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Preparation and Properties of Self-healing Luminescent Polyurethane Elastomer
| Updated：2023-02-10
|
Preparation and Properties of Self-healing Luminescent Polyurethane Elastomer Enhanced Publication
- Chinese Journal of Luminescence Vol.null, Issue null, (2023)
- Affiliations：School of Chemical Engineering and Technology， State Key Laboratory of Chemical Engineering， Tianjin University,Tianjin,P.R.China,300350;Hebei Research Center for Geoanalysis， Hebei Key Laboratory of Mineral Resources and Ecological Environment Monitoring,Baoding,P.R.China,071051;Science and Technology on Combustion and Explosion Laboratory， Xi’an Modern Chemistry Research Institute,Xi’an,P.R.China,710065
- Author bio：
- Funds：National Natural Science Foundation of China(21875157);Equipment Preliminary Research Key Laboratory Foundation(6142603190303);the open foundation of State Key Laboratory of Chemical Engineering(SKL-ChE-20B04)
- DOI：10.37188/CJL.20230005 CLC： O482.31
-
Published Online：09 February 2023，
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Cite this article
李子欣,黄汉军,You Somary等.自愈合发光聚氨酯弹性体的制备与性能研究[J].发光学报,
LI Zi-xin,HUANG Han-jun,YOU Somary,et al.Preparation and Properties of Self-healing Luminescent Polyurethane Elastomer[J].Chinese Journal of Luminescence,
李子欣,黄汉军,You Somary等.自愈合发光聚氨酯弹性体的制备与性能研究[J].发光学报, DOI：10.37188/CJL.20230005
LI Zi-xin,HUANG Han-jun,YOU Somary,et al.Preparation and Properties of Self-healing Luminescent Polyurethane Elastomer[J].Chinese Journal of Luminescence, DOI：10.37188/CJL.20230005
Preparation and Properties of Self-healing Luminescent Polyurethane Elastomer Enhanced Publication
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"data": "聚氨酯材料具有优异的力学性能，而发光自愈合聚氨酯在裂缝自诊断和修复等领域具有广阔的应用前景。本文将双（2-羟乙基）二硫化物（HEDS）和1-（4-羟基苯基）-1，2，2-三苯乙烯（TPE-OH）通过化学键键接到聚氨酯体系中，制备了一种具有光致发光性质的自愈合聚氨酯（PUDS），采用傅里叶红外光谱对其化学结构进行了表征，通过X射线衍射仪、万能拉力试验机、荧光分光光度计等方法详细研究了材料的聚集态结构、力学性质、自愈合性能以及光致发光性质。实验结果表明，PUDS具有优异的光致发光性质，其自愈合性能及力学性能与动态二硫键及硬段含量有关。随着动态二硫键含量的增加，材料的自愈合性能逐渐增强，但力学性能逐渐减弱；随着硬段含量的增加，其自愈合性能逐渐减弱，但力学性能逐渐增强。因此，PUDS的力学性能和自愈合性能可通过改变动态二硫键及硬段的含量来调节。在工作中，动态二硫键含量为6.9%（wt%）时，样品具有最佳的自愈合性能、力学性能以及光致发光性质。"
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}
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"data": [
{
"name": "text",
"data": "Polyurethane materials have excellent mechanical properties， and luminescent self-healing polyurethanes have promising applications in areas such as crack self-diagnosis and repair.In this paper， a self-healing polyurethane （PUDS） with photoluminescent property was prepared by bonding bis（2-hydroxyethyl） disulfide （HEDS） and 1-（4-hydroxyphenyl）-1，2，2-tristyrene （TPE-OH） to a polyurethane system through chemical bonding， and its chemical structure was characterized by Fourier infrared spectroscopy.The aggregated structure， mechanical properties， self-healing properties and photoluminescence properties of PUDS were investigated in detail by X-ray diffraction， universal tensile tester， fluorescence spectrophotometer and other methods.The experimental results show that PUDS has excellent photoluminescence property， and its self-healing property and mechanical property are related to the dynamic disulfide bonding and hard segment content.With the increase of dynamic disulfide bonding， the self-healing property of materials gradually increases， but the mechanical property gradually decreases； with the increase of hard segment content， the self-healing property gradually decreases， but the mechanical property gradually increases.Therefore， the mechanical property and self-healing property of PUDS can be adjusted by changing the content of dynamic disulfide bonding and hard segment.In the work， the best self-healing property， mechanical property and photoluminescence property of the samples were obtained at 6.9% （wt%） of dynamic disulfide bonding."
