CN115368501B - 一种含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料及其器件 - Google Patents
一种含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料及其器件 Download PDFInfo
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Abstract
本发明属于功能材料与化学传感器技术领域,公开了一种含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料及其器件。该材料由5‑13质量份双官能丙烯酸酯、2‑5质量份季铵化丙烯酸酯、3‑8质量份甲基丙烯酸甲酯、2‑5质量份己二酸、0.05~0.25质量份Ti3C2纳米粉体与10‑26质量份甲醇,聚合得到粘度200‑1000mPa.s的聚合物胶体溶液。湿度响应器件在25%~90%RH范围,不同温度时,其湿度的相对误差≤0.57%,相对偏差≤0.16%,响应的线性度R2=0.9991,湿滞≤0.4%,水浸24h质量损失≤0.05%,良好地兼顾了交变温度稳定性、线性度、低湿滞、高精度、高准确度与稳定性。
Description
技术领域
本发明属于功能材料与化学传感器技术领域,具体涉及一种含碳化钛(Ti3C2)纳米颗粒的具有良好温变稳定性的湿敏响应材料及其器件。
背景技术
决定湿度传感器性能的关键是湿敏响应材料。性能先进的湿度响应材料应能兼顾满足湿度传感器对灵敏度、准确度、精密度、抗干扰性、稳定性及可靠性等的综合性能要求。
在CN202111339665.1中,采用壳聚糖、丙烯酰胺、N,N-亚甲基双丙烯酰胺与纳米二硫化钼混合,通过多硫酸钾引发自由基聚合与交联反应,制备高分子/无机复合水凝胶,其对水分子具有较高的吸附性和一定的选择能力。无机纳米材料的高比表面与具有交联结构的聚合物形成复合水凝胶,实现了湿度响应材料对水分子的吸附,并利用石英晶体微天平技术实现该复合水凝胶材料对不同环境中湿度的吸附响应行为,该材料有望应用于对湿度的实时检测。不足是该材料的感湿特性曲线不呈线性,难以通过单一的电化学信号对应出环境中的相对湿度情况,其所具备的性能与高精度湿度响应材料性能的实际需求还存在较大的差距。
在CN202010223240.3中,采用具有大比表面积与优异吸水性的MXene纳米碳化铌片材料,制备了具有响应范围广、速度快等优点的纳米片状MXene碳化铌湿度传感器。获得宽数量级(三个数量级)电阻变化范围。遗憾的是材料的湿度响应线性度欠佳,从其材料湿滞曲线可推测材料湿度响应线性度较差,湿滞为2.5%RH。此外材料在器件表面的结合性欠缺,影响器件的稳定性与可靠性,这制约了所制备器件对实际使用工况的适应性。
在CN201811614121.X中,采用季铵盐类聚合物、电解质盐共同结合形成聚合物网络凝胶,得到具有拉伸效果的柔性湿度传感器。其中的季铵盐类功能基团作为对水分子的响应点,在湿度变化时可有效捕捉变化的水分子,从而对环境湿度变化敏感。但在该工作中不同双网络组成的水凝胶材料,均存在与拟合线性差异大,线性度差或对水分子响应信号变化小等不足。
一般地,在对湿度响应性能(如精确度、响应性及稳定性等)要求不是太高的场景下,通用型的湿度传感器即可具有较好的适用性。与此相对,在涉及到高精准度与稳定性的定量、计量等实际场景与工况时,通用型的湿度响应材料及其器件,则表现出较为明显的局限,如材料线性度、高低湿度数据易出现较大偏差,温度变化时也易表现较大偏差,缺乏必须的稳定性等,难易满足现实工况条件下的湿度实时测量需要。
发明内容
为了克服现有实用技术中存在的不足,本发明的首要目的在于提供一种含碳化钛(Ti3C2)纳米颗粒的具有良好温变稳定性的湿敏响应材料及其器件。
本发明所述的一种含Ti3C2纳米颗粒的具有良好温变稳定性的湿敏响应材料及其器件,其制备过程采用了Ti3C2纳米粉体为原位中心,通过共聚反应制备可以兼顾实现对湿度响应的准确度、精密度、线性度、低湿滞性以及温变稳定性等性能。
本发明的再一目的,在于提供一种含Ti3C2纳米颗粒,具有对温变的良好稳定性的湿敏响应高精度湿度响应元件。
本发明的目的还在于,提供一种含Ti3C2纳米颗粒的具有良好温变适应性的高精度湿度响应元件的应用。
本发明的目的通过下述技术方案实现:
