Fabrication of ITNPs nanocomposite by two-stepchronoamperometry electrode

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Study on Modified Graphene/Butyl Rubber Nanocomposites.I.Preparation and CharacterizationHuiqin Lian,1,2,3Shuxin Li,1Kelong Liu,1Liangrui Xu,1Kuisheng Wang,2Wenli Guo11Department of Materials Science and Engineering,Beijing Institute of Petrochemical Technology,Beijing,China2Department of Materials Science and Engineering,Beijing University of Chemical Technology,Beijing,China 3Department of Chemical Engineering,Yanbian University,Beijing,ChinaButyl rubber,IIR nanocomposites based on modified graphene sheets,were fabricated by solution process-ing followed by compression molding.MG was pre-pared from natural graphite,NG through graphite oxide route.X-ray diffraction showed that the exfoliated MG was homogeneously dispersed in the IIR matrix with doping levels of1-10wt%as evidenced by the lack of the characteristic graphite reflection in the compo-sites.In contrast,the graphite retained its stacking order and showed the sharp characteristic peak in the NG-IIR composites.Scanning electron microscope images of the fracture surfaces of the IIR matrix showed that MG nanofillers exhibited better compati-bility than NG did.The mechanical properties of the MG-IIR nanocomposites were significantly improved due to the efficient distribution of the large surface area MG sheet.The tensile modulus of nanocomposite with doping level of MG10wt%was16times that of the pure IIR.POLYM.ENG.SCI.,00:000–000,2011.ª2011 Society of Plastics EngineersINTRODUCTIONCommercial butyl rubber(IIR)is a copolymer of isobu-tylene and a small amount of isoprene.It is employed in the inner linings of automobile tires and in other specialty application due to its characteristics of chemical inertness, impermeability to gases and weatherability.However, unsaturated bonds in IIR,due to the presence of isoprene monomer units in the backbone,can be attacked by atmos-pheric ozone leading to oxidative degradation and chain cleavage.Also in somefields,such as aerospace,aircraft and high-vacuum systems,IIR does not meet the extremely high-gas barrier as well as the high mechanical properties requirements.Therefore,there exists a continuous interest in lowering gas permeability and improving the mechanical properties of IIR by various techniques[1,2].It is well known that polymeric nanocomposites are of great interest for both scientific challenges and industrial applications due to their enhanced mechanical properties and unique material properties[3–5].Compared with con-ventional systems,nanomaterials are more effective rein-forcements because the stress transfer from the matrix to the reinforcement is more efficient in nanocomposites due to the increased surface area,assuming good adhesion at the interface.Also,the crack propagation length at the interface becomes longer,improving the strength and toughness.In addition to improving the mechanical prop-erty,nanofillers,such as layered silicate or carbon nanotubes,can provide dramatic improvement in thermal stability,dimensional stability,heat-distortion tempera-ture,and barrier property[6–11].Recently,graphite oxide (GO)has attracted increasing interest as afiller for poly-mer nanocomposites due to its high dispersive capacity, long coherence length and the barrier property[12,13]. GO with a typical pseudo-two-dimensional structure gen-erally contains hydroxyl,carboxyl and ether groups, which causes GO to absorb polar molecules easily and thus GO/polymer composites can be formed.Such struc-tural nanocomposites can provide reinforcement to the base polymer matrix.Also,GO may also have other desirable properties,such as mass diffusion coefficients, coefficients of thermal expansion,dielectric constants, thermal/chemical stability,solvent resistance,selectivity, conductivity,and resistivity to membrane fouling and poisoning.However,as a reinforcement of IIR,the hydro-philic surface of GO makes it difficult to disperse in the hydrophobic IIR matrix.Therefore,it is an importantCorrespondence to:Wenli Guo;e-mail:wlguo2008@Contract grant sponsor:Natural Science Foundation of China(NSFC);contract grant number:51063009;contract grant sponsor:BeijingNatural Science Foundation of China;contract grant number:KZ200910017001.DOI10.1002/pen.21997Published online in Wiley Online Library().V C2011Society of Plastics EngineersPOLYMER ENGINEERING AND SCIENCE—-2011Administratorissue to improve the compatibility of the GO sheet with the IIR matrix.Moreover,methods used to prepare polymeric nano-composites include in-situ polymerization [14],solution mixing [15],melting compound [16],and cocoagulating of polymeric composite solution [17].Considering the manufacture process of the IIR,slurry and solution pro-cess,the solution mixing is promising to fabricate IIR hybrids in the IIR industry.In this study,we report for the first time the fabrication of well-dispersed modified graphene in IIR composites through solution process.The MG nanosheets are homo-geneously dispersed in the IIR matrix with doping level of 1–10wt%.Compared with the pure IIR,the resulting nanocomposite membranes exhibit dramatic enhancement of mechanical properties.To the best of our knowledge,this is the first report of totally exfoliated graphite to reinforce IIR with outstanding mechanical property.The properties of vulcanization plateau,gas barrier,cure capa-bility,and rubber damping are under study and the results will be published in the near future.EXPERIMENTAL PROCEDURES MaterialsNatural graphite flakes with a partical size of 30l m were purchased from Aladdin Reagent Company (China).Cetyltrimethylammonium bromide (CTAB)was bought from Fuchen Chemical Reagents(Tianjin,China).Butyl rubber (IIR 1751)was obtained from YanShan Petrochem-ical Company of China.The other reagents (NaOH,NaNO 3,and KMnO 4)of analytical grade and 98%H 2SO 4,30%H 2O 2were purchased from Sinopharm Chemical Reagent Co.Ltd.(China)and were used as received with-out further purification.Ultrapure water with resistivity of 18M O was produced by a Milli-Q(Millipore,USA)and was used for solution preparation.Preparation of MG/NG-IIR Composite SheetsThe procedure used to prepare the MG-IIR nano-composite sheets was shown in Fig. 1.First,based on Hummers’method [18],the graphite was oxidized by con-centrated sulfuric acid to create polar hydrophilic groups (ÀÀCOOH,C ¼¼O,ÀÀOH)on the surface.The GO was dispersed in cetyltrimethylammonium bromide solution (20wt%)and ultrasonicated for 0.5h,followed by me-chanical stirring at 258C for 24h.During this process,the tertiary amine reacted with the carboxylic groups on the oxidized surface via an acid-base reaction or via hydrogen bonding between the surface ÀÀOH or C ¼¼O group and the amine groups.The suspension was filtrated and washed three times with water,dried at 408C in a vacuum for 24h.The resulting MG was added into the 15wt%solution of IIR in hexane by sonication for 0.5h to form a colloidal suspension.Then the mixture was stirred for 6h at 258C.The amounts of MG/NG added were 0,1,3,5,10wt%ofthe mass of rubber.The composite solution was then coa-gulated by adding methanol and the precipitated nanocom-posite was dried in a vacuum.Finally,sheet samples were prepared by vacuum compression molding using a 2mm thick spacer at 1008C under 10MPa for ing this procedure,the NG-IIR composite sheets were prepared.CHARACTERIZATION AND MEASUREMENTS The as-made membrane was characterized by X-ray diffraction (XRD,Scintag PAD X diffractometer,Cu K a source,operated at 45kV and 40mA).The samples were scanned with 58/min between 2y of 28–308.SEM observation was performed using Tecnai T12,at an acceleration voltage of 15kV with gold -posite samples were imaged by first fracturing in liquid nitrogen.TGA was performed using a TA Instrument Q500attached to an automatic programmer from ambient tem-perature to 5008C at a heating rate of 108C/min in a nitro-gen atmosphere.A TA instrument Q1000was used to record the DSC traces at a heating rate of 108C/min.Measurements of mechanical properties were con-ducted at 25628C according to relevant ISO standard (ISO 37).Tensile tests were measured on an Autograph AGS-J SHIMADZU universal testing machine at a cross-head speed of 500mm/min.The reported values were the average of five measurements.RESULTS AND DISCUSSIONThe FTIR spectra of NG,GO,and MG were shown in Fig.2.The FT-IR spectrum of NG showed no significant features.While that of GO showed quite differentFIG.1.Schematic representation for the fabrication of MG-IIR nano-composite membrane.2POLYMER ENGINEERING AND SCIENCE—-2011DOI 10.1002/pencharacter by the presence of new bands.The broad bandat3405cm21could be assigned to stretching of the ÀÀOH groups on the GO surface.The bands at1720and 1070cm21were associated with stretching of the C¼¼Oand CÀÀO stretching vibrations of carboxylic groupsrespectively.The FTIR spectrum of MG confirmed theeffective functionalization of graphene.The double bandsat2849and2919cm21were antisymmetric and symmet-ric CÀÀH stretching vibrations of theÀÀCH2ÀÀgroups from surfactant molecules[19]respectively.The bands at 1463and1127cm21were corresponding to CÀÀH bend-ing and the C-N stretching vibration respectively.The spectrum also showed a C¼¼C peak at1574cm21corre-sponding to the skeletal vibration of graphene sheets[20]. These spectral features showed that MG was successfully synthesized.The XRD patterns of the NG,GO,MG were shown inFig.3.The sharp diffraction peak around26.5o for pris-tine graphite(Fig.3a)showed that the basal spacing was0.34nm.Because of the strong Van der Waals force andstatic electric force between the sheets of graphite,thesheet was difficult to disperse.Thus a relatively strongoxidative acid was used to oxidize the graphite creatingpolar groups on the surface of graphite sheet.The surfac-tant of cetyltrimethyl ammonium bromide was used to functionalize the oxidized graphite through acid-base reaction to obtain stable exfoliated graphene sheets.As shown in Fig.3a,the GO showed two diffraction peaks at 2y of9.7o and25.3o,corresponding to a d-spacing of0.91 and0.35nm,respectively,and indicated that the GO was not fully oxidized and the additional peak at25.3o was that of unoxidized graphite.From Fig.3b,MG showed no characteristic peak indicating that the modified graphene sheet had been exfoliated completely.The XRD patterns of MG/NG-IIR nanocomposites membranes with different doping levels were presented in Fig.4.As shown in Fig.4a,the broad peak of2y around 15o appeared in IIR and NG-IIR membranes,due to the amorphous phase of IIR.Toki et al.