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"keyword": [
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"data": [
[
{
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}
],
[
{
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"data": "四苯基乙烯"
}
],
[
{
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"data": "聚氨酯"
}
],
[
{
"name": "text",
"data": "自愈合"
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[
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}
]
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},
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"data": [
[
{
"name": "text",
"data": "aggregation induced emission"
}
],
[
{
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"data": "tetraphenylethylene"
}
],
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{
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"data": "polyurethane"
}
],
[
{
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"data": "self-healing"
}
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[
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"name": "text",
"data": "photoluminescenc"
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"data": "近年来，聚氨酯（polyurethane，PU）材料发展迅速，因具有优异的力学性能、耐老化性能以及制备简单等优点，聚氨酯被广泛应用于建筑、汽车、生物医学和纺织等领域"
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"data": "。聚氨酯材料的种类有很多，例如：聚氨酯泡沫、聚氨酯弹性体、聚氨酯纤维复合材料、聚氨酯涂料和粘合剂等"
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{
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"data": "。其中，热塑性聚氨酯弹性体具有优异的拉伸性能和弹性恢复性能。因此许多研究人员利用碳纳米管"
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"data": "、MXene"
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"data": "["
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"data": "等修饰静电纺丝热塑性聚氨酯，制备了多种可穿戴式柔性应变传感器。此外，热塑性聚氨酯因其高载药量的特性而被应用于3D打印高药物含量的剂型"
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"data": "["
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]
},
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"data": "。"
}
]
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"name": "text",
"data": "聚氨酯虽然是一种机械性能十分优异的聚合物材料，但是像其他材料一样，在日常生活的使用中也会发生损坏而出现裂痕。因此，自愈合材料在近年来得到了广泛研究。当前聚氨酯实现自愈合的策略主要是利用动态键可逆重排作用实现自愈合，主要分为两种：（1）动态共价反应；（2）超分子相互作用"
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"data": [
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},
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"data": "。动态共价反应中包括动态金属配位键"
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"data": "、动态硼-氮（B-N）配位键"
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"data": {
"data": [
{
"name": "xref",
"data": {
"text": "14",
"type": "bibr",
"rid": "R14",
"data": [
{
"name": "text",
"data": "14"
}
]
}
},
{
"name": "text",
"data": "-"
},
{
"name": "xref",
"data": {
"text": "17",
"type": "bibr",
"rid": "R17",
"data": [
{
"name": "text",
"data": "17"
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]
}
}
],
"rid": [
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"type": "bibr"
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "等。其中，动态二硫键因其中等温和的反应温度而被广泛使用。Dong"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "18",
"type": "bibr",
"rid": "R18",
"data": [
{
"name": "text",
"data": "18"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "等人将动态二硫键嵌入在聚氨酯的硬链段中，锁定在粘弹性硬微相区域，该锁相设计在中等温度下表现出优异的机械性能和有效的愈合性。Tang"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "19",
"type": "bibr",
"rid": "R19",
"data": [
{
"name": "text",
"data": "19"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "等人利用动态二硫键设计了一种热触发自愈合聚氨酯，以同时提高无机材料CsPbIBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": " PSCs的效率和稳定性，高温下动态二硫键可修复钙钛矿薄膜中的缺陷。Park"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "20",
"type": "bibr",
"rid": "R20",
"data": [
{
"name": "text",
"data": "20"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "等人利用芳香族二硫化物制备了一种透明且易于加工的热塑性聚氨酯，其拉伸强度和韧性可达6.8 MPa 和26.9 MJ·m"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-3"