一种含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料,所述的湿敏响应材料,是由5-13质量份双官能丙烯酸酯、2-5质量份季铵化丙烯酸酯、3-8质量份甲基丙烯酸甲酯、2-5质量份己二酸、0.05~0.25质量份Ti3C2纳米粉体与10-26质量份甲醇,通过聚合得到粘度为200-1000mPa.s的聚合物胶体溶液。
所述双官能丙烯酸酯包括丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸羟乙酯、甲基丙烯酸羟丙酯、乙二醇二甲基丙烯酸酯、1,4-丁二醇二甲基丙烯酸酯、甲基丙烯酸烯丙酯和烯丙基缩水甘油醚中的至少一种,更加优选为甲基丙烯酸羟乙酯。
所述季铵化丙烯酸酯包括丙烯酰氧乙基三甲基氯化铵、甲基丙烯酰氧乙基三甲基氯化铵、丙烯酰氧乙基三甲基溴化铵、甲基丙烯酰氧乙基三甲基溴化铵、(3-丙烯酰胺丙基)三甲基氯化铵、(3-丙烯酰胺丙基)三甲基溴化铵、环氧丙基三甲基氯化铵、环氧丙基三甲基溴化铵、烯丙基三甲基氯化铵和烯丙基三甲基溴化铵中的至少一种,更加优选为甲基丙烯酰氧乙基三甲基氯化铵。
所述的Ti3C2纳米粉体为二维结构材料。
一种由上述湿敏响应材料制成的具有对温变良好稳定性的湿度响应器件,该器件是采用25%wt浓度的含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料,经超声分散并剥离Ti3C2粉体5-20min,对叉指电极表面进行浸渍涂覆,经热固化干燥后,得到的叉指湿敏响应器件。
所述超声分散并剥离Ti3C2粉体的时间优选为10min。
该器件在25~90%RH及20-40℃温度范围,其湿度的相对误差(δ)≤0.57%,相对偏差(Re)≤0.16%,响应的线性度R2=0.9991,湿滞≤0.4%,水浸24h质量损失≤0.05%。
上述具有良好温变稳定性的湿敏响应材料或上述具有对温变良好稳定性的湿度响应器件在湿度传感器技术领域中的应用。
相对于现有技术,本发明一种含Ti3C2纳米颗粒的具有良好温变稳定性的湿敏响应材料及其器件,具有如下的优点及有益效果:
(1)Ti3C2二维纳米颗粒的引入,使所制备的湿敏响应复合材料及器件,具有更为稳定的电性能,所制备的湿敏响应叉指器件,在30天的不定期累计监测中表现出优良的稳定性。
(2)在103-109Ω电阻范围,所制备的湿敏响应复合材料及器件,表现出较高的灵敏度。在25~90%RH的湿度范围,所制备的湿敏响应器件,其电阻对数值与相对湿度具有良好的线性关系R2=0.9991,湿滞+0.4%,材料偏移小,器件精度高,与湿度表数值对应性好。
(3)所制备的湿敏响应器件具有较优的温变稳定性,在温变20-40℃范围内湿度飘移量<0.4%RH/℃,湿度相对误差(δ)≤0.57%,相对偏差(Re)≤0.16%,水浸24h质量损失≤0.05%。
附图说明
图1为本发明含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料的微观形貌照片。
图2为本发明湿敏响应器件的湿度特性响应图。
图3为本发明湿敏响应器件的湿度特性响应线性拟合图。
图4为本发明含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料所制备的湿度传感器,经30天监测,器件稳定性测试图。
图5为本发明含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料所制备的湿度传感器,在不同温度下,器件温漂测试图。
图6为本发明不同方案的感湿特性曲线图。
图7为含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料,存放30天后与新合成树脂形态的对比。
具体实施方式
下面结合实施例及附图对本发明作进一步详细的描述,但本发明的实施方式不限于此。
实施例1
(1)将5质量份甲基丙烯酸羟乙酯、2质量份甲基丙烯酰氧乙基三甲基氯化铵、3质量份甲基丙烯酸甲酯、2质量份己二酸、0.05质量份Ti3C2纳米粉体与10质量份甲醇,依次加入反应器,于83℃恒温反应4小时,聚合而得的粘度700mPa.s的聚合物复合树脂溶液,即为含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料。
