Ag-BiOBr/WO<sub>3</sub>复合材料的制备及强化磺胺异噁唑去除性能

高生旺; 赵星鹏; 陆迦勒; 崔娟; 王国英; 张青

doi:10.13801/j.cnki.fhclxb.20220424.003

Ag-BiOBr/WO₃复合材料的制备及强化磺胺异噁唑去除性能

高生旺^1,,
赵星鹏^{1, 2},
陆迦勒³,
崔娟^{1, 3},
王国英²,
张青^4, ,

1.
中国环境科学研究院　环境基准与风险评估国家重点实验室，北京 100012
2.
太原理工大学　环境科学与工程学院，太原 030024
3.
中北大学　理学院，先进碳基电极材料山西省重点实验室，太原 030051
4.
齐鲁工业大学　山东省科技发展战略研究所，济南 250100

基金项目: 国家重点研发计划项目(2019YFD1100201；2018YFD1100505)；中北大学创新训练项目(185)

详细信息

通讯作者:
张青，博士，高级工程师，硕士生导师，研究方向为污水处理　E-mail: xvhqing@163.com

中图分类号: X52
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出版历程
- 收稿日期: 2022-02-10
- 修回日期: 2022-04-12
- 录用日期: 2022-04-15
- 网络出版日期: 2022-04-24
- 刊出日期: 2023-03-14

Preparation of Ag-BiOBr/WO₃ composites and enhanced sulfisoxazole removal performance

1.
State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Academy of Environmental Sciences, Beijing 100012, China
2.
School of Environmental Science and Engineering, Taiyuan University of Technology, Taiyuan 030024, China
3.
Shanxi Key Laboratory of Advanced Carbon Based Electrode Materials, School of Science, North University of China, Taiyuan 030051, China
4.
Institute of Science and Technology for Development of Shandong, Qilu University of Technology, Jinan 250100, China

Funds: National Key R&D Program Project (2019YFD1100201; 2018YFD1100505); Innovative Training Program of North University of China (185)

摘要

摘要: 抗生素类药物因其抗菌效果好在人畜医疗等领域得到广泛应用，但其在环境中难以自然分解，光催化氧化技术在降解持久型有机物方面有着光明的应用前景。然而，常规的光催化材料光谱吸收范围不够宽、光生载流子复合率过高，严重制约了催化材料的应用推广。因此，亟待研发更有效安全的去除技术。本文利用光沉积法将Ag单质负载于BiOBr/WO₃ p-n型异质结材料表面，构建出新型Ag-BiOBr/WO₃材料，并将其用于光催化降解磺胺异噁唑。采用XRD、TEM、XPS、UV-vis DRS等技术对其进行表征表明，Ag的沉积拓展了材料的光响应范围，显著加快光生载流子的分离速度，从而提高了光催化性能。单质Ag含量为15wt%的材料为降解磺胺异噁唑效率最高的复合材料。当溶液中催化剂浓度为0.3 g/L，磺胺异噁唑浓度为5 mg/L，pH为7时，在60 min时光催化降解磺胺异噁唑的效率最高，可达98.1%，降解速率常数分别为BiOBr、WO₃和BiOBr/WO₃的28.79倍、36.37倍和7.59倍。经过5次循环实验后，15wt%Ag-BiOBr/WO₃复合材料仍具备较高的光催化活性，表明材料可循环回收利用，具备良好的稳定性。淬灭实验和电子自旋共振(ESR)结果表明，•O₂^–为15wt%Ag-BiOBr/WO₃体系中最活跃的自由基团，而¹O₂和h⁺发挥了次要作用。这为催化材料的制备和抗生素降解提供了理论基础。
- 磺胺异噁唑 /
- 光催化技术 /
- 溴氧化铋 /
- 三氧化钨 /
- 银
Abstract: Antibiotics have been widely used to treat human and animal diseases with good antibacterial effect. However, antibiotics are difficult to be degraded naturally in natural environment. The photocatalytic oxidation technology has bright application prospects in the degradation of persistent organic compounds. However, the spectral absorption range of conventional photocatalytic materials is not wide enough, and the recombination rate of photogenerated carriers is too high, which seriously restricts the application and promotion of catalytic materials. So, it is urgent to develop more effective and safe removal technologies. The photodeposition method was used to load Ag element on the surface of BiOBr/WO₃ p-n type heterojunction material to construct a new type of Ag-BiOBr/WO₃ material and apply to the photocatalytic degradation of sulfisoxazole. The samples were characterized by various techniques, such as XRD, TEM, XPS, UV-vis DRS et al. The result show that the deposition of Ag expands the photo-response range of the material, significantly accelerates the separation speed of photogenerated carriers, and thus improves the photocatalytic performance. The 15wt%Ag-BiOBr/WO₃ with an Ag content of 15wt% is considered to be the most efficient composite material for the removal of sulfisoxazole. When the catalyst concentration is 0.3 g/L, the sulfisoxazole concentration is 5 mg/L, and the pH is 7, 15wt%Ag-BiOBr/WO₃ demonstrates the highest photocatalytic degradation efficiency of sulfisoxazole in 60 min, which reaches up to 98.1%. The degradation rate is 28.79, 36.37 and 7.59 times higher than those of BiOBr, WO₃ and BiOBr/WO₃, respectively. After 5 cycles of experiments, the 15wt%Ag-BiOBr/WO₃ composite material still maintains high photocatalytic activity, indicating that the material can be recycled and reuses with good stability. The quenching experiments and electron spin resonance (ESR) shows that •O₂^– is the most active radical group in the BiOBr/WO₃ system, while ¹O₂ and h⁺ played relatively minor roles. This provides a theoretical basis for the preparation of catalytic materials and the degradation of antibiotics.
- sulfisoxazole /
- photocatalytic technology /
- bismuth bromide oxide /
- tungsten trioxide /
- silver