}
]
},
{
"name": "text",
"data": "，并且芳香族二硫化物为其提供了优秀的室温自愈合性能。"
}
]
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "传统聚氨酯材料在出现细小的裂纹时很难被发现，在某些情况下，未能及时发现并修复裂纹将造成巨大的损失。因此，裂纹的定位和诊断是一项很重要的内容"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "21",
"type": "bibr",
"rid": "R21",
"data": [
{
"name": "text",
"data": "21"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。聚氨酯凭借其特有的微相分离结构很容易被化学修饰，因此科研人员们对此进行了许多工作，例如将一些稀土配合物"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "blockXref",
"data": {
"data": [
{
"name": "xref",
"data": {
"text": "22",
"type": "bibr",
"rid": "R22",
"data": [
{
"name": "text",
"data": "22"
}
]
}
},
{
"name": "text",
"data": "-"
},
{
"name": "xref",
"data": {
"text": "25",
"type": "bibr",
"rid": "R25",
"data": [
{
"name": "text",
"data": "25"
}
]
}
}
],
"rid": [
"R22",
"R23",
"R24",
"R25"
],
"text": "22-25",
"type": "bibr"
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "、荧光染料"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "blockXref",
"data": {
"data": [
{
"name": "xref",
"data": {
"text": "26",
"type": "bibr",
"rid": "R26",
"data": [
{
"name": "text",
"data": "26"
}
]
}
},
{
"name": "text",
"data": "-"
},
{
"name": "xref",
"data": {
"text": "31",
"type": "bibr",
"rid": "R31",
"data": [
{
"name": "text",
"data": "31"
}
]
}
}
],
"rid": [
"R26",
"R27",
"R28",
"R29",
"R30",
"R31"
],
"text": "26-31",
"type": "bibr"
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "分子引入聚氨酯中以制备各种光致发光聚氨酯。传统的发光材料处于固态时会发生聚集导致猝灭效应（aggregation caused quenching, ACQ），这使其在实际应用中受到了很大的限制。2001年，唐本忠"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "32",
"type": "bibr",
"rid": "R32",
"data": [
{
"name": "text",
"data": "32"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "课题组发现了聚集诱导发光（aggregation induced emission, AIE）现象，为固态发光材料的制备提供了新的思路"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "blockXref",
"data": {
"data": [
{
"name": "xref",
"data": {
"text": "33",
"type": "bibr",
"rid": "R33",
"data": [
{
"name": "text",
"data": "33"
}
]
}
},
{
"name": "text",
"data": "-"
},
{
"name": "xref",
"data": {
"text": "34",
"type": "bibr",
"rid": "R34",
"data": [
{
"name": "text",
"data": "34"
}
]
}
}
],
"rid": [
"R33",
"R34"
],
"text": "33-34",
"type": "bibr"
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。其中，四苯基乙烯（tetraphenylethylene，TPE）"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "blockXref",
"data": {
"data": [
{
"name": "xref",
"data": {
"text": "35",
"type": "bibr",
"rid": "R35",
"data": [
{
"name": "text",
"data": "35"
}
]
}
},
{
"name": "text",
"data": "-"
},
{
"name": "xref",
"data": {
"text": "36",
"type": "bibr",
"rid": "R36",
"data": [
{
"name": "text",
"data": "36"
}
]
}
}
],
"rid": [
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"R36"
],
"text": "35-36",
"type": "bibr"
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "具有高固体发光效率、高产率和易于功能化的优点，是典型的AIE材料之一，被广泛应用于发光液晶、有机发光二极管、离子识别和传感等领域。"
}
]
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "考虑到聚氨酯材料在自愈合、裂纹定位可视化等方面的需求，结合TPE分子的AIE特性，本文将二硫键和TPE嵌入在聚氨酯的硬段部分，制备了一种具有光致发光性质的自愈合聚氨酯弹性体材料。二硫键为聚氨酯提供了自愈合性能，TPE使该体系具有光致发光的性质。通过广角X射线衍射研究了其聚集态结构，通过拉伸实验对其力学性能以及自愈合性能进行了表征，通过荧光分光光度计对其光致发光性质进行了表征。实验结果表明：二硫键含量为6.9%的PUDS样品具有最佳的力学性能、自愈合性能以及光致发光性能。"
}
]
}
]
},
{
"name": "sec",
"data": [
{
"name": "sectitle",
"data": {
"title": [
{
"name": "text",
"data": "2 实 验"
}
],
"level": "1",
"id": "s2"
}
},
{
"name": "sec",
"data": [
{
"name": "sectitle",
"data": {
"title": [
{
"name": "text",
"data": "2.1 材料"
}
],
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"id": "s2a"
}
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "聚四亚甲基醚二醇（PTMG，Mn=1000 g/mol），天津希恩思奥普德科技有限公司；4,4'-二环己基甲烷二异氰酸酯（HMDI），>90.0%（GC），上海阿拉丁生化科技股份有限公司；二月桂酸二丁基锡（DBTDL），98%，安徽泽升科技有限公司；双（2-羟乙基）二硫化物，≥90%，上海阿拉丁生化科技股份有限公司；1,4-丁二醇（BDO），99%，天津希恩思奥普德科技有限公司；1-（4-羟基苯基）-1,2,2-三苯乙烯，>98%（GC），上海麦克林生化科技有限公司；N,N-二甲基甲酰胺（DMF），99.9%，超干，含分子筛，Water≤30ppm，安徽泽升科技有限公司。"
}
]
}
]
},