[21]reported that the amorphous peak of IIR changed during uniaxial deforma-tion.In this case,with NG loading increase,the broad peak shifted slightly,from2y of14.7o in IIR to14.4o in 10wt%NG-IIR composite.It was deduced that NG did not influence the crystallization behavior of IIR very much.From Fig.4a,the diffraction peak at2y around 26.5o appeared in NG and NG-IIR composites because the NG retained its stacking order in the composite.XRD diffraction curves of MG-IR nanocomposites were shown in Fig.4b.The diffraction ascribed to graphite or oxidized graphite did not appear in all of the XRD patterns of composites,indicating the complete exfoliation of the MG in the IIR matrix.SEM images of the fractured surfaces of the as-made MG-IIR and NG-IIR composites were shown in Fig.5. SEM images of NG-IIR composites showed a smooth to-pography with the NG remained its stacking order in the IIR matrix(Fig.5a and b).In contrast,the MG-IIR com-posites appeared a rough surface and the MG dispersed in IIR matrix homogenously(Fig.5c and d).This is likely due to the organic modifier on the surface of MG produc-ing good compatibility with IIR matrix.These results were coincident with the XRD test.TGA under a nitrogen atmosphere was performed on NG,MG,IIR and MG-IIR composites to obtain the struc-ture of MG and composites,as well as to determine the effects of the MG on the thermal stability of the compo-sites.The resulting curves were shown in Fig.6.From FIG.2.FT-IR spectra of NG,GO andMG.FIG.3.The XRD patterns of(a)NG,GO and(b)MG.The curves are shifted vertically for clarity.DOI10.1002/pen POLYMER ENGINEERING AND SCIENCE—-20113FIG.4.The XRD patterns of composites(a)NG-IIR and(b)MG-IIR.The curves are shifted vertically forclarity.FIG.5.SEM images of fracture surface of(a,b)NG-IIR nanocomposites and(c,d)MG-IIR nanocompo-sites.4POLYMER ENGINEERING AND SCIENCE—-2011DOI10.1002/penNG curve of Fig.6a,graphite maintained its weight under the test condition.The curve of MG indicated that MG was composed of 17wt%graphene and 83wt%organicmodifiers.The functional surface contributed to the dis-persion of MG in the IIR solution as well as to the com-patibility with the IIR matrix in the composite membrane.Figure 6b indicated that the IIR began to decompose at 2698C and degraded completely at 4158C.In the case of MG/IIR composites,the weight loss below 3008C was attributed to the decomposition of the small organic molecules on the surface of graphene.Table 1listed the temperature at 5wt%loss of the TGA curve of IIR and MG-IIR composites.The pure IIR lost 5wt%at 3248C and the value was the highest of all the curvesobtained.FIG.6.(a)TG curves of NG and MG;(b)TG curves of MG-IIR nano-composites and (c)DTG curves of MG-IIR nanocomposites.TABLE 1.Thermal propertiesofpureIIRandMG-IIRnanocomposites.IIR 1%MG-IIR 3%MG-IIR 5%MG-IIR 10%MG-IIRT 5wt%(8C)a 324297321256236T mrv (8C)b 372368375378383a Temperature at 5wt%loss.bTemperature at the maximum reactivevelocity.FIG.7.DSC curves of MG-IIRnanocomposites.FIG.8.Tensile stress-strain curve of (a)MG-IIR nanocomposites and (b)NG-IIR nanocomposites.DOI 10.1002/pen POLYMER ENGINEERING AND SCIENCE—-20115The temperature at5wt%loss decreased with the increas-ing MG content when the MG contents were3,5,and10wt%in composites respectively.This might be due to theamount of small molecule of organic modifier increasedwith the increasing MG content.Thefirst derivative of the TGA curve(DTA curvesshown in Fig.6c showed the variation in weight withtime(dW/dT)as a function of temperature.The DTApeaks indicated the temperature of the maximum reactivevelocity.Table1listed the temperature at the maximumreactive velocity of the DTA curve of IIR and MG-IIRcomposites.Pure rubber reached the maximum reactivevelocity at3728C.The value of1wt%MG-IIR nanocom-posite was3688C and it was lower than that of IIR.Thismight be that the amount of graphene was too low toinfluence the thermal stability of the composite,whilesmall organic molecules on the surface of graphene withlow decomposition temperature induced the thermaldecomposition.For all other composites,the temperatureat the maximum reactive velocity increased with increas-ing graphene content,and for the10wt%composite itwas increased by118C compared with pure IIR.Thisindicated that the thermal stability of IIR was improvedby the addition of graphene.A significant number ofpapers had reported increased thermal stability of variouspolymers using graphene asfiller[15,22,23].T.Kuilaet al.reported that the better thermal stability of gra-phene/polyethylene composite system was due to the highaspect ratio of the monodispersed graphene layers whichacted as a barrier and inhibited the emission of small gas-eous molecules[23].DSC for the MG/IIR nanocomposites was shown inFig.7.The glass transition(T g)temperature of IIR wasobserved at270.58C,and the MG loading increased,theT g values of composites which were269.28C,268.68C, 268.98C,and269.18C with the loading levels of1,3,5, 10wt%,respectively.All the composites showed aslightly higher T g than that of pure IIR;among them thehighest one was268.68C of3wt%MG-IIR nanocompo-site.It indicated that the effective exfoliation of the MGincreased the T g due to the interaction between MG andpared with the results of graphene/polystyrenenanocomposite[24],the incorporation of PS nanoparticleson graphene sheets resulted in an increase in T g by178C,while the exfoliated MG did not influence the T g of MG-IIR nanocomposite very much.Therefore,the properties of nano-filler influenced the phase behavior of polymer matrix.The interaction between MG and IIR is under further study.The typical stress–strain curves for the MG-IIR and NG-IIR compositesfilms were presented in Fig.8.The mechanical performance of MG/IIR and NG/IIR compos-itefilms was significantly increased compared with pure IIRfilm(Fig.8a and b).The effect of MG content on mechanical properties of the nanocomposites was shown in Table 2.Stresses at 100%,200,and300%elongation of composites increased along with the MG loading increase.Therefore,in this study,MG-IIR nanocomposites had higher mechanical properties than that of pure IIR.On the basis of these stress–strain curves of tensile tests(Fig.8a and b),Young’s moduli were taken as the linear regression of the initial linear part of stress–strain curves.Figure9a showed the representative calculated Young’s moduli of IIR,NG-IIR,and MG-IIR.The corre-sponding Young’s modulus values were shown in Fig.9b. The addition of MG grapheneflakes significantly increased the Young’s modulus.Remarkably,the Young’s modulus of10wt%MG-IIR was16times that of pure IIR.In comparison,the10wt%NG-IIR compositesTABLE 2.Mechanical properties of pure IIR and MG-IIR nanocomposites.Stress at 100%(MPa)Stress at200%(MPa)Stress at300%(MPa)IIR0.170.190.181%MG-IIR0.250.230.183%MG-IIR0.440.380.295%MG-IIR0.540.430.3110%MG-IIR0.770.590.40FIG.9.(a)Representative calculated Young’s moduli of IIR,NG-IIR,and MG-IIR based on the slope of the elastic region.(b)Dependence ofYoung’s modulus on loading offillers in MG-IIR and NG-IIR nanocom-posites.6POLYMER ENGINEERING AND SCIENCE—-2011DOI10.1002/penimproved3.5times only,as shown in Fig.9b.It might be that the NG stacks did not exfoliate or intercalate in the IIR matrix.This result coincided with the results of the XRD and SEM analysis.Therefore,from the result of mechanical properties,it was deduced that the modifier on the surface of the gra-phene sheet not only caused the sheet to disperse in the IIR matrix,but also bonded to the large rubber chain in two dimensions,which gave the nanocomposite better tensile performance.According to the reference[25],gra-phene layers in poly(vinyl chloride)matrix enhanced the mechanical properties of PVC,because of the strong interfacial adhesion.Therefore,in our case,MG-IIR nano-composites had higher mechanical properties than the pure IIR,which may be due to the homogenous distribu-tion of exfoliated MG and the good compatibility with polymer matrix.CONCLUSIONMG-IIR nanocomposites were prepared by solution processing.SEM and XRD analysis indicated that the exfoliated MG was homogeneously disperse in the IIR matrix.The addition of MG greatly improved the mechan-ical property of the nanocomposites.The nanocomposites with10wt%MG showed the highest Young’s modulus, 3.4MPa,which was about16times higher than that of pure IIR,0.21MPa.REFERENCES1.S.Takahashi,H.A.Goldberg,C.A.Feeney,D.P.Karim,M.Farrell,K.O’Leary,and R.Paul,Polymer,47,3083 (2006).2.Y.Liang,W.Cao,Z.Li,Y.Wang,Y.Wu,and L.Zhang,Polym.Test.,27,270(2008).3.N.A.Kotov,Nature,442,254(2006).4.M.A.Pulickel and M.T.James,Nature,447,1066(2007).5.E.P.Giannelis,Adv.Mater.,8,29(1996).6.Camenzinda,W.R.Caserib,and S.E.Pratsinis,Nano Today,5,48(2010).7.S.C.Tjong,Mater.Sci.Eng.,R53,73(2006).8.Suresha,B.N.Ravi Kumar,M.Venkataramareddy,and T.Jayaraju,Mater.Des.,31,1993(2010).9.H.Kim and C.W.Macosko,Polymer,50,3797(2009).10.Y.Liang,Y.Wang,Y.Wu,Y.Lu,H.Zhang,and L.Zhang,Polym.Test.,24,12(2005).11.E.Burgaz,H.Lian,R.H.Alonso,L.Estevez,and E.P.Gian-nelis,Polymer,50,2348(2009).12.Y.Lian,Y.Liu,T.Jiang,J.Shu,H.Lian,and M.Cao,J.Phys.Chem.C,114,21(2010).13.K.Kalaitzidou,H.Fukushima,and L.T.Drzal,Compos.Sci.Technol.,67,2045(2007).14.J.M.Herrera-Alonso,Z.Sedlakova,and E.Marand,J.Membr.Sci.,349,251(2010).15.S.Ansari and E.P.Giannelis,J.Polym.Sci.Part B:Polym.Phys.,47,888(2009).uki, A.Tukigase,and M.Kato,Polymer,43,2185(2002).17.L.Q.Zhang,Y.Z.Wang,Y.Q.Wang,Y.Sui,and D.S.Yu,J.Appl.Polym.Sci.,78,1873(2000).18.W.S.Hummers and R.E.Offeman,J.Am.Chem.Soc.,80,1339(1958).19.P.J.Thistlethwaite and M.S.Hook,Langmuir,16,4993(2000).20.T.Szabo,O.Berkesi,and I.Dekany,Carbon,43,3186(2005).21.S.Toki,I.Sics,B.S.Hsiao,S.Murakami,M.Tosaka,S.Poompradub,S.Kohjiya,and Y.Ikeda,J.Polym.Sci.Part B:Polym.Phys.,42,956(2004).22.Q.L.Bao,H.Zhang,J.X.Yang,S.Wang,D.Y.Tong,R.Jose,S.Ramakrishna,C.T.Lim,and K.P.Loh,Adv.Funct.Mater.,20,1(2010).23.T.Kuila,S.Bose,C.E.Hong,M.E.Uddin,P.Khanra,N.H.Kim,and J.H.Lee,Carbon,49,1033(2011).24.A.S.Patole,S.P.Patole,H.Kang,J.Yoo,T.Kim,and J.Ahn,J.Colloid Interface Sci.,350,530(2010).25.S.Vadukumpully,J.Paul,N.Mahanta,and S.Valiyaveettil,Carbon,49,198(2011).DOI10.1002/pen POLYMER ENGINEERING AND SCIENCE—-20117。