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具有轻质、高强、免锈蚀及抗疲劳性能良好等诸多优点的碳纤维增强聚合物复合材料(Carbon fiber reinforced polymer，CFRP)筋有望成为传统钢制筋材的替代品，特别是对于在恶劣环境下工作的预应力结构^[1-3]。相较于易导致CFRP筋出现“切口效应”而过早发生横向破坏的夹持型锚固系统，粘结型锚固系统通过CFRP筋-粘结介质界面的化学胶着力、摩擦力及机械咬合力可实现对CFRP筋更可靠、有效的锚固^[4-5]。活性粉末混凝土(Reactive powder concrete，RPC)以其优异的力学性能和耐久性能可成为有效锚固CFRP筋的粘结介质^[6]。RPC灌注的CFRP筋粘结型锚固系统已在实际工程中得以成功应用，并表现出优异的锚固性能^[7-8]。然而，CFRP筋及其粘结型锚固系统在建造和运营过程中可能遭受火灾作用^[9-12]。火灾下CFRP筋及CFRP筋-粘结介质界面因树脂基体较弱的耐高温性能而易成为受力薄弱环节，则高温下CFRP筋及其粘结型锚固系统的力学性能值得关注。因此，对CFRP筋及其粘结型锚固系统的高温力学性能进行研究是十分必要的。

国内外部分学者对高温下CFRP筋的力学性能开展了研究。Wang等^[13]试验研究了20~600℃作用下CFRP筋力学性能退化规律，结果表明：高温下CFRP筋应力-应变始终呈线性关系；CFRP筋抗拉强度随处理温度升高而近似线性衰减，并在500℃时完全丧失；处理温度高于350℃时，CFRP筋弹性模量急剧下降。杨桢楠^[14]试验研究了100~500℃作用下CFRP筋的力学性能，结果表明：处理温度大于200℃时，CFRP筋的抗拉强度与弹性模量均大幅下降。周飞^[15]对20~500℃作用下CFRP筋力学性能进行了试验研究，提出了适于表征高温下CFRP筋轴拉性能退化规律的指数函数模型。上述研究所采用CFRP筋的树脂玻璃化转变温度T_g均小于200℃。

另有部分学者对高温下纤维增强塑料(Fiber reinforce plastic，FRP)筋-混凝土界面的粘结性能进行了试验研究。吕西林等^[16]研究了处理温度、混凝土强度与粗骨料粒径等参数对20~250℃作用下玻璃纤维增强聚合物复合材料(Glass fiber reinforced polymer，GFRP)筋-混凝土界面粘结性能的影响规律，结果表明处理温度高于110℃时，界面粘结强度相较于常温下降低了85%~90%。Katz等^[17-18]对20~250℃作用下GFRP筋-混凝土界面粘结性能进行了研究，给出了适于表征界面粘结强度衰减规律的半经验模型，结果表明处理温度为250℃时，界面粘结强度仅为常温时的10%~20%；筋材表面处理方式是影响界面粘结强度的重要因素。王晓璐等^[19]研究了20~350℃作用下FRP (GFRP、玄武岩纤维增强聚合物复合材料(Basalt fiber reinforced polymer，BFRP))筋-混凝土界面的粘结性能，提出了高温下界面粘结强度衰减模型与粘结-滑移本构模型，结果表明处理温度由60℃增至120℃时，界面粘结强度的衰减幅度最大；200℃时界面粘结强度仅为常温时的15%。鞠竹等^[20]对20~190℃作用下GFRP筋-混凝土界面的粘结性能进行了研究，并提出了适用于表征高温下界面粘结-滑移行为的双折线模型。

综上所述，现有研究侧重于高温下具有较低T_g(T_g<200℃) FRP筋材轴拉性能及FRP筋-混凝土界面粘结性能，鲜见关于高温下CFRP筋(T_g>200℃)及其粘结型锚固系统力学性能研究的报道。为此，本文将在方志等^[21]的研究(侧重于研究高温后CFRP筋及其粘结型锚固系统的残余力学性能，是开展火灾后相应评估工作的依据)的基础上，对高温下一种抗火性能优良的CFRP筋(T_g>200℃)及其粘结型锚固系统的静力性能进行试验研究，以揭示处理温度对高温下CFRP筋轴拉性能及其锚固性能的影响规律，提出适于表征高温下CFRP筋轴拉性能及其锚固性能的实用计算公式，为评估CFRP筋及其锚固系统的抗火性能提供依据。本文与前期研究的成果将共同为高性能CFRP筋材的工程应用提供理论基础。