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"name": "sectitle",
"data": {
"title": [
{
"name": "text",
"data": "2.2 分析测试仪器"
}
],
"level": "2",
"id": "s2b"
}
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "采用美国Nicolet 6700傅立叶变换红外光谱仪分析样品所含的特征官能团，采用衰减全反射方法，扫描波数范围为4000~650 cm"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-1"
}
]
},
{
"name": "text",
"data": "；使用日本理学SmartLab（9KW）型X射线衍射仪（XRD）分析样品的聚集态结构，扫描范围为10~40°；通过德国布鲁克Bruker Dimension icon原子力显微镜（AFM）研究了样品的表面形貌特征，扫描范围为5 μm，扫描频率为0.25 Hz；使用瑞士梅特勒-托利多TGA/DSC1同步热分析仪测试了样品的热稳定性；使用美国TA Q800动态热机械分析仪（DMA）研究了样品的动态力学性能；通过WDW-05L型电子万能试验机测试每个样品的力学性能和自愈合性能；采用日立F-2500荧光分光光度计分析了样品的荧光发射性质；使用日本岛津UV-1800紫外可见分光光度计测定了样品的光学透过率。"
}
]
}
]
},
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"name": "sec",
"data": [
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"name": "sectitle",
"data": {
"title": [
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"name": "text",
"data": "2.3 合成方法"
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],
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},
{
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"data": [
{
"name": "text",
"data": "以PUDS-3为例详细介绍合成步骤。首先称取4.00 g PTMG和一滴DBTDL于三口圆底烧瓶中，于120 ℃下真空干燥2 h以除去水分。干燥完毕后向体系中充满氮气，将温度降至80 ℃，通过注射器加入3.15 g HMDI，恒温反应3 h。预聚反应完成后，将温度降至65 ℃，先向反应体系加入30 ml无水DMF，然后用10 ml无水DMF溶解0.62 g HEDS，加入到反应体系中，恒温反应2 h。扩链反应完成后，用5 ml无水DMF溶解0.02 g TPE-OH，加入到反应体系中，恒温反应2 h。反应完毕后，将混合溶液倒入硅胶模具中，放入烘箱，40 ℃加热12 h，再升温至50 ℃加热12 h，最后升温至60 ℃加热12 h以挥干溶剂。最后得到无色透明的聚氨酯弹性体薄膜，命名为PUDS-3。合成路线如"
},
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"data": {
"text": "图1",
"type": "fig",
"rid": "F1",
"data": [
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"data": "图1"
}
]
}
},
{
"name": "text",
"data": "所示。其他样品也可通过相同的方法制得。为了作对照，空白组样品用BDO代替HEDS作为扩链剂加入到聚氨酯体系中，命名为PUDS-0。四种PUDS样品的单体组成见"
},
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"data": {
"text": "表1",
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"data": [
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"name": "text",
"data": "表1"
}
]
}
},
{
"name": "text",
"data": "。PUDS样品的二硫键含量计算公式如下："
}
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"data": "Fig.1"
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"data": "Synthetic routes of PUDS"
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"data": [
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"data": "我们进行了红外光谱实验来确认聚合物的生成，PUDS-0到PUDS-7的红外光谱如"
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"data": "所示。对应于HMDI单体的2260 cm"
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]
},
{
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"data": "处的N=C=O的伸缩振动峰消失，与此同时在3320 cm"
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{
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"data": [
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]
},
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"name": "text",
"data": "和1699 cm"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-1"
}
]
},
{
"name": "text",
"data": "处出现了对应于氨基甲酸酯键的N-H和C=O的伸缩振动峰，异氰酸酯键的消失以及氨基甲酸酯键的出现证明了PUDS聚合物的成功合成。此外，PUDS系列聚合物中均出现了对应于亚甲基2922 cm"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-1"
}
]
},
{
"name": "text",
"data": "和2856 cm"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-1"
}
]
},
{
"name": "text",
"data": " 的反对称伸缩振动峰和醚键1097 cm"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-1"
}
]
},
{
"name": "text",
"data": "的伸缩振动峰的，证明了PUDS中聚醚软段的成功引入。"
}
]
},
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"label": [
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"data": "图2"
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"title": [
{
"name": "text",
"data": "PUDS的红外光谱图"
}
]
},
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"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.2"
}
],
"title": [
{
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"data": "FTIR spectra of PUDS"
}
]
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"data": "3.2 PUDS的聚集态结构"