万方数据　万方数据第ｌｏ期束华东等表面修饰纳米二氧化硅及其与聚合物的作用条件，如一ＣＯＯＨ、一ＮｃＯ和一ＣＨｃＨ：０等，以保证修饰的稳定性。

Ｔａｎｇ等ｍ１和Ｄｉｎｇ等汹１在各自的工作中都用油酸修饰纳米ＳｉＯ：，修饰剂以稳定的化学键与纳米颗粒连接，同时油酸上带有的Ｃ—Ｃ又为ＳｉＯ：提供了表面功能化的基团。

此外，乙烯基吡啶协１、丙烯基缩水甘油醚ｍ１和对乙烯基苯磺酰肼Ⅲ１等用作纳米ｓｊ０２表面修饰剂的工作都有报道。

在我们以前的工作中，用六甲基二硅氮烷作为修饰剂合成了具有超强疏水性能的可分散型纳米ＳｉＯ：颗粒，涂层与水的接触角可达１７００，同时在有机溶剂中有良好的分散性，分散在ｃｏ，中溶液的透光率可达９７％以上旧Ｊ。

还有用乙二胺和硬脂酸对纳米ＳｉＯ：颗粒表面双重修饰，这是一种以离子键连接表面修饰剂和纳米颗粒的修饰方式，产物的粒径在２０ｎｍ左右ｍｏ。

此外，我们还利用不同的硅烷偶联剂合成了表面带有不同官能团的可反应性纳米ＳｉＯ，颗粒ｂ“。

目前，我们所开发的上述产品已经在本单位的纳米材料工程技术研究中心实现了规模化生产。

图３为生产的ＤＮＳ．２可分散型纳米ＳｉＯ，的透射电镜形貌，从图中可以看出纳米ＳｉＯ，颗粒粒径均匀，平均约２０ｎｍ，分散优良，以链状或网状存在。

图３ＤＮＳ－２可分散型纳米ｓｉ０２的ＴＥＭ形貌Ｆｉｇ．３ＴＥＭｉｍａｇｅｏｆｔｈｅｄｉｓｐｅｒｓｉｂｌｅｎｌｌｌｌＯ—Ｓｉ０２２纳米ＳｉＯ：颗粒与聚合物基体的作用方式及其对材料性能的影响聚合物／ＳｉＯ：纳米复合材料能有效地综合利用纳米ｓｉ０２和聚合物材料的各项优越性能，使材料的功能多样化，性能优越化。