1. 试验概况

1.1 试件设计

参照《纤维增强复合材料筋基本力学性能试验方法》(GB/T 30022—2013)^[22]设计CFRP筋轴拉试件，以筋材处理温度T(分别为25℃、100℃、210℃和300℃)为试验参数，设计4组试件，每组3个试件，共计12个试件。

CFRP筋轴拉试件由长为680 mm的自由段及其两端长为360 mm的粘结型锚固系统组成，总长共计1400 mm，如图1所示。其中，锚固CFRP筋的粘结型锚固系统通过在外径为42 mm、内径为36 mm的钢套筒内灌注RPC形成，筋材周围RPC保护层厚度为12 mm。

选取试验锚的处理温度T (分别为25℃、100℃、210℃、300℃)为锚固性能试验的参数，设计4组试件，每组2个试件，共计8个试件。锚固性能试件的粘结长度l均设置为5d，其中d为CFRP筋的公称直径，d=12 mm。

CFRP筋-RPC锚固性能试件由CFRP筋材自由段及其位于左右两侧的工具锚与试验锚组成，如图2所示。以CFRP筋轴拉试件的粘结型锚固系统作为锚固性能试件的工具锚。为便于测定CFRP筋-RPC界面粘结-滑移性能，锚固性能试件右侧的试验锚通过在外径为76 mm、内径为72 mm的钢套筒内灌注RPC形成。试验锚长度设置为420 mm，以与高温炉炉腔长度380 mm相匹配。为获取试验预设的粘结长度l=5d，试验锚加载端与自由端的CFRP筋外侧均预埋长度为180 mm的耐高温陶瓷套管。利用耐高温胶密封陶瓷套管与CFRP筋间的孔隙，以防止灌注粘结介质时RPC进入陶瓷套管内。此外，利用耐高温胶带将K型热电偶的较少部分金属探头固定于CFRP筋-RPC界面，以实时监测试验过程中粘结界面的温度。

图 1 碳纤维增强聚合物复合材料(CFRP)筋轴拉试件

Figure 1. Axial tensile specimen of carbon fiber reinforced polymer (CFRP) bar

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图 2 CFRP筋-活性粉末混凝土(RPC)锚固性能试件

Figure 2. Anchorage performance specimen of CFRP bar-reactive powder concrete (RPC)

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利用设置在锚筒两端的聚乙烯封盖中心处圆孔精确定位轴拉试件或锚固系统性能试件的CFRP筋。浇筑钢锚筒的粘结介质RPC形成粘结型锚固系统，将其静置24 h后再采用90℃蒸汽养护48 h。

1.2 试验材料

轴拉与锚固性能试验所用的CFRP筋材均由江苏连云港中复碳芯电缆科技有限公司提供，其外观尺寸及T_g如图3和表1所示。CFRP筋由体积含量为66.3vol%的T700SC连续碳纤维丝束与TP224环氧树脂拉挤而成。

CFRP筋粘结型锚固系统的粘结介质-RPC由不含钢纤维的商品预混料加水拌制而成，其设计强度等级为RPC150。边长100 mm的立方体实测抗压强度为158 MPa，RPC配合比(单方质量比)如表2所示。

图 3 CFRP筋及其外观尺寸

Figure 3. CFRP bar and its external dimensions

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表 1 CFRP筋外观尺寸及玻璃化转变温度T_g

Table 1. Dimensions and glass transition temperatureT_g of CFRP bar

Nominal diameter/mm	Rib width/mm	Rib height/mm	Embossing space/mm	T_g/℃
12	9.26	0.27	14.8	210

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表 2 RPC配合比及抗压强度

Table 2. Mix proportion and compressive strength of RPC

Strength grade	Cement	Silica fume	Quartz flour	Quartz sand	Water reducer	Water binder ratio
RPC150	1	0.25	0.25	1.1	0.02	0.16

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1.3 温升加载方式与测点布置

轴拉与锚固性能试验的温升加载及测量装置分别如图4、图5所示。试验中采用的温升加载方式参考金属材料高温拉伸试验方法(GB/T 4338—2006)^[23]，如图6所示。将轴拉试件的筋材自由段或锚固性能试件的试验锚放置于高温试验炉(尺寸为380 mm (长)×410 mm (宽)×650 mm (高)) 中，以3℃/min的温升速率温升至目标温度，恒温一定时间(对于轴拉试件，通常恒温20 min；对于锚固性能试件，恒温至CFRP筋-RPC界面温度达到目标温度)后再进行单调加载。高温炉由长沙科辉炉业科技有限公司提供，其升温区间和最大升温速率分别为100~1200℃和100℃/min。利用设置在CFRP筋表面与CFRP筋-RPC界面的K型热电偶分别监测轴拉与锚固性能试件的实时温度。

图 4 轴拉试验的温升及加载装置

MTS—Mechanical testing and simulation

Figure 4. Setups of elevated temperature and loading of axial tensile test

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图 5 锚固性能试验的温升及加载装置

Figure 5. Setups of elevated temperature and loading of anchorage performance test

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图 6 温升及加载过程

Figure 6. Processes of elevated temperature and loading

T₀—Room temperature; T_a—Target temperature; P_u—Ultimate load; T—Temperature; P—Load; t—Time; t₀—Test start time; t₁—Time to target temperature; t₂—Start load time; t₃—Time to failure