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"data": [
{
"name": "text",
"data": "红外光谱证实了聚合物的生成，之后我们通过广角X射线衍射（WAXD）进一步研究了PUDS的微观结构。如"
},
{
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"data": {
"text": "图3",
"type": "fig",
"rid": "F3",
"data": [
{
"name": "text",
"data": "图3"
}
]
}
},
{
"name": "text",
"data": "所示，PUDS-0到PUDS-7均只在2θ = 19°的位置有一个对应于非晶态聚合物的短程有序的衍射峰。不含动态二硫键的PUDS-0衍射峰的强度最高，二硫键含量的增加使得PUDS的分子量增加，分子链之间的缠结导致PUDS聚合物的非晶区的扩大，从而衍射峰强度逐渐减小。当HEDS扩链剂的含量达到最高的6.9wt%时，PUDS-7的衍射峰强度最低，峰形明显趋于平缓，证实二硫键的引入能有效改变PUDS体系中分子链的聚集状况。"
}
]
},
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"lang": "zh",
"label": [
{
"name": "text",
"data": "图3"
}
],
"title": [
{
"name": "text",
"data": "PUDS的X射线衍射图"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.3"
}
],
"title": [
{
"name": "text",
"data": "X-ray diffraction pattern of PUDS"
}
]
}
],
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"data": "聚氨酯具有典型的微相分离结构。为了进一步分析PUDS的微相分离结构，我们通过原子力显微镜观察了其表面形貌。如"
},
{
"name": "xref",
"data": {
"text": "图4",
"type": "fig",
"rid": "F4",
"data": [
{
"name": "text",
"data": "图4"
}
]
}
},
{
"name": "text",
"data": "所示，亮区和暗区是不相容的。亮区和暗区分别代表硬段相和软段相，亮区呈弥散分布状，暗区呈连续分布状。从图中不难看出，PUDS-0的亮区明显少于PUDS-3、PUDS-5和PUDS-7，这是因为二硫键的引入使得硬链段的活动能力加强，从而使得硬段分布更加均匀，亮区增加。两相结构对PUDS材料的力学性能具有至关重要的影响：软段相含量增加可以提高材料的断裂伸长率和韧性；硬段相含量增加可以提高材料的断裂强度和刚性。"
}
]
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"label": [
{
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"data": "图4"
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"title": [
{
"name": "text",
"data": "PUDS的AFM表面形貌图"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.4"
}
],
"title": [
{
"name": "text",
"data": "AFM surface topography of PUDS"
}
]
}
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"data": [
{
"name": "text",
"data": "热稳定性是聚氨酯样品应用的重要指标之一，因此我们对所有样品进行了热重分析测试。PUDS的TGA曲线如"
},
{
"name": "xref",
"data": {
"text": "图5",
"type": "fig",
"rid": "F5",
"data": [
{
"name": "text",
"data": "图5"
}
]
}
},
{
"name": "text",
"data": "所示，PUDS-0、PUDS-3、PUDS-5、PUDS-7在5%失重时的温度分别为299℃、301℃、294℃、289℃，表明PUDS具有良好的热稳定性。PUDS-0和PUDS-3硬段含量基本一致，不同的是PUDS-3引入了二硫键，但是他们的初始分解温度相差很小，说明二硫键对PUDS的热稳定性影响不大。而PUDS-3、PUDS-5、PUDS-7三组样品，随着硬链段含量的增加，PUDS初始分解温度降低，因此PUDS-7因其硬链段含量最高而最先开始分解。结果表明，聚氨酯弹性体的硬链段比软链段更容易发生热分解。"
}
]
},
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"data": {
"id": "F5",
"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图5"
}
],
"title": [
{
"name": "text",
"data": "PUDS的TGA曲线"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.5"
}
],
"title": [
{
"name": "text",
"data": "TGA curves of PUDS"
}
]
}
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"data": {
"title": [
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"data": "3.4 PUDS的力学性能"
}
],
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{
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"data": [
{
"name": "text",
"data": "我们通过DMA对PUDS的力学性能对温度的敏感性进行了表征，"
},
{
"name": "xref",
"data": {
"text": "图6",
"type": "fig",
"rid": "F6",
"data": [
{
"name": "text",
"data": "图6"
}
]
}
},
{
"name": "text",
"data": "显示了所有PUDS样品的储能模量（E´）和损耗因子（tanδ）随温度的变化。Tanδ曲线的峰值温度就是PUDS聚合物的玻璃化转变温度（Tg），从图中可以得出PUDS-0、PUDS-3、PUDS-5、PUDS-7的Tg分别为38.15 ℃、30.65 ℃、41.63 ℃、57.00 ℃，较低的玻璃化转变温度证明了PUDS可划分为聚氨酯弹性体材料。同时PUDS-3到PUDS-7在玻璃化转变区间内储能模量的变化速率比不含二硫键的PUDS-0快，说明了二硫键的引入能够增加聚合物分子链段的运动能力，使体系的粘弹性在玻璃化转变后出现较大变化。这一结果与WAXD实验相一致，证明了动态二硫键的引入对聚合物体系的微观相行为有着显著影响。"
}
]
},
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"data": {
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"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图6"
}
],
"title": [
{
"name": "text",
"data": "PUDS的DMA曲线"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.6"
}
],
"title": [
{
"name": "text",
"data": "DMA curves of PUDS"
}
]
}
],
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"data": [
{
"name": "text",
"data": "之前的实验结果表明动态二硫键的引入使得PUDS体系的分子链活动能力加强。为了评估PUDS的拉伸力学性能，我们对每组样品进行拉伸测试得到如"