纳米ＳｉＯ，与聚合物基体的复合方法主要包括：机械共混法、熔融共混法、溶胶．凝胶法和原位分散聚合法等。

不同的复合方法各有其优点，适用于不同的材料，对纳米颗粒和基体材料的作用方式也有着不同的影响。

在聚合物／ＳｉＯ：纳米复合材料中，纳米颗粒与聚合物基体间作用力的形式和大小对材料的性能会产生较大的影响，提高二者间的作用力是提升材料性能的主要手段。

水凝胶简介水凝胶是一种具有亲水性的三维网状交联结构的高分子网络体系。

水凝胶性质柔软，能保持一定的形状，能吸收大量的水，具有良好的生物相容性和生物降解性。

自从20世纪50年代由Wichterle等首次报道后，就被广泛地应用于组织工程、药物输送、3D细胞培养等医药学领域。

[1]水凝胶根据交联方式不同，分为物理交联水凝胶和化学交联水凝胶。

物理凝胶是指通过静电力、氢键、疏水相互作用等分子间作用力交联形成的水凝胶。

这种水凝胶力学强度低，温度升高会转变成溶胶。

化学交联水凝胶是指通过共价键将聚合物交联成网络的凝胶。

其中，共价键通过“点击”反应生成，比如硫醇-烯/炔加成、硫醇-环氧反应、叠氮-炔环加成、席夫碱反应、环氧-胺反应、硫醇-二硫化物交换反应等。

Gao Lilong等在生理条件下将N,N-二甲基丙烯酰胺、甲基丙烯酸缩水甘油酯和聚低聚乙二醇巯基丁二酸通过巯基-环氧“点击”反应制备得到可注射水凝胶。

[2]和物理凝胶相比，化学交联水凝胶稳定性较好，力学性能优异。

根据来源不同，水凝胶又可分为天然水凝胶和合成水凝胶。

天然水凝胶包括琼脂、壳聚糖、胶原、明胶等，它们大都通过氢键交联形成。

合成水凝胶包括聚乙二醇、丙烯酸及其衍生物类（聚丙烯酸，聚甲基丙烯酸，聚丙烯酰胺，聚N-聚代丙烯酰胺等）。

和合成水凝胶相比，天然水凝胶生物相容性较好，环境敏感性好，价格低廉，但稳定性较差。

目前，有学者将天然高分子和合成高分子交联制备杂化水凝胶。

比如，Lei Wang等将壳聚糖和聚异丙基丙烯酰胺交联得到热敏性杂化水凝胶用于体内药物输送，并利用近红外光引发药物释放。

[3]水凝胶凭借良好的生物相容性广泛地应用于药物输送、组织再生等医药学领域。

药物可以通过化学接枝和包埋等方式实现负载。

负载药物的水凝胶通过移植或注射进入生物体内，然后在体内逐渐降解实现药物的缓慢释放。

为了更好地实现药物的输送和释放，智能水凝胶应运而生，所谓智能水凝胶，是指能够对外界环境的变化，比如pH、温度等做出反应的水凝胶，从而实现药物的可控释放。

Electro-Fenton Degradation of Rhodamine B Based on a Composite Cathode of Cu 2O Nanocubes and Carbon NanotubesZhihui Ai,†Haiyan Xiao,†Tao Mei,†Juan Liu,†Lizhi Zhang,*,†Kejian Deng,*,‡and Jianrong Qiu §Key Laboratory of Pesticide &Chemical Biology of Ministry of Education,College of Chemistry,Central China Normal Uni V ersity,Wuhan 430079,People’s Republic of China,Key Laboratory of Catalysis andMaterials Science of the State Ethnic Affairs Commission &Ministry of Education,College of Chemistry and Materials Science,South-Central Uni V ersity for Nationalities,Wuhan 430074,People’s Republic of China,and National Coal Combustion Laboratory,Huazhong Uni V ersity of Science and Technology,Wuhan 430074,People’s Republic of ChinaRecei V ed:April 15,2008;Re V ised Manuscript Recei V ed:May 26,2008In this study,rhodamine B (RhB)in aqueous solution was effectively degraded by an electro-Fenton (E-Fenton)system with a novel oxygen-fed gas diffusion electrode.This electrode was prepared by combining Cu 2O nanocubes and multiwall carbon nanotubes with poly tetrafluoroethylene (Cu 2O/CNTs/PTFE).The resulting Cu 2O nanocubes and Cu 2O/CNTs/PTFE composite cathode were examined by X-ray diffraction (XRD),scanning electron microscopy (SEM),energy dispersive X-ray analysis (EDX),and transmission electron microscopy (TEM).The degradation of RhB in this E-Fenton system reached 80.2%and 89.3%in 120min at neutral pH and pH 3,respectively.A pseudofirst-order kinetics was observed for the degradation of RhB in this E-Fenton system.We studied the factors affecting the degradation of RhB with Cu 2O/CNTs/PTFE composite cathodes in detail,and detected hydrogen peroxide electro-generated through the reduction of O 2adsorbed on the cathode and copper ions produced by the slow leakage of Cu 2O nanocubes.Cyclic voltammetry (CV)experiments revealed that a two-electron reversible redox reaction happened on the Cu 2O/CNTs/PTFE cathode in this new E-Fenton system.More importantly,we found the Cu 2O/CNTs/PTFE cathode was very stable and could be reused without catalytic activity decrease,suggesting its potential in the wastewater treatment.IntroductionWater pollution by toxic and nonbiodegradable organic materials brings about very serious health threats to the living species.The enormous diversity of pollutants with different chemical composition excludes the possibility of using a universal treatment method and thus requires the development of special treatment methods for contaminated water.1Recently,advanced oxidation processes (AOPs)for wastewater treatment have attracted more attention because of their formation of hydroxyl radicals (•OH).•OH radicals are the most powerful oxidizing species after fluorine in aqueous environment.2Among the AOPs technologies,Fenton reaction has proven to be one of the most effective methods to degrade organic pollutants in wastewater.The generally accepted free radical chain mecha-nism for the classic homogeneous Fenton reactions consisting of the ferrous ions and hydrogen peroxide is shown in eqs 1–5.3Fe2++H 2O 2f Fe3++•OH +OH-(1)Fe 3++H 2O 2f Fe 2++•HO 2+H +(2)Fe 2++•OH f Fe 3++OH -(3)•OH +H 2O 2f •HO 2+H 2O(4)•HO 2+•HO 2f H 2O 2+O 2(5)However,there are some drawbacks in this classic homoge-neous Fenton system.First,the ferric ions remaining in the treated wastewater require a separation step.This complicates the overall process and makes it uneconomical.Second,classic Fenton’s reagents work well only within a narrow pH range (pH 3-4)because iron precipitates as a hydroxide at higher pH values.Third,the cost of H 2O 2is very high for its large-scale application in wastewater treatment engineering.4There-fore,researchers have been making great efforts to overcome these problems.One effort is to develop a Fenton-like system containing other transition metals (Fe 3+,Co 2+,Ni 2+,and Cu 2+)and H 2O 2shown in eq 6M (n -1)++H 2O 2+H +f M n ++•OH +H 2O(6)where M is the transition metal and n is the charge of the metal ion in an oxidized state.Another effort is to develop heterogeneous Fenton-like system containing solid phase catalysts and H 2O 2.For example,Fe containing solids,such as goethite,hematite,clay minerals,iron hydroxide and iron supported on silica and on alumina were used previously.An advantage of a Fenton-like or heterogeneous Fenton system arises from its characteristics of a wide-working pH range (pH 3-7)compared to the classic homogeneous Fenton system.5For instance,copper ions have been selected as the Fenton reagent instead of Fe ions because copper ions are able to work well at neutral pH,allowing treatment of industrial organic contaminated wastewater without the pread-*To whom correspondence should be addressed.E-mail:zhanglz@;dengkj@.Tel/Fax:+86-27-67867535,67843930.†Central China Normal University.‡South-Central University for Nationalities.§Huazhong University of Science and Technology.J.Phys.Chem.C 2008,112,11929–119351192910.1021/jp803243t CCC:$40.75 2008American Chemical SocietyPublished on Web 07/16/2008justment of pH.The reactions using copper ions as the Fenton-like reagent are similar to that of Fe ions (eqs 7and 8).62Cu ++O 2+2H +f 2Cu 2++H 2O 2(7)Cu ++H 2O 2+H +f Cu 2++•OH +H 2O(8)The third effort is to develop some combinations of AOP technologies such as photo-Fenton process,sono-Fenton process,and electro-Fenton process to enhance the generation of hy-droxyl radicals,and thus reduce the consumption of H 2O 2.Recently,an increasing number of papers have been published that deal with the destruction of toxic and refractory organic pollutants in waters by means of E-Fenton methods.7–12The E-Fenton systems can continuously supply H 2O 2to the con-taminated water through the two-electron reduction of oxygen gas given by eq 9.Meanwhile,the transition metal ions (M n +)are added to the contaminated water to catalyze electro-generated H 2O 2to produce the oxidizing agent ·OH via Fenton reactions.In the E-Fenton systems,the regeneration of M (n -1)+can occur either by a direct cathodic reaction (eq 10),by the oxidation with an organic radical (eq 11),or by the reaction with H 2O 2(eq 12).13Compared with the classic Fenton systems,the E-Fenton systems can avoid the addition of expensive H 2O 2and maintain an almost constant concentration of electro-generated H 2O 2during the whole pollutants removal process as follows:O 2(g)+2H ++2e -f H 2O 2(9)M n ++e -f M (n -1)+(10)M n ++•R f M (n -1)++R +(11)M n ++H 2O 2T [M -O 2H](n -1)++H +T M (n -1)++•HO 2(12)In E-Fenton systems,the common supports for electrocata-lysts are high surface area carbon blacks.This is because ideal supports for electrocatalysts should also have the characteristics of high electrical conductivities,good reactant gas access to the electrocatalyst,adequate water handling capability,and good corrosion resistance,especially under the highly oxidizing conditions.Some carbon blacks like Vulcan XC-72R,for instance,possess all of the above mentioned characteristics.14Other well-studied carbon supports mainly focus on traditional forms of carbon such as reticulated vitreous carbon,15,16carbon felt,17activated carbon fiber,18,19and carbon-PTFE O 2-diffusion cathodes.11,20–22Much less attention has been paid to a new carbon materials carbon nanotubes (CNTs)as the cathode for H 2O 2electro-generation,although CNTs have good electrical conductivity and mechanical strength,as well as relative chemical inertness to most electrolyte solutions,high surface activity,and a wide operational potential window.23–28Our previous work revealed that H 2O 2with a constant concentration can be continuously electro-generated on the Fe@Fe 2O 3/CNTs composite electrode during the E-Fenton process of degradation of RhB.19However,we found that the Fe@Fe 2O 3/CNTs composite electrode was not stable enough.Its activity decreased after several heterogeneous E-Fenton treatment processes.This instability may hamper its application in practical wastewater remediation engineering.Therefore,it is still necessary to develop more stable and efficient electrodes for a heterogeneous E-Fenton system.Cuprous oxide (Cu 2O)offers important applications in hydrogen production,superconductor,solar cell,and negative electrode materials;it also has a potential application in photo-Fenton degradation of organic pollutants.In the present study,we synthesized Cu 2O nanocubes via a microwave-assisted benzyl alcohol approach.The as-prepared Cu 2O nanocubes were combined with multiwall carbon nanotubes by using poly tetrafluoroethylene to form a novel oxygen-fed gas diffusion electrode (Cu 2O/CNTs/PTFE).We established a new and scalable E-Fenton system on the basis of this novel oxygen-fed gas diffusion electrode for the first time.In this new E-Fenton system,both copper ions (Cu 2+/Cu +)and H 2O 2were in situ produced.Meanwhile,this system could work at a wide pH range.29,30It was interesting to find that the E-Fenton system with Cu 2O/CNTs/PTFE cathodes could efficiently degrade RhB without losing activity after long-term run,suggesting its potential in the wastewater treatment.Experimental SectionChemicals.Cu(NO 3)2·6H 2O and benzyl alcohol were pur-chased from Sinopharm Chemical Reagent Co.,Ltd.