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当试件温度达到目标温度且稳定时，利用600 kN液压伺服试验机(南京诺尔泰设备制造有限公司)以1 mm/min的位移加载速率对试件施加轴向拉力或拉拔力。其中，锚固性能试件的拉拔力需借助固定于液压伺服试验机夹具上的工具锚，对放置在反力架上的试验锚进行施加，如图5所示。为使锚固性能试件始终处于铅直受力状态，在反力架与试验锚之间设置了可转动的开孔球铰。利用液压伺服试验机的力传感器采集试件拉拔力。采用与CFRP筋表面紧密接触的高温引伸计测量轴拉试件筋材自由段中部的应变。锚固性能试件加载端CFRP筋-RPC界面滑移通过固定于CFRP筋上的位移传感器获取。

2. CFRP筋轴拉试验结果及分析

2.1 CFRP筋轴拉试件的破坏形态

高温下各CFRP筋轴拉试件的典型破坏形态均为拉断破坏，破断位置均分布于筋材自由段区域内；随着处理温度逐渐升高，拉断破坏形态由筋材断口破坏与少量丝束分离的片状形态转变为纤维丝“蓬松”的形态，如图7所示。

常温下，试件的轴拉应力超过80%极限抗拉强度后，少量纤维丝破断而发出细小声响；当轴拉应力达到极限抗拉强度时，试件会突然破坏而形成位于自由段中部的断口，并伴随有轻微的炸裂现象。但文中常温试件炸裂程度较轻，且筋材自由段左侧区域因炸裂形成的碳纤维细条未能及时收集而丢失，导致图7中所示常温试件的破坏形态与典型的纤维束爆裂形态(纤维束炸开的扫帚状)存在一定的差别。

图 7 CFRP筋轴拉试件的破坏形态

Figure 7. Typical failure modes of CFRP bar axial tensile specimens

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对于处理温度为100~210℃的轴拉试件，其轴拉应力接近极限抗拉强度时因少量纤维丝破断而发出细小声响。由于树脂性能退化较轻微，少量破断的纤维丝呈丝束分离的片状形态。筋材轴拉应力达到极限抗拉强度后突然发生伴有清脆响声的破断，其断口位置靠近筋材自由段中间区域。

对于处理温度不低于T_g=210℃的轴拉试件，其自由段中部树脂因高温作用而逐渐软化、甚至部分分解(厂家提供的树脂基体5wt%质量损失相应温度为318℃)，导致树脂-纤维界面粘结性能快速衰减、部分纤维丝间无树脂而裸露。筋材轴拉应力达到极限抗拉强度后，其自由段中部裸露的纤维丝发生破断而呈现“蓬松”的状态。

2.2 CFRP筋轴拉试验结果

各轴拉试件的主要试验结果、应力-应变曲线如表3与图8所示。可见，高温下轴拉试件破断前的应力-应变基本呈线性关系。利用应力-应变曲线中0.2~0.5倍极限抗拉强度范围内的割线模量确定筋材轴向试件的弹性模量^[24]。高温下CFRP筋轴拉性能的衰减规律如图9所示。

表 3 CFRP筋轴向拉伸试验结果

Table 3. Results of axial tensile test for CFRP bar

Specimen	P_u/kN	f_u/MPa	${\overline f _{\text{u}}}/{\text{MPa}}$	E/GPa	$\overline E /{\text{GPa}}$	${ \varepsilon _{\text{u}}}/{10^{ - 6}}$	${\overline \varepsilon _{\text{u}}}/{10^{ - 6}}$
AT-T25-1	280.8	2631	2650	162.2	159.9	15627	15513
AT-T25-2	283.1	2653		161.8		15464
AT-T25-3	284.5	2666		155.6		15448
AT-T100-1	274.2	2569	2588	133.0	141.6	18506	18387
AT-T100-2	278.0	2605		143.5		18343
AT-T100-3	276.3	2589		148.3		18312
AT-T210-1	198.9	1864	1861	98.7	102.9	18298	18201
AT-T210-2	192.7	1806		105.5		18254
AT-T210-3	204.3	1914		104.4		18051
AT-T300-1	176.0	1649	1566	82.6	87.9	17963	17816
AT-T300-2	157.0	1471		92.4		17762
AT-T300-3	168.3	1577		88.8		17723
Notes: In the specimen code, AT is axial tensile, T indicates the treatment temperature, the last number indicates the same specimen number; P_u—Ultimate bearing capacity; f_u—Tensile strength; ${\overline f _{\text{u}}}$ —Average value; E—Elastic modulus; $\overline E$ —Average value; ${ \varepsilon _{\text{u}}}$ —Ultimate tensile strain; ${\overline \varepsilon _{\text{u}}}$ —Average value.