},
{
"name": "xref",
"data": {
"text": "图7",
"type": "fig",
"rid": "F7",
"data": [
{
"name": "text",
"data": "图7"
}
]
}
},
{
"name": "text",
"data": "所示的应力-应变曲线。与PUDS-0相比较，引入动态二硫键的PUDS-3模量较低，断裂伸长率较高达到了381.19%（如"
},
{
"name": "xref",
"data": {
"text": "图7",
"type": "fig",
"rid": "F7",
"data": [
{
"name": "text",
"data": "图7"
}
]
}
},
{
"name": "text",
"data": "插图所示），韧性随着二硫键的增加得到了明显改善。从"
},
{
"name": "xref",
"data": {
"text": "图7",
"type": "fig",
"rid": "F7",
"data": [
{
"name": "text",
"data": "图7"
}
]
}
},
{
"name": "text",
"data": "中我们可以看出PUDS-5和PUDS-7的断裂强度明显高于PUDS-0和PUDS-3，但是韧性稍差，断裂伸长率稍低，这是因为PUDS-5和PUDS-7的硬段含量明显高于PUDS-0和PUDS-3，随着硬段含量的增加，氢键含量逐渐增加，硬段之间的相互作用增强，从而表现为断裂强度增加。其中PUDS-5强度最高，其断裂强度为25.85 MPa。PUDS-5的断裂强度高于PUDS-7，这可归因于硬段含量和二硫键含量的共同作用，且二硫键含量占主导作用。综上所述，PUDS样品的力学性能可以通过改变硬段和二硫键的含量来调节。"
}
]
},
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"data": {
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"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图7"
}
],
"title": [
{
"name": "text",
"data": "PUDS的应力-应变曲线，插图：PUDS-3哑铃样条的拉伸实物图"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.7"
}
],
"title": [
{
"name": "text",
"data": "Stress-strain curves of PUDS.Inset： stretching photo of PUDS-3 dumbbell sample"
}
]
}
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"data": {
"title": [
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"name": "text",
"data": "3.5 PUDS的自愈合性质"
}
],
"level": "2",
"id": "s3e"
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"data": [
{
"name": "text",
"data": "从XRD和力学性能的测试中我们得到PUDS是一类良好的弹性体材料。在实际生产和生活中具有自愈合能力的弹性体材料能显著提高产品的质量和使用寿命，PUDS分子链段的活动性随着动态二硫键的引入有明显提升，因此我们考察了体系的自愈合能力。"
},
{
"name": "xref",
"data": {
"text": "图8",
"type": "fig",
"rid": "F8",
"data": [
{
"name": "text",
"data": "图8"
}
]
}
},
{
"name": "text",
"data": "是PUDS-7的原始、切断和愈合后实物图，我们先将切断的两个PUDS-7样品切片自然接触30秒，然后在90 ℃下静置24 h。可以看到PUDS-7在24 h后基本愈合，没有明显的切割痕迹。之后我们对PUDS-3、PUDS-5、PUDS-7切断后自愈合的样品进行拉伸测试，原始和愈合后的应力-应变曲线如"
},
{
"name": "xref",
"data": {
"text": "图9",
"type": "fig",
"rid": "F9",
"data": [
{
"name": "text",
"data": "图9"
}
]
}
},
{
"name": "text",
"data": "所示。原始PUDS-3和PUDS-5断裂伸长率均能达到275%以上，而自愈合样品的断裂伸长率不到50%，这是因为二硫键含量太低导致自愈合效果太差。而PUDS-7原始和自愈合样品的应力-应变曲线基本一致，力学性能略微超出原始样品，证明了二硫键有效调节了PUDS-7的分子排列，愈合断面消除了内部结构缺陷。综上所述，随着二硫键含量的增加，PUDS的自愈合性能逐渐增强。"
}
]
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"title": [
{
"name": "text",
"data": "PUDS-7的实物图：（a）原始；（b）切断；（c）愈合"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.8"
}
],
"title": [
{
"name": "text",
"data": "Photos of PUDS-7： （a） original； （b） severed； （c） healed"
}
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"data": "PUDS的应力-应变曲线（实线和相应的虚线分别代表原始样品和在90 ℃下愈合24小时后的断裂样品）"
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"data": "Stress-strain curves of PUDS （solid lines and corresponding dashed lines represent the original samples and the fractured samples after healing at 90 ℃ for 24 hours， respectively）"
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"data": "根据"
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"data": "公式2"
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"data": "和"
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"data": {
"text": "图9",
"type": "fig",
"rid": "F9",
"data": [
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"data": "图9"
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"data": "的数据可以计算出PUDS-3、PUDS-5、PUDS-7的自愈合效率，如"
},
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"data": {
"text": "图10",
"type": "fig",
"rid": "F10",
"data": [
{
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"data": "图10"
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"data": "所示。从"
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"text": "图10",
"type": "fig",
"rid": "F10",
"data": [
{
"name": "text",
"data": "图10"
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}
