-共轭体系,获得发射波长570-780nm的稳定的荧光信号,根据不同的侧链基R形成有以下产物:
如图2和图3所示,一种传感膜的使用方法,包括以下步骤:
S1、用红光作为参比光源,用绿光或蓝光作为激发光源的辐照传感膜的透明支撑层,利用荧光淬灭原理,通过氧气分子与荧光染料分子的相互作用,产生激发红光;
S2、经光电二极管检测采集,将光信号转换为电信号,通过处理模块对数据进行非线性算法拟合处理,获得氧气浓度的变化。
水中溶解氧的氧气含量根据亨利定律取决于水中氧分压;在一定浓度的氧气存在条件下,荧光染料分子受激后荧光淬灭效应可以根据Stern-Volmer方程计算对应产生荧光淬灭效应的氧气浓度(或氧分压):
其中:I0和I分别表示无氧和有氧条件下荧光光强;τ0和τ分别表示无氧和有氧条件下荧光寿命;kq表示荧光分子反应速率常数;Ksv表示荧光淬灭反应常数;p02表示被测氧分压或对应的氧分子浓度。
应当指出,对于本领域的普通技术人员来说,在不脱离本发明创造构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。
Claims (9)
1.一种基于荧光法检测氧气的复合传感膜,其特征在于,包括有透明支撑基材层,所述透明支撑基材层表面结合有荧光材料镀层,所述荧光材料镀层表面结合有散射光镀层,所述散射光镀层表面结合有黑色镀层。
2.根据权利要求1所述的一种基于荧光法检测氧气的复合传感膜,其特征在于,所述散射光镀层与所述黑色镀层之间设置有反光层。
3.根据权利要求2所述的一种基于荧光法检测氧气的复合传感膜,其特征在于,反光层采用Ag或Pt或Pd金屈材料制成,所述反光层的厚度在0.0-100μm。
4.根据权利要求1所述的一种基于荧光法检测氧气的复合传感膜,其特征在于,所述透明支撑基材层采用玻璃或塑料材质制成。
5.根据权利要求1所述的一种基于荧光法检测氧气的复合传感膜,其特征在于,所述散射光镀层采用钛白粉(TiO2)、SiO2、六方氮化硼、ZrO2、TiO2、MgF2、Al2O3、MgO、ZnO中的多种纳米颗粒混合物制成,纳米颗粒的粒径在1nm-500nm范围。
7.根据权利要求6所述的一种基于荧光法检测氧气的复合传感膜,其特征在于,所述侧链基R还包括有相同或不同R1、R2、R3、R4,通过调节侧链基R获得拓展的π-共轭体系,获得发射波长570-780nm的稳定的荧光信号。
8.根据权利要求1所述的一种基于荧光法检测氧气的复合传感膜,其特征在于,黑色镀层采用黑色石墨、碳粉、黑色金屈纳米颗粒中的一种或多种制成,黑色颗粒浓度控制在1-100g/L。
9.一种如权利要求1至8任一所述传感膜的使用方法,其特征在于,包括以下步骤:
S1、用红光作为参比光源,用绿光或蓝光作为激发光源,辐照传感膜的透明支撑层,利用荧光淬灭原理,通过氧气分子与荧光染料分子的相互作用,产生激发红光;
S2、经光电二极管检测采集,将光信号转换为电信号,通过处理模块对数据进行非线性算法拟合处理,获得氧气浓度的变化。
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