(Shanghai,China)and used without further purification.All chemicals used in this study were of commercially available analytical grade.Deionized water was used in all experiments.Synthesis of Cu 2O Nanocubes.In a typical synthesis,0.1mol of copper nitrate was dissolved in 20mL of benzyl alcohol.The resulting solution was reacted at 180°C for 45min under irradiation produced by a microwave oven (MAS-1,Shanghai Xinyi Ltd.).During the reaction,the solution was magnetically stirred.The product was centrifuged,washed thoroughly with anhydrous ethanol,and finally dried in a vacuum oven at 60°C.Preparation of the Cu 2O/CNTs/PTFE Cathodes.The Cu 2O/CNTs/PTFE cathodes were prepared by combining Cu 2O nanocubes and multiwall carbon nanotubes with poly tetrafluo-roethylene (PTFE),which was slightly modified from the method reported in our previous study.19In a typical procedure,CNTs with width of 40-60nm and length of 3-5µm (Shenzhen Nano-Harbor Co.),PTFE suspension (60wt%),and Cu 2O nanocubes were first mixed in ethanol and ground and then dried at 80°C to form a dough-like paste.The paste was finally rolled to be a thin layer of 0.2mm thickness.This layer of catalyst was fixed between two pieces of nickel mesh current collectors and then dried.The final thickness of the electrode was controlled at about 0.50mm.The optimal mass ratio of CNTs:Cu 2O:PTFE was found to be 10:30:1(Supporting Information).Characterization of the Cu 2O Nanocubes and the Cu 2O/CNTs/PTFE Cathodes.X-ray powder diffraction (XRD)pat-terns were obtained on a Bruker D8Advance X-ray diffracto-meter with Cu Ka radiation (λ)1.54178Å).Scanning electron microscopy (SEM)and energy dispersive X-ray (EDX)analysis were performed on a LEO 1450VP scanning electron micro-scope.Transmission electron microscopy (TEM)study was carried out on a Philips CM-120electron microscopy instrument.Degradation of Rhodamine B.Degradation of Rhodamine B by E-Fenton processes was preformed in a divided thermo-static cell of 150mL in volume by using CHI-660B (Shanghai,China)as a potentiostat.31During our experiments,the potential between the anode and the cathode was controlled at 1.2V (∆E )1.2V).The anode was a Pt sheet (purity:99.99%)of 2.0cm 2in area obtained from Beijing Academy of Steel Service (China).The as-prepared Cu 2O/CNTs/PTFE cathode was used as the working cathode (3.0cm 2in area).The initial concentra-tion of RhB was 1.044×10-5M.A 0.05mol ·L -1of Na 2SO 4aqueous solution was used as the supporting electrolyte to increased the conductivity.The initial pH of the dye solution11930J.Phys.Chem.C,Vol.112,No.31,2008Ai et al.was about6without adjusting.In some cases,the initial pH value of RhB solution was adjusted to3or9by the addition of 0.10M H2SO4or0.10M NaOH,respectively.A5L·min-1flow of gas(pure N2gas,air or O2gas)was fed to the cathode. The solution was magnetically stirred and maintained at room temperature during the whole degradation reaction.Before degradation,the system was kept in the dark for30min to establish adsorption/desorption equilibrium between the solution and electrode in the cathodic cell.Analytical Methods.A UV-visible spectrophotometer(S-3100,Scinco)was used to monitor the concentration of RhB in water at its maximum absorption wavelength of555nm.The analysis of hydrogen peroxide was carried out using the UV-vis spectrum and off-line sampling.32The concentrations of copper ion(Cu2+and Cu+)in the solution were measured by atom absorption spectrometry(WFX-1F2,China).Cyclic voltammetry (CV)was performed on a computer-controlled CHI-660B electrochemical workstation in the cathodic cell with three electrodes,with Cu2O/CNTs/PTFE cathode as working elec-trode,an Ag/AgCl electrode(saturated with KCl)as reference electrode,and a platinum electrode as auxiliary electrode between-0.80and0V,respectively.The scan rate was50 mV/s.Results and DiscussionCharacterization of the As-Prepared Cu2O Nanocubes and the Cu2O/CNTs/PTFE Cathodes.The X-ray diffraction (XRD)was used to characterize the phase structure of both the as-prepared Cu2O sample and the Cu2O/CNTs/PTFE cathode (Figure1).Figure1a shows the XRD pattern of the as-prepared Cu2O.It was found that the pattern matched well with the standard cubic Cu2O pattern(JCPDS,file No.75-1531).The broadening of the XRD peaks reflects the nanocrystalline nature of the resulting Cu2O.According to Figure1a,cubic Cu2O is the only detectable crystalline phase,suggesting the high purity of Cu2O sample.Figure1b displays the XRD pattern of theas-prepared Cu2O/CNTs/PTFE cathode.The diffraction peaks at2θvalue of26.5°is ascribed to the(002)reflection of the CNTs(JCPDS,file No.74-444).33The diffraction peaks at2θvalue of18.1°belongs to the PTFE(JCPDS,file No.47-2217). The diffraction peaks at2θvalues of29.60°,36.55°,42.39°, and61.63°can be assigned to the reflection of the(110),(111), (200),and the(220)reflection of Cu2O nanocubes(JCPDSfile No.75-1531),respectively.These XRD results suggested that PTFE successfully combined Cu2O nanocubes together with CNTs in the resulting cathodes.Figure2shows the SEM images of the Cu2O sample and the prepared Cu2O/CNTs/PTFE cathode.It was found from Figure 2a that the Cu2O sample consisted of well-defined cubes of about 80nm in sizes.Figure2b reveals that the surface layer of the cathode isflat.Many macro or micropores were observed on the surface of the Cu2O/CNTs/PTFE cathodes,suggesting that the electrode could be easily penetrated by the electrolyte and gas components in the solution and provide plenty of sites for oxygen adsorption.Energy-dispersive X-ray analysis(EDX) reveals that carbon,copper,and oxygen elements coexist in the Cu2O/CNTs/PTFE cathodes(inset of Figure2b),which is in good agreement with the result of XRD.The TEM image of the Cu2O sample in Figure3reveals that the sizes of nanocubes range from80-100nm with narrow size distribution,which is consistent with the SEM observation.Degradation of RhB in the E-Fenton System Based on the Cu2O/CNTs/PTFE Cathode.Degradation of RhB in aqueous solution was used to test the efficiency of the E-Fenton system based on the Cu2O/CNTs/PTFE cathode in this study, because RhB was found to be stable at different pH values.In order to compare catalytic performance,the degradation of RhB was also carried out on blank PTFE cathode and CNTs/PTFE cathode without binding Cu2O nanocubes(Figure4).After120 min of reaction,no obvious RhB degradation was observed on both the blank CNTs cathode and the CNTs/PTFE cathode. However,80.2%of RhB were degraded on the Cu2O/CNTs/ PTFE cathodes at neutral pH.Therefore,the presence of Cu2O nanocubes is crucial for the proceeding of the E-Fenton reaction. The Cu2O nanocubes could serve as an effective heterogeneous Fenten reagent to catalytic produce•OH radicals.This reveal that the Cu2O/CNTs/PTFE cathode is an excellent cathode in E-Fenton system at neutral pH,which may be attributed to better diffusion conditions offered by the porous Cu2O/CNTs/PTFE cathode where two-dimensional electrochemistry is converted to“quasi-three-dimensional”behavior due to the large distrib-uted area.34The influence of the initial pH on the degradation efficiency of this new E-Fenton system was also investigated(Figure5). It was found that the catalytic ability of the Cu2O/CNTs/PTFE cathode was affected by pH value.After120min of reaction, the degradation ratio at neutral pH(80.2%)was slightly lower than that(89.3%)at pH3but higher than that(54.4%)at pH9. The highest degradation was obtained at pH3.This is because Cu2O nanocubes would be partially dissolved to form copper ions(Cu2+/Cu+)in solution to produce•OH radicals effectively. In addition,the degradation of RhB by this E-Fentonsystem Figure1.XRD patterns of(a)the as-prepared Cu2O nanocubes and (b)the as-prepared Cu2O/CNTs/PTFE cathode.Electro-Fenton Degradation of Rhodamine B J.Phys.Chem.C,Vol.112,No.31,200811931based on Cu 2O/CNTs/PTFE cathode was found to follow the pseudo-first-order decay kinetics (Figure 6).Figure 6sum-marized the pseudo-first-order constants (k )and the correspond-ing coefficients (R 2)of the degradation under different pH values.These results clearly revealed that the E-Fenton system based on the Cu 2O/CNTs/PTFE cathode can effectively work under pH ranging from the acid to the neutral.Fenton-like reaction could hardly happen because few copper ions would leach from the cathode to the bulk solution at a basic pH value.This accounts for the low degradation of RhB at pH 9.UV -vis spectra changes of the RhB dye solution as a function of reaction time can be used to clarify the changes ofmolecular and structural characteristics of RhB during E-Fenton oxidation at neutral pH (inset of Figure 5).The absorption spectrum of the RhB solution was characterized by its maximum absorption at 