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"data": "可以看出PUDS-3和PUDS-5的自愈合效率极低，基本没有自愈合性能。而PUDS-7的自愈合效率非常高，达到了惊人的106.37%，并且其断裂应力也有21.61 MPa，如此高的机械强度和自愈合效率使其在实际应用中有着巨大的应用潜力。"
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"data": "PUDS的断裂应力（原始和愈合后的样品）和自愈合效率"
}
]
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"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.10"
}
],
"title": [
{
"name": "text",
"data": "Breaking stress （original and healed samples） and self-healing efficiency of PUDS"
}
]
}
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"data": "本文工作中的PUDS样品由惰性的软链段和动态的硬链段组成，其中软链段由PTMG聚醚构成，而硬链段由HMDI、HEDS、TPE-OH组成。由于氨基甲酸酯键的存在，聚氨酯体系中存在大量的氢键，从而形成微相分离结构。动态二硫键的存在使得硬链段具有良好的活动能力。如"
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"text": "图11",
"type": "fig",
"rid": "F11",
"data": [
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"data": "图11"
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}
},
{
"name": "text",
"data": "所示，当该PUDS样品被切断时，硬链段中的氢键和动态二硫键会断开，在Tg以上的温度加热一定时间后，断裂的动态二硫键和氢键会重新排列键合使样品恢复原样。"
}
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"title": [
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"name": "text",
"data": "PUDS的自愈合机理示意图"
}
]
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"label": [
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"name": "text",
"data": "Fig.11"
}
],
"title": [
{
"name": "text",
"data": "Schematic diagram of the self-healing mechanism of PUDS"
}
]
}
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"data": "3.6 PUDS的光致发光性质"
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"data": [
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"name": "text",
"data": "四苯基乙烯（TPE）作为典型的聚集诱导发光基元，在固态具有优秀的光致发光能力。因此我们对PUDS-0、PUDS-3、PUDS-5、PUDS-7的荧光发射行为进行了研究。如"
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"text": "图12",
"type": "fig",
"rid": "F12",
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"data": "图12"
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"data": "所示，PUDS-0、PUDS-3、PUDS-5、PUDS-7的最大发射波长均在465 nm处，相比于TPE单体的荧光发射有所红移。TPE基元在聚合物中被压缩导致平面化、共轭效应有所增加，故而荧光光谱红移。PUDS-0、PUDS-3、PUDS-5、PUDS-7的发光强度与聚氨酯体系的有序程度有关，二硫键含量的增加使体系更加无序，发光强度减弱，而硬段含量的增加使体系趋于有序，发光强度增强。"
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"text": "图12",
"type": "fig",
"rid": "F12",
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"data": "图12"
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{
"name": "text",
"data": "插图展示了PUDS-0、PUDS-3、PUDS-5、PUDS-7在365 nm紫外照射下的发光情况。可以看出四种样品均发出青色荧光，发光强度较强，证明了TPE-OH的引入使PUDS表现出良好的光致发光性质。"
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"title": [
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"data": "PUDS薄膜样品的荧光光谱。插图：PUDS的荧光实物图（a）PUDS-0；（b）PUDS-3；（c）PUDS-5；（d）PUDS-7（在365 nm紫外灯下照射）"
}
]
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"label": [
{
"name": "text",
"data": "Fig.12"
}
],
"title": [
{
"name": "text",
"data": "Fluorescence spectra of PUDS film samples.Inset： fluorescence photos of PUDS （a） PUDS-0， （b） PUDS-3， （c） PUDS-5， （d）PUDS-7 （under 365 nm UV lamp irradiation）"
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"data": [
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"name": "text",
"data": "聚合物的内部裂纹显著影响材料的使用寿命和安全，而内部裂纹往往细小，不易被观察到。在裂纹处由于内应力很大，聚集诱导发光材料往往会出现荧光增强效应，能够有效观察到裂纹的存在。结合PUDS材料中TPE基元和二硫键的存在，我们考察了PUDS-7的裂纹自诊断和划痕自愈合性能。如"
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"data": {
"text": "图13",
"type": "fig",
"rid": "F13",
"data": [
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"name": "text",
"data": "图13"
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{
"name": "text",
"data": "a所示，我们在PUDS-7薄膜上刻出“TJU”字样，在365 nm紫外灯照射下薄膜呈现青色荧光发射，在“TJU”处出现明显的荧光增强。在90 ℃下加热5 h后可以看到“TJU”划痕完全消失（"
},
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"data": {
"text": "图13",
"type": "fig",
"rid": "F13",
"data": [
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"data": "图13"
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},