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图 8 CFRP筋轴拉试件的应力-应变曲线

Figure 8. Stress-strain curves of CFRP bar axial tensile specimen

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相较于常温试件，100℃下轴拉试件的抗拉强度、弹性模量分别减小了2.3%、11.4%，而极限拉应变增大了18.5%；210℃和300℃下轴拉试件的抗拉强度、弹性模量分别减小了(29.8%、40.9%)和(35.6%、45%)，而极限拉应变分别增大了17.3%和14.8%。可见，高温下筋材弹性模量较抗拉强度受处理温度的影响更为显著，两者的衰减幅度在处理温度由100℃增至210℃时达到最大。高温下筋材的极限拉应变较常温下有所增大，并随处理温度升高而呈先增大后减小的变化趋势。究其原因，处理温度为T_g时，筋材自由段区域的树脂逐渐软化，导致筋材整体性退化明显，各纤维间的受力更趋不均，使筋材抗拉强度与弹性模量退化显著。此外，高温下筋材的弹性模量(或轴拉刚度)较抗拉强度更依赖于树脂基体的力学性能。高温下树脂基体的力学性能因其较差的耐高温性能而快速衰减，其退化幅度远大于碳纤维，进而导致高温下筋材弹性模量的衰减幅度较抗拉强度更大、极限拉应变较常温下有所增加。

图 9 高温下CFRP筋轴拉性能衰减规律

$f_u(T)/f_u$ —Reduction coefficient of tensile strength under high-temperature;

$E_u(T)/E_u$ —Reduction coefficient of elastic modulus under high-temperature;

$\varepsilon _u(T)/\varepsilon_u$ —Reduction coefficient of ultimate tensile strain under high-temperature

Figure 9. Decay law of axial tensile performance of CFRP bar exposed to elevated temperature

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3. CFRP筋-RPC锚固性能试验结果及分析

3.1 CFRP筋-RPC锚固性能试件的破坏形态

图10为CFRP 筋-RPC 锚固性能试件破坏形态。将锚固性能试件破坏后的试验锚加载端含陶瓷套管区域切除，以便观察CFRP筋-RPC界面的破坏形态，如图10(a)所示。高温下锚固性能试件的破坏形态均为滑移破坏，具体表现为筋材表面压纹肋发生剪切破坏，其核心部分从锚固区被拔出，筋材肋间RPC未被拔出。随着处理温度升高，筋材压纹肋及肋间表面树脂逐渐软化、甚至部分分解，而高温下RPC的剩余剪切性能远高于树脂；导致压纹肋更易发生剪切破坏、从锚固区拔出的筋材核心部分表面压纹肋残留的痕迹越发模糊，无树脂包裹而裸露的部分纤维丝因与肋间RPC发生摩擦而破坏，如图10(b)所示。因此，高温下CFRP筋-RPC界面粘结性能主要取决于树脂的剩余剪切性能。

图 10 CFRP筋-RPC锚固性能试件破坏形态

Figure 10. Typical failure modes of CFRP bar-RPC anchorage performance specimens

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3.2 CFRP筋-RPC锚固性能试件的粘结-滑移曲线

各锚固性能试件的试验结果、高温下的粘结-滑移曲线分别如表4和图11所示。可见，各锚固性能试件的粘结-滑移曲线均可分为以下四个阶段：(1) 线性段。粘结-滑移基本呈线性关系，加载端的粘结界面滑移较小，均在0~1 mm之间。粘结界面的切应力主要由筋材与RPC间化学胶着力抵抗。粘结界面的化学胶着力随处理温度升高而逐渐减小，导致加载端的初期滑移逐渐增大；(2) 非线性上升段。粘结-滑移呈明显的非线性关系，筋材与粘结介质间化学胶着力丧失，粘结界面的切应力主要由筋材与RPC间摩擦力、筋材表面凸起的压纹肋及肋间RPC形成的机械咬合力共同抵抗。筋材表面的压纹肋树脂抗剪性能逐渐衰减，导致粘结强度逐渐降低；(3) 下降段。筋材表面的部分压纹肋发生剪切破坏，其与肋间RPC的机械咬合力丧失。抵抗粘结界面切应力的机械咬合力逐渐减小，导致CFRP筋-RPC界面滑移继续增大；(4) 残余段。界面的切应力主要由未拔出的筋材核心部分与RPC界面间摩擦力抵抗。随着滑移增大，试验锚陶瓷管内的带肋筋材进入锚固区，其表面压纹肋与RPC间机械咬合力参与抵抗粘结界面切应力，进而导致残余段可承担的粘结界面切应力逐渐增加。

图 11 高温下CFRP筋-RPC锚固性能试件的粘结-滑移曲线

Figure 11. Bond-slip curves of CFRP bar-RPC anchorage performance specimens exposed to elevated temperature

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采用下式计算试件锚固区CFRP筋-RPC界面的平均粘结强度τ_u，并将计算结果示于表4：

${\tau _{\text{u}}} = \frac{{{P_{\text{u}}}}}{{{\text{π}}dl}}$

(1)