555nm in the visible region,which was attributed to the chromophore-containing azo linkage (conjugated xanthene ring)of the dye molecules.35The absorption peak at 555nm diminished with increasing E-Fenton reaction time,indicating that the rapid degradation of RhB was attributed to the decomposition of the conjugated xanthene ring in RhB.31This is reasonable because the N d N bond of the azo dye is a most active site for attack by ·OH radicals.36The role of gas bubbling onto the electrode in the degradation of RhB by this E-Fenton system based on the Cu 2O/CNTs/PTFE cathode was studied in this paper.We compared the degradation under either reactive (air,oxygen)or inert gas (nitrogen)conditions,their pseudofirst-order decay curves were fitted and the kinetic constants were calculated (Figure 7).Figure 7shows that RhB degradations under both O 2and air conditions are obviously more efficient than in N 2systems.The kinetic constants were 0.0193and 0.0130min -1under the O 2and air conditions,respectively,while a much smaller constant of 5.06×10-4min -1was observed under the N 2condition.Therefore,Figure 2.SEM image of the as-prepared (a)Cu 2O nanocubes and (b)Cu 2O/CNTs/PTFE cathode.The inset in panel b is the EDX pattern of Cu 2O/CNTs/PTFEcathode.Figure 3.TEM image of the as-prepared Cu 2Onanocubes.Figure 4.Degradation curves of RhB in E-Fenton systems with different cathodes at neutral pH under oxygenated condition withair.Figure 5.Degradation of RhB in the E-Fenton system based on the Cu 2O/CNTs/PTFE cathode at different pH under oxygenated condition with air.The inset is the UV -vis spectral changes of RhB with reaction time at neutral pH.11932J.Phys.Chem.C,Vol.112,No.31,2008Ai et al.the presence of more oxygen resulted in faster and more complete degradation of RhB.This is because oxygen plays an important role in the degradation,involving the reductive produce of H 2O 2according to eq 9.To understand high degradation efficiency of this E-Fenton process at neutral pH,the two main species involved in Fenton’s reactions,copper ions (Cu 2+/Cu +)and hydrogen peroxide (H 2O 2)were monitored (Figure 8).As shown in Figure 8a,the concentration of copper ions did not increase lineally with reaction time.After approximately 60min,the copper ions leaching from the electrode reached steady-state concentrations and remained almost constant between 17.25×10-5and 19.11×10-5M.This result suggests that the Cu 2O/CNTs/PTFE cathode is stable and can be reused.Figure 8b presents the concentration of H 2O 2electro-generated in the solution at neutral pH under 1.2V of the applied potential in the current two-electrode system (∆E )1.2V).As illustrated in Figure 8b,the H 2O 2concentration progressively grew during the first 30min and then reached a balance ranging from 1.27×10-5to 1.40×10-5M.These results indicate that the Cu 2O/CNTs/PTFE cathode is a favorable cathode for H 2O 2electro-generation.This phenomenon could be likely explained by the fact that the as-prepared Cu 2O/CNTs/PTFE cathode had numerous macro-ormicropores (Figure 2),so that O 2could easily be electro-reduced on the cathode surface to form H 2O 2substantially.Obviously,more H 2O 2results in more •OH radicals via Fenton reactions.Therefore,the simultaneous and effective formation of Cu n +and H 2O 2during the reaction is the reason for the high efficiency of this E-Fenton system with Cu 2O/CNTs/PTFE cathode under neutral pH.The stability of electrodes is a key issue for their practical application.We cleaned the used Cu 2O/CNTs/PTFE electrode with deionized water and then reused it for E-Fenton degradation of RhB under the same conditions.It is very interesting to find that there is no obvious decrease in degradation efficiency after several processes (Figure 9),indicating that the Cu 2O/CNTs/PTFE cathode is very stable and reusable.The reusability of the Cu 2O/CNTs/PTFE cathodes suggested it is promising for wastewater treatment.In order to further understand the oxidation and reduction reactions on the Cu 2O/CNTs/PTFE cathode in the E-Fenton process at neutral pH,cyclic voltammetric experiments were performed (Figure 10).Figure 10a shows the cyclic voltam-mograms of the Cu 2O/CNTs/PTFE cathode in the pure sup-porting electrolyte (0.05mol ·L -1of Na 2SO 4aqueous solution)at neutral pH under the deoxygenated (N 2)and oxygenated conditions (O 2or air).It was found that the peak at about -0.52V under the oxygenated condition with pure O 2was stronger than that under the oxygenated condition with air,while no obvious redox peak was found under the deoxygenatedconditionFigure 6.Pseudo-first-order degradation of RhB in the E-Fenton system with the Cu 2O/CNTs/PTFE cathode at different pH under oxygenated conditions with air as a function of reactiontime.Figure 7.Pseudo-first-order degradation of RhB in the E-Fenton system based on the Cu 2O/CNTs/PTFE cathode at neutral pH under different gas bubblingconditions.Figure 8.Concentration changes of copper ions (a)and concentration changes of hydrogen peroxide (b)as a function of the reaction time in the E-Fenton system with Cu 2O/CNTs/PTFE cathode at neutral pH under oxygenated condition with air.Electro-Fenton Degradation of Rhodamine B J.Phys.Chem.C,Vol.112,No.31,200811933with pure N 2,confirming the Cu 2O/CNTs/PTFE cathode was effective to adsorb and electrochemically reduce O 2to produce H 2O 2under oxygenated conditions.These results are consistent with the observations in Figure 7.Figure 10b is the typical cyclic voltammograms of the Cu 2O/CNTs/PTFE cathode in the 1.044×10-5M of RhB solution at neutral pH.Two anodic peaks appear at about -0.77and -0.36V,and two cathodic peaks at -0.65and -0.24V are also observed.One couple of peaks at ca.-0.77V in the cathode sweep and -0.65V in the anodic sweep were ascribed to the overall redox potentials of the O 2/H 2O 2couple,whereas the large reduction peak corresponds to the reduction of O 2.The difference between the peaks of -0.77and -0.65V is 0.12(≈2×0.059),suggesting a two-electron reversible redox reaction.Meanwhile,another couple of peaks at about -0.36and -0.24V were assigned to the redox potentials of Cu 2+/Cu.The difference of these two peaks also illustrates a two-electron reversible redox reaction.37All of these results reveal that Cu 2+and H 2O 2could be easily electro-produced and regenerated in this E-Fenton process based on the Cu 2O/CNTs/PTFE cathode.The produced two Fenton reagents (Cu 2+and H 2O 2)would further react together to produce hydroxyl radicals to degrade RhB effectively at neutral pH.ConclusionsIn summary,we prepared a composite Cu 2O/CNTs/PTFE cathode by combining Cu 2O nanocubes and multiwall carbon nanotubes with poly tetrafluoroethylene and developed a novel E-Fenton system with this oxygen-fed gas diffusion cathode.This E-Fenton system produced copper ions in situ from Cu 2O nanocubes and simultaneously electrochemically reduced oxygen into hydrogen peroxide.These two Fenton reagents further reacted together to produce hydroxyl radicals to degrade RhB effectively at neutral pH.Cyclic voltammetric experiments revealed that a two-electron reversible redox reaction happened in this new E-Fenton system.More importantly,the E-Fenton system with this Cu 2O/CNTs/PTFE cathode could efficiently degradation of RhB without losing activity after long-term run.The high efficiency and stability of this system makes it very promising for wastewater treatment.Acknowledgment.This work was supported by National Basic Research Program of China (973Program;Grant 2007CB613301),National Science Foundation of China (Grants 20503009,20673041,and 20777026),Program for New Century Excellent Talents in University (Grant NCET-07-0352),and the Key Project of Ministry of Education of China (Grant 108097),Outstanding Young Research Award of National Natural Science Foundation of China (Grant 50525619),Open Fund of Key Laboratory of Catalysis and Materials Science of the State Ethnic Affairs Commission &Ministry of Education,Hubei Province (Grant CHCL06012),and Postdoctors Foundation of China (Grant 20070410935).Supporting Information Available:The degradation curves of RhB in E-Fenton systems with Cu 2O/CNTs/PTFE cathodes with different mass ratios of CNTs:Cu 2O:PTFE at neutral pH.This material is available free of charge via the Internet at .References and Notes(1)Oturan,M.A.;Peiroten,J.;Chartrin,P.;Acher,A.J.En V iron.Sci.Technol.2000,34,3474.(2)Liu,H.;Wang,C.;Li,X.Z.;Xuan,X.;Jiang,C.;Cui,H.En V iron.Sci.Technol.2007,41,2937.(3)Vinu,A.;Sawant,D.P.;Ariga,K.;Hartmann,M.;Halligudi,S.B.Microporous Mesoporous Mater.2005,80,195.(4)Ventura,A.;Jacquet,G.;Bermond,A.;Camel,V.Water Res.2002,36,3517.(5)Lam,F.L.Y.;Yip,A.C.K.;Hu,X.Ind.Eng.Chem.Res.2007,46,3328.Figure 9.Stability of the Cu 2O/CNTs/PTFE cathode for degradation of RhB 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纳米纸作文开头50字
英文回答：
Nanoparticulate cellulose (NPC), a versatile nanomaterial derived from renewable sources, has emerged as a promising constituent for the fabrication of advanced materials and devices. Its unique properties, including high specific surface area, mechanical strength, biodegradability, and optical transparency, render it suitable for a wide range of applications, such as energy storage, electronics, sensing, and healthcare. Among the various NPC-based materials, nanocellulose paper (NCP) stands out as a remarkable substrate with exceptional properties that enable its utilization in diverse fields.
中文回答：
纳米纸作为一种新兴材料，因其优良的性能和广泛的应用前景而备受关注。