{
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"data": "b），说明该样品具有良好的自愈合能力。这种裂纹自诊断和自愈合的集成设计开发了一种新颖、简便、低成本的方法来避免裂纹的扩展和积累，并延长聚合物的使用寿命。"
}
]
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"title": [
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"data": "PUDS-7薄膜上的裂纹“TJU”在90 ℃下愈合（a）0 h、（b）5 h后的荧光实物图（365 nm紫外灯下照射）"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.13"
}
],
"title": [
{
"name": "text",
"data": "Fluorescence photos of cracked “TJU” on PUDS-7 film healed at 90 ℃ after （a） 0 h， （b） 5 h （under 365 nm UV lamp irradiation）"
}
]
}
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"data": [
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"data": "PUDS薄膜是无色且高度透明的，PUDS-7的薄膜实物图如"
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"data": {
"text": "图14",
"type": "fig",
"rid": "F14",
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"data": "图14"
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"data": "插图所示。薄膜呈无色透明状，薄膜下的校徽清晰可见。为了定量分析PUDS薄膜的透明度，我们通过紫外-可见分光光度测试得到PUDS薄膜的透射光谱，如"
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"data": "所示。四种PUDS薄膜的透过率无明显差异，均在94%以上。其中，PUDS-7的透过率更是达到了97%以上，该值与石英玻璃的透明度相近，这意味着其在光学器件领域有着巨大的应用潜力。"
}
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"title": [
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"data": "PUDS薄膜的透射光谱（膜厚约0.5 mm）。插图：PUDS-7的透明薄膜实物图"
}
]
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"label": [
{
"name": "text",
"data": "Fig.14"
}
],
"title": [
{
"name": "text",
"data": "Transmission spectra of PUDS films （film thickness： ~0.5 mm）.Inset： transparent film photos of PUDS-7"
}
]
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"data": "4 结 论"
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"data": "综上所述，本工作制备了一种基于TPE和二硫键的透明自愈合发光聚氨酯PUDS，其断裂强度达20.46-25.85 MPa。 同时，动态二硫键为PUDS提供了优异的自愈合能力，PUDS-7在中等温度下的自愈合效率接近100%。由于其无色透明且具有自愈合能力，该类聚氨酯材料在光学镜头、汽车和柔性显示屏的保护膜等领域具有潜在的应用价值。此外，由于引入了具有聚集诱导发光特性的TPE发色团，PUDS具有良好的光致发光性质，其发光强度与聚氨酯体系的有序程度有关，二硫键含量的增加使体系更加无序，发光强度减弱，而硬段含量的增加使体系趋于有序，发光强度增强。因此，该工作为具有裂纹自诊断和自愈合性能的透明聚氨酯弹性体的制备提供了新的设计思路。"
}
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"data": [
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"id": "R1",
"label": "1",
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"data": [
{
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"data": "李子欣,黄汉军,You Somary等.自愈合发光聚氨酯弹性体的制备与性能研究[J].发光学报,DOI:10.37188/CJL.20230005"
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"text": "李子欣,黄汉军,You Somary等.自愈合发光聚氨酯弹性体的制备与性能研究[J].发光学报,DOI:10.37188/CJL.20230005"
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"data": [
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"data": "LI Zi-xin,HUANG Han-jun,YOU Somary,et al.Preparation and Properties of Self-healing Luminescent Polyurethane Elastomer[J].Chinese Journal of Luminescence,DOI:10.37188/CJL.20230005"
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"text": "LI Zi-xin,HUANG Han-jun,YOU Somary,et al.Preparation and Properties of Self-healing Luminescent Polyurethane Elastomer[J].Chinese Journal of Luminescence,DOI:10.37188/CJL.20230005"
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"text": [
{
"name": "text",
"data": "国家自然科学基金（21875157）；装备预研重点实验室基金（6142603190303）；化学工程联合国家重点实验室开放课题（SKL-ChE-20B04）。"
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"text": [
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"data": "Supported by National Natural Science Foundation of China （21875157）； Equipment Preliminary Research Key Laboratory Foundation （6142603190303）； the open foundation of State Key Laboratory of Chemical Engineering （SKL-ChE-20B04）"
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"opub": "2023-02-10"
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"appendix": [],
"type": "research-article",
"ethics": [],
"supplementary": [],
"journalTitle": "发光学报",
"originalSource": []
}
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