式中：P_u为极限荷载值；d为筋材公称直径；l为粘结长度。

表 4 CFRP筋-RPC锚固性能试验结果

Table 4. Results of CFRP bar-RPC anchorage performance test

Specimen	T/℃	P_u/kN	${\overline P _{\text{u}}}/{\text{kN}}$	τ_u/MPa	s/mm	$\overline s_{\rm{u}} /{\text{mm}}$
A-T25-L5d-1	25	66.74	66.38	29.36	6.74	6.67
A-T25-L5d-2	25	66.02	66.38	29.36	6.60	6.67
A-T100-L5d-1	100	50.58	52.84	23.37	6.44	6.53
A-T100-L5d-2	100	55.10	52.84	23.37	6.62	6.53
A-T210-L5d-1	210	34.30	31.47	13.92	5.88	6.01
A-T210-L5d-2	210	28.64	31.47	13.92	6.14	6.01
A-T300-L5d-1	300	11.85	9.85	4.36	5.69	5.63
A-T300-L5d-2	300	7.85	9.85	4.36	5.57	5.63
Notes: In the specimen code, A is anchorage, T indicates the treatment temperature, the last number indicates the same specimen number; T—Treatment temperature; L—Bond length; τ_u—Average bond strength; s—Slip of loading end corresponding to P_u; d—Diameter of CFRP bar; $\bar P_{\rm{u}}$ —Average value of ultimate bearing capacity for anchorage system; $\bar s_{\rm{u}}$ —Average value of the slip of loading end corresponding to P_u。

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3.3 温度对CFRP筋-RPC锚固性能试件粘结强度的影响

锚固性能试件粘结强度随温度的变化规律如表4与图12所示。可见，试件粘结强度随处理温度升高而线性退化。相较于常温下的锚固性能试件，100℃、210℃和300℃下试件粘结强度分别减小了20.4%、52.6%和85.1%。究其原因为随着处理温度逐渐升至210℃和300℃，筋材表面的压纹肋树脂逐渐软化、甚至部分分解，导致用于抵抗粘结界面切应力的主要抗力—筋材压纹肋与肋间RPC的机械咬合力大幅退化。

4. 公式建立

4.1 高温下CFRP筋轴拉性能

对本文高温下轴拉试验结果进行回归分析，构建适于表征高温下(25℃ $\leqslant$ T $\leqslant$ 300℃) CFRP筋轴拉性能退化规律的计算模型，如以下两式及图9(a)、图9(b)所示：

$\frac{{{f_{\rm{u}}} \left( T \right)}}{{{f_{\rm{u}}}}} = 0.387 \exp \left[ { - 3 {{\left( {\frac{{T - {T_0}}}{{{T_{\rm{g}}}}}} \right)}^4}} \right] + 0.613$

(2)

$\frac{{{E_{\rm{u}}} \left( T \right)}}{{{E_{\rm{u}}}}} = 0.47 \exp \left[ { - 3 {{\left( {\frac{{T - {T_0}}}{{{T_{\rm{g}}}}}} \right)}^2}} \right] + 0.53$

(3)

将式(2)除以式(3)，可得高温下CFRP筋极限拉应变退化规律的计算公式为

$\frac{{{\varepsilon _{\rm{u}}} \left( T \right)}}{{{\varepsilon _{\rm{u}}}}} = \frac{{0.387 \exp \left[ { - 3 {{\left( {\dfrac{{T - {T_0}}}{{{T_{\rm{g}}}}}} \right)}^4}} \right] + 0.613}}{{0.47 \exp \left[ { - 3 {{\left( {\dfrac{{T - {T_0}}}{{{T_{\rm{g}}}}}} \right)}^2}} \right] + 0.53}}$

(4)

式中：f_u(T)、E_u(T)、ε_u(T)分别为高温下CFRP筋的抗拉强度、弹性模量及极限拉应变；f_u、E_u、ε_u为常温下CFRP筋的抗拉强度、弹性模量及极限拉应变；T₀为常温25℃；25℃ $\leqslant$ T $\leqslant$ 300℃。

图 12 处理温度对CFRP筋-RPC界面黏结强度的影响

Figure 12. Effect of elevated temperature on bond strength of CFRP bar-RPC interface

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利用式(4)计算本文各轴拉试件的极限拉应变，并将其与试验值进行对比分析，结果如表5与图9(c)所示。试验值/计算值的平均值及变异系数分别为1.010与0.01，表明式(4)可较准确地表征高温下(25℃ $\leqslant$ T $\leqslant$ 300℃) CFRP筋极限拉应变的退化规律，亦表明式(2)、式(3)均具有较高计算精度。

为明确T_g对高温下CFRP筋轴拉性能的影响规律，将本文CFRP筋(T_g=210℃)轴拉性能退化规律与文献[15]中CFRP筋(T_g=126℃)相应结果进行对比分析，如图9(a)、图9(b)及图13所示。可见本文CFRP筋极限抗拉强度和弹性模量随温度的衰减规律与文献[15]试验结果基本相似；相较于文献[15]选用的CFRP筋(T_g=126℃)，本文筋材(T_g=210℃)的高温轴拉性能更优，300℃下本文筋材的轴拉性能较常温试件仅退化46%~50%，如图9(a)与图9(b)所示；但本文筋材轴拉性能受(T−T₀)/T_g的影响更显著，如图13所示。

表 5 CFRP筋轴拉试件极限拉应变试验值与计算值对比

Table 5. Comparison of measured and predicted ultimate tensile strain of CFRP bar axial tensile specimens

Specimen	ε_u,t/10⁻⁶	ε_u,c/10⁻⁶	ε_u,t/ε_u,c
AT-T25	15513	15513	1.000
AT-T100	18387	17902	1.030
AT-T210	18201	18227	0.999
AT-T300	17816	17852	0.998
Average			1.010
Variation coefficient			0.01
Note: ε_u,t, ε_u,c—Experimental and calculated values of ultimate tensile strain of axial tensile specimen respectively.