它是由可再生资源制备而成，具有高比表面积、高机械强度、可生物降解和良好的透光性等特性。

与其他纳米纤维素基
材料相比，纳米纸是一种独特的基材，其出色的性能使其在能源储存、电子、传感和医疗保健等领域具有巨大的应用潜力。

第53卷第6期表面技术2024年3月SURFACE TECHNOLOGY·1·研究综述极地航行船舶防覆冰涂层研究进展张祎轩1，刘涛2，刘耀虎3，刘杰1*，王健君4（1.中国科学院化学研究所，北京 100190；2.上海海事大学，上海 201306；3.中国科学院 前沿科学与教育局，北京 100864；4.中国科学院理化技术研究所，北京 100190）摘要：两极地区是未来重要的能源和资源基地。

然而，极地长年低温多冰，极大限制了我国对两极地区的科学考察、商业航运和能源开发进程。

因此，发展长效稳定的防覆冰技术是推进极地发展战略的关键。

系统阐明了船舶在极地航行过程中面临的结冰困境，分析了船舶积冰的类型，总结了目前解决船舶覆冰问题的多种防除冰技术及发展现状，包括主动防除冰技术（机械除冰、超声导波除冰、加热除冰、化学熔融除冰等）和被动防覆冰涂层技术（气体润滑防覆冰涂层、液体润滑防覆冰涂层、“类液体”润滑防覆冰涂层、界面可控断裂防覆冰涂层等），同时对各技术在极地船舶防冰应用中的优缺点和可行性进行了深入分析。