(2)将上述所制备的含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料稀释至25%wt,经超声分散并剥离Ti3C2粉体约10min,在叉指器件表面进行涂布,经热固化干燥后,即为湿度传感器用湿敏响应器件,材料表面形态如图1所示。
(3)对所制备湿敏响应器件试样进行测试,获得实测湿敏数据,获得实测的性能数据如图2所示。
(4)通过该方案所得湿敏响应器件对湿度响应具有良好的线性响应特征。R2=0.9991,其线性拟合情况如图3所示。
(5)对所制备湿敏响应器件试样进行稳定性测试,该器件在30天监测中具有良好的稳定性,如图4所示。
(6)对所制备湿敏响应器件试样进行温度稳定性测试,该器件在温度变化下,具有良好的稳定性及线性关系,如图5所示。
(7)对所制备湿敏响应材料放置30天观察,其黏度也维持在700mPa.s数量级,树脂形态及颜色无明显变化,未出现氧化变色,如图7所示。
本实施例1所制备湿敏响应器件与对比湿敏响应器件实测数据对比见下表1。
所述的对比湿敏响应器件为市场采购的主流湿度传感器用叉指器件,按照同等条件进行测试。
表1实施例1所制备湿敏响应器件与对比湿敏响应器件实测温度数据对比表
可见本材料制备湿敏响应器件相比市场主流湿度传感器用叉指器件具有更好的热稳定性。制备树脂湿度测量值较主流湿敏响应器件(对比样)具有更高精度的湿度表达情况,更加贴近实际相对湿度值。
实施例2~4及对比例1
实施例2~4及对比例1采用的制备方法与实施例1的基本相似,唯一不同的是采用了不同的原料配比。为方便不同实施例以及与对比例间的对比,以下将实施例1-4及对比例1的湿敏响应测试数据统一列于表2中。
表2实施例1-4及对比例1的湿敏响应测试数据
表2中①所示为不同实施例具体原料配比,②为不同实施例所对应反应温度及时间,③为不同实施例所得树脂黏度值,④为不同实施例所得湿敏元件的各项性能值。
上述各实例感湿特性曲线如图6所示。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (7)
1.一种含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料,其特征在于:所述的湿敏响应材料,是由5-13质量份双官能丙烯酸酯、2-5质量份季铵化丙烯酸酯、3-8质量份甲基丙烯酸甲酯、2-5质量份己二酸、0.05~0.25质量份Ti3C2纳米粉体与10-26质量份甲醇,通过聚合得到粘度为200-1000mPa.s的聚合物胶体溶液;
所述双官能丙烯酸酯包括丙烯酸羟乙酯、甲基丙烯酸羟乙酯、甲基丙烯酸羟丙酯和烯丙基缩水甘油醚中的至少一种;
所述季铵化丙烯酸酯包括丙烯酰氧乙基三甲基氯化铵、甲基丙烯酰氧乙基三甲基氯化铵、丙烯酰氧乙基三甲基溴化铵和甲基丙烯酰氧乙基三甲基溴化铵中的至少一种。
2.根据权利要求1所述的一种含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料,其特征在于:所述双官能丙烯酸酯为甲基丙烯酸羟乙酯;所述季铵化丙烯酸酯为甲基丙烯酰氧乙基三甲基氯化铵。
3.根据权利要求1所述的一种含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料,其特征在于:所述的Ti3C2纳米粉体为二维结构材料。
4.一种由权利要求1所述的材料制成的具有对温变良好稳定性的湿度响应器件,其特征在于:该器件是采用25%wt浓度的含碳化钛纳米颗粒的具有良好温变稳定性的湿敏响应材料,经超声分散并剥离Ti3C2粉体5-20min,对叉指电极表面进行浸渍涂覆,经热固化干燥后,得到的叉指湿敏响应器件。
5.根据权利要求4所述的具有对温变良好稳定性的湿度响应器件,其特征在于:所述超声分散并剥离Ti3C2粉体的时间为10min。
6.根据权利要求4所述的具有对温变良好稳定性的湿度响应器件,其特征在于:该器件在25 ~ 90%RH及20-40℃温度范围,其湿度的相对误差≤0.57%,相对偏差≤0.16%,响应的线性度R2=0.9991,湿滞≤0.4%,水浸24h质量损失≤0.05%。
7.根据权利要求1所述的具有良好温变稳定性的湿敏响应材料或权利要求4所述的具有对温变良好稳定性的湿度响应器件在湿度传感器技术领域中的应用。
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