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图 13 (T−T₀)/T_g对高温下CFRP筋轴拉性能的影响

Figure 13. Effect of (T−T₀)/T_g on axial tensile performance of CFRP bar exposed to elevated temperature

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4.2 高温下CFRP筋-RPC锚固性能试件界面粘结强度

基于ACI 440.1R-15^[24]中FRP筋-普通混凝土界面粘结强度的理论模型，对表4中的实测数据进行回归分析，构建适于表征高温下CFRP筋-RPC界面粘结强度退化规律的计算公式，如下式所示：

$\frac{{{\tau _{\rm{u}}}(T)}}{{\sqrt {{f_{{\rm{cu}}}}} }} = \left[ {1 - \frac{{0.64(T - {T_0})}}{{{T_{\rm{g}}}}}} \right]\left( {2 + 1.89\frac{d}{l}} \right)$

(5)

式中：f_cu为RPC的立方体抗压强度；T₀为室温，25℃；25℃ $\leqslant$ T $\leqslant$ 300℃。

利用式(5)预测各试件的平均粘结强度，结果如表6所示，实测值/预测值的平均值及变异系数分别为0.99与0.06，表明式(5)可较准确地表征高温下(25℃ $\leqslant$ T $\leqslant$ 300℃) CFRP筋-RPC界面粘结强度的退化规律。

表 6 CFRP筋-RPC界面粘结强度试验值与计算值对比

Table 6. Comparison between measured and predicted bond strength of CFRP bar-RPC interface

Specimen	f_cu/MPa	τ_u,t/MPa	τ_u,c/MPa	τ_u,t/τ_u,c
A-T25-L5d	158	29.36	29.89	0.98
A-T100-L5d	158	23.37	23.06	1.01
A-T210-L5d	158	13.92	13.04	1.07
A-T300-L5d	158	4.36	4.84	0.90
Average				0.99
Variation coefficient				0.06
Notes: f_cu—Cube compressive strength of RPC; τ_u,t, τ_u,c—Experimental and calculated values of interfacial bond strength between CFRP bars and RPC, respectively.

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4.3 高温下CFRP筋-RPC锚固性能试件临界锚固长度

将温升处理下CFRP筋的拉断破坏与高温下锚固区滑移破坏同时发生时所对应的筋材锚固长度定义为高温下筋材的临界锚固长度l_cr(T)，则由临界破坏时的平衡条件可知：

${\tau _{\text{u}}}(T){\text{π}}d{l_{{\text{cr}}}}(T) = {f_{\text{u}}}(T)({\text{π}}{d^2} /4)$

(6)

将式(5)代入式(6)，可得高温下CFRP筋的临界锚固长度(25℃ $\leqslant$ T $\leqslant$ 300℃)为

${l_{{\rm{cr}}}}(T) = \frac{{{f_{\rm{u}}}(T)d}}{{8\sqrt {{f_{{\rm{cu}}}}} \left( {1 - \dfrac{{0.64(T - {T_0})}}{{{T_{\rm{g}}}}}} \right)}} - 0.945d$

(7)

利用式(7)计算本文中各试件的临界锚固长度，并将其与试件实际锚固长度进行比较，以预测试件发生的破坏形态，结果如表7所示。可见，基于式(7)预测的破坏形态与实际情况吻合。

表 7 CFRP筋-RPC锚固性能试件临界锚固长度计算值及预测的破坏形态

Table 7. Critical anchorage length determined by formula and predicted failure mode of CFRP bar-RPC anchorage performance test

Specimen	T/℃	Anchorage length/mm	Actual failure mode	Critical anchorage length/mm	Predicted failure mode
A-T25-L5d	25	60	Slip	304.9	Slip
A-T100-L5d	100			389.0
A-T210-L5d	210			497.8
A-T300-L5d	300			1142.9

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5. 结论

(1) 相较于常温试件，100℃、210℃和300℃下轴拉试件的抗拉强度、弹性模量分别下降了(2.3%、11.4%)、(29.8%、40.9%)和(35.6%、45%)；而极限拉应变分别增大了18.5%、17.3%和14.8%。高温下筋材的弹性模量较抗拉强度受处理温度的影响更为显著；筋材的极限拉应变随处理温度升高而先增大后减小。

(2) 锚固性能试件碳纤维增强聚合物复合材料(CFRP)筋-活性粉末混凝土(RPC)界面的粘结强度随处理温度升高而线性退化。100℃、210℃和300℃下CFRP筋-RPC界面的粘结强度较常温试件分别下降20.4%、52.6%与85.1%。

(3) 构建了适于表征高温下CFRP筋及其粘结型锚固系统力学性能退化规律的实用计算公式，均具有较高计算精度。

(4) 高温下文中所用筋材轴拉性能较玻璃化转变温度T_g<200℃的CFRP筋更优良，但本文筋材轴拉性能受(T−T₀)/T_g(T为处理温度，T₀为室温)的影响更显著。

(5) 文中针对CFRP筋及其锚固系统高温力学性能的研究均未考虑筋材初应力的影响，与预应力结构中CFRP筋的实际受力情形存在一定偏差。但本文研究可视为后续含初应力的CFRP预应力筋及其锚固系统高温力学性能研究的基础，有必要先行开展。