展望了船舶装备对特种防冰涂层的关键需求，提出主、被动协同除冰技术是实现极地船舶防覆冰的重要策略。

关键词：极地；船舶；防冰；涂层材料；冰黏附中图分类号：TQ050.4 文献标志码：A 文章编号：1001-3660(2024)06-0001-10DOI：10.16490/ki.issn.1001-3660.2024.06.001Research Progress on Anti-icing Coatings for Polar ShipsZHANG Yixuan1, LIU Tao2, LIU Yaohu3, LIU Jie1*, WANG Jianjun4(1. Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190, China; 2. Shanghai Maritime University,Shanghai 201306, China; 3. Bureau of Frontier Sciences and Education, Chinese Academy of Sciences, Beijing 100864, China; 4. Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100190, China)ABSTRACT: The polar regions are strategically important for the sustainable development of the global economy due to their abundant natural resources and special geographical location. However, the prolonged low temperature and heavy icing in the polar regions have greatly restricted the process of scientific research, commercial shipping, and energy development. Therefore, the icing problem of various types of equipment has become a hot topic of research and the development of long-lasting and stable anti-icing technology is crucial to advancing the polar development strategy.The icing dilemma faced by ships during polar navigation was systematically expounded. Types of ice accretion on ships were analyzed according to the origin of ice. Various anti-icing technologies were summarized, including active anti-icing technologies (mechanical de-icing, ultrasonic de-icing, heating de-icing, chemical de-icing, etc.) and passive anti-icing coating technologies (gas lubrication, liquid lubrication, "liquid-like" lubrication, interface-controlled fracture, etc.).The gas lubrication is mainly composed of micro/nanocomposite structure in the surface and low surface energy hydrophobic layer, which effectively inhibits the icing process by reducing the attachment of water droplets. However, the收稿日期：2023-03-29；修订日期：2023-10-23Received：2023-03-29；Revised：2023-10-23基金项目：国家自然科学基金面上项目（52273220）Fund：National Natural Science Foundation of China (52273220)引文格式：张祎轩, 刘涛, 刘耀虎, 等. 极地航行船舶防覆冰涂层研究进展[J]. 表面技术, 2024, 53(6): 1-10.ZHANG Yixuan, LIU Tao, LIU Yaohu, et al. Research Progress on Anti-icing Coatings for Polar Ships[J]. Surface Technology, 2024, 53(6): 1-10.*通信作者（Corresponding author）·2·表面技术 2024年3月disadvantage of it is liquid generally slipping into a hierarchical scale and adhering to the surface, resulting in the Cassie-Baxter state converting into the Wenzel state. Water freezing in the Wenzel state will cause mechanical interlocking forces and invalid deicing capabilities. Subsequently, the surface can be worn away after repeatedly de-icing. Although certain special structures have been proven to reduce the transition to the Wenzel state, the complex fabrication process is almost impossible to cover on a large scale. Liquid lubrication and "liquid-like" lubrication can greatly reduce the adhesion strength of ice on the solid surface by effectively reducing the strong physical interaction between ice and surface. Liquid lubrication is built through the overfilling lubricating liquid to the micro/nanopores substrate. Despite adhering within the substrate, lubrication becomes invalid over time by evaporation, erosion, and is contaminated. "Liquid-like" lubrication, covalently attached on one end of a flexible macromolecule onto a smooth substrate, determines the lubricating property. The high mobility and small intermolecular force of polymer enable it to function as a lubricating layer. "Liquid-like" lubrication has been considered a promising coating for its extreme uniformity, low adhesion, transparency, and safety. Interface-controlled fracture makes the crack nucleation and growth at the specific position of the interface quickly, accelerates the interface fracture process, and then makes the ice desorb quickly under the action of low shear stress. Under the action of shear stress, the interface between ice and substrate is not uniform, and macroscopic cracks are preferentially generated in the low shear modulus region. The cracks propagate rapidly, making the ice easier to break away from the substrate surface. The current development of anti-icing technologies in solving the icing problem is summarized. The feasibility of each technology to be applied in polar ships is discussed in depth according to their advantages and disadvantages.In the last section, the work emphasizes the key requirements for special anti-icing coatings for ship equipment, and the importance of active and passive cooperative de-icing strategies in polar ship protection technology is proposed.KEY WORDS: polar; ships; anti-icing; coating materials; ice adhesion极地地区具备丰富的自然资源和特殊的地理位置，对全球经济的可持续发展具有重要的战略意义。

Mn-Si金属间化合物多孔材料的制备李文浩;贺跃辉;康建刚【摘要】以Mn、Si元素粉末为原料,用反应合成方法制备Mn-Si金属间化合物多孔材料,表征各烧结温度所对应的孔结构、膨胀率和微观形貌,研究烧结过程中孔隙产生的机理.结果表明:在Mn-Si金属间化合物多孔材料的制备过程中烧结体发生明显的体积膨胀,烧结温度在800℃之前时膨胀率和开孔隙率随着温度的升高不断增大,800℃以后,膨胀率和开孔隙率均呈下降趋势;在最终烧结温度1040℃下得到开孔隙率为47.60％、平均孔径为11.97μm、孔结构均匀的多孔材料.探讨多孔材料的造孔机理,主要为压制孔隙的演变,成型剂的脱除,以及Mn元素和Si元素在扩散反应中不同扩散速度引起的Kirkendall效应.【期刊名称】《中国有色金属学报》【年(卷),期】2018(028)009【总页数】8页(P1791-1798)【关键词】Mn-Si;多孔材料;金属间化合物;造孔机理【作者】李文浩;贺跃辉;康建刚【作者单位】中南大学粉末冶金国家重点实验室,长沙 410083;中南大学粉末冶金国家重点实验室,长沙 410083;中南大学粉末冶金国家重点实验室,长沙 410083【正文语种】中文【中图分类】TG145多孔材料由于其特殊的孔结构，有着高的比表面积、高透过率、以及良好的吸附性等优良性能。

目前多孔材料已广泛应用在生物、医药、化工、冶金、环境保护等领域[1−4]。

多孔材料按材料类型主要可以分为两类，有机多孔材料和无机多孔材料，无机多孔材料又可分为陶瓷多孔材料和金属多孔材料[5]。

有机多孔材料不能适应高温高压的工作环境，不耐有机溶剂，使用环境受到较大的局限，一般仅用于工作条件较柔和的场合[6]。

金属多孔材料有着良好的力学性能和抗热震性能，以及较好的机械加工性能和焊接性能，易于实现工件的复杂形状以及加工和组装。

但由于金属的特性，金属多孔材料往往不耐酸碱，且在高温下易氧化。

不能适应强酸碱性的工况[7]。

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fabrication英语解释-回复Fabrication, in its broadest sense, refers to the process of making or creating something, usually through the manipulation or combination of materials, components, or ideas. It can be applied to various fields and industries, such as manufacturing, engineering, and even storytelling. In this article, we will explore the concept of fabrication and delve into its different aspects and applications.At its core, fabrication involves transforming raw materials into finished products or creating something entirely new. In the manufacturing industry, this process often entails cutting, shaping, and assembling various components to create a final product. For example, in the automotive industry, fabrication includes the manufacturing of car bodies, engine components, and other mechanical parts. In these cases, fabrication requires expertise in using specialized machinery, precision tools, and technical knowledge to ensure the quality and functionality of the final product.Similarly, fabrication plays a significant role in engineering. Engineers may fabricate prototypes or custom parts to test andvalidate their designs before mass production. This allows them to identify any potential flaws or improvements in their designs, reducing the risks and costs associated with mass production. This process often involves computer-aided design (CAD) software and the use of advanced machinery, such as 3D printers or CNC (Computer Numerical Control) machines, to accurately fabricate complex shapes and intricate details.While fabrication is commonly associated with physical manufacturing processes, it also extends to the realm of ideas and storytelling. In literature and the arts, fabrication refers to the creation of fictional narratives or fictionalized accounts of real events. Writers and storytellers often fabricate characters, plotlines, and settings to entertain or convey specific messages to their audiences. This form of fabrication allows for creativity and imagination to shape unique stories that can captivate readers and evoke emotions.In the digital age, fabrication has taken on a new dimension through the emergence of virtual reality (VR) and augmented reality (AR). These technologies allow for the fabrication of immersive virtual environments or the overlaying of digitalinformation onto the real world, blurring the lines between what is real and what is fabricated. Artists and developers can now create digital artworks, interactive experiences, and simulations that offer a new level of creativity and engagement.Furthermore, fabrication has also found its way into the field of medicine and healthcare. Medical professionals use fabrication techniques to create customized prosthetics, orthotics, and even human tissues or organs through techniques like 3D bioprinting. This form of fabrication enables personalized and precise medical interventions, offering patients enhanced functionality and quality of life.In conclusion, fabrication encompasses the process of creating or making something, whether it involves manipulating physical materials, designing virtual worlds, or fabricating narratives. It is a versatile concept that applies to various fields, such as manufacturing, engineering, arts, and even healthcare. As technology continues to advance, the possibilities for fabrication are expanding, allowing for unprecedented levels of creativity,customization, and innovation.。

TFN膜纳米材料的选择及其在水处理中的应用摘要当下水危机愈发严重，掺杂纳米材料制备成的薄膜纳米复合材料（TFN）膜，有望缓解传统薄膜复合材料（TFC）膜的缺陷。

本文对无机、有机和复合纳米材料进行了比较，简述了不同尺寸、形状纳米材料的特点，回顾了TFN膜在水处理过程中的表现。

希望可为研究人员制造TFN膜提供见解。

关键词：TFN膜；纳米材料；水处理引言在微孔支撑基底沉积形成薄的聚酰胺选择层（PA层）的膜称为TFC膜。

TFN膜是指将纳米级材料应用到基膜或者PA层的表面或内部。

纳米材料在分离膜中的作用主要有：（1）借助纳米材料内部的尺寸通道过滤水[1]；（2）改变膜的亲/疏水性；（3）一定程度上干扰PA层聚合物的形成，使PA层结构更疏松[2]；（4）引入一些功能官能团[3]。

本文主要对TFN膜中纳米材料的类别及特性进行了相关阐述，并介绍了当前TFN膜在水处理中的应用概况。

1纳米材料的选择及对膜性能的影响1.1 纳米材料的种类1.1.1 无机纳米材料利用无机纳米材料的掺杂制备而成的TFN膜，常可以显著改变膜表面荷电性、抗菌性[4]、亲疏水性和选择性等。

常用的无机纳米材料有：二氧化钛、二氧化硅、石墨烯和氧化石墨烯（GO）等。

Shao等人[5]