图 1 Ag-BiOBr/WO₃复合材料的XRD图谱

Figure 1. XRD spectra of Ag-BiOBr/WO₃ composite

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图 2 15wt%Ag-BiOBr/WO₃的XPS图谱：(a) 总谱；(b) Bi4f；(c) Br3d; (d) O1s；(e) W4f; (f) Ag3d

Figure 2. XPS spectra of 15wt%Ag-BiOBr/WO₃: (a) Full spectra; (b) Bi4f; (c) Br3d; (d) O1s; (e) W4f; (f) Ag3d

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图 3 BiOBr (a)、WO₃(b)、BiOBr/WO₃(c) 和15wt%Ag-BiOBr/WO₃(d) 的SEM图像；(e) 15wt%Ag-BiOBr/WO₃的TEM图像；(f) 15wt%Ag-BiOBr/WO₃的HRTEM图像

Figure 3. SEM images of BiOBr (a), WO₃ (b), BiOBr/WO₃ (c) and 15wt%Ag-BiOBr/WO₃ (d); (e) TEM image of 15wt%Ag-BiOBr/WO₃; (f) HRTEM image of 15wt%Ag-BiOBr/WO₃

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图 4 15wt%Ag-BiOBr/WO₃的元素面扫图及EDS能谱图

Figure 4. Element surface scan and EDS spectrum of 15wt%Ag-BiOBr/WO₃

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图 5 复合材料的氮气吸附-脱附等温线(插图为孔径分布曲线)

Figure 5. Nitrogen adsorption-desorption isotherms of composite materials (Inset is the pore size distribution curves)

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图 6 复合催化剂对磺胺异噁唑的降解曲线 (a) 和反应动力学 (b)

Figure 6. Degradation curves (a) and reaction kinetics (b) of sulfisoxazole by composite catalyst

C₀—Initial concentration of the degradation substrate; C_t—Concentration at the t time of the degradation substrate

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图 7 不同投加量 (a) 和反应初始浓度 (b) 对15wt%Ag-BiOBr/WO₃催化性能的影响；(c) 15wt%Ag-BiOBr/WO₃的Zeta 电位

Figure 7. Different dosage (a) and influence of initial reaction concentration (b) on the catalytic performance of 15wt%Ag-BiOBr/WO₃; (c) Zeta potential of 15wt%Ag-BiOBr/WO₃

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图 8 所制备催化剂的电化学阻抗图谱 (a)、光电流响应 (b) 和荧光图谱 (c)

Figure 8. Electrochemical impedance spectra (a), photocurrent response (b) and fluorescence spectra (c) of the prepared material

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图 9 Ag-BiOBr/WO₃复合材料的紫外-可见漫反射光谱图和(αhv)²和hv的关系曲线(插图)

Figure 9. Ultraviolet-visible diffuse reflectance spectra of the Ag-BiOBr/WO₃ composite and the relationship curve between (αhv²) and hv (Inset)

α—Absorption coefficient; h—Planck constant; v—frequency

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图 10 (a) 15wt%Ag-BiOBr/WO₃降解磺胺异噁唑(SSX)过程中的自由基捕获实验(浓度[SSX]=5 mg/L、[15wt%Ag-BiOBr/WO₃]=0.3 g/L); (b) ¹O₂和•O₂^–的电子顺磁共振检测

Figure 10. (a) Free radical capture experiment in the process of 15wt%Ag-BiOBr/WO₃ degradation of sulfisoxazole (SSX) (Concentration [SSX]=5 mg/L, [15wt%Ag-BiOBr/WO₃]=0.3 g/L); (b) Electron paramagnetic resonance detection of ¹O₂ and •O₂^–

IPA—Isopropanol; EDTA-2Na—Disodium ethylene diamine tetraacetic acid; BQ—Benzoquinone

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图 11 15wt%Ag-BiOBr/WO₃在可见光照射下的光催化反应机制

Figure 11. Photocatalytic reaction mechanism of 15wt%Ag-BiOBr/WO₃ under visible light irradiation

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图 12 15wt%Ag-BiOBr/WO₃对光催化降解磺胺异噁唑的回收利用实验

Figure 12. Recycling experiment of 15wt%Ag-BiOBr/WO₃ for photocatalytic degradation of sulfisoxazole

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表 1 Ag-BiOBr/WO₃复合材料比例

Table 1 Proportion of Ag-BiOBr/WO₃ composites

Specimen	Mass fraction of Ag/wt%
BiOBr/WO₃	0
1wt%Ag-BiOBr/WO₃	1
5wt%Ag-BiOBr/WO₃	5
10wt%Ag-BiOBr/WO₃	10
15wt%Ag-BiOBr/WO₃	15
20wt%Ag-BiOBr/WO₃	20

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表 2 氮气吸附-脱附法测定复合材料比表面积

Table 2 Nitrogen adsorption-desorption method to determine the specific surface area of composite materials

Sample	Specific surface area/(m²·g^–1)	Pore volume/ (cm³·g^–1)	Average pore size/nm
WO₃	6.5917	0.0088	5.3087
BiOBr	12.4277	0.0158	5.0858
BiOBr/WO₃	13.6590	0.0685	20.5770
15wt%Ag-BiOBr/WO₃	9.0180	0.0431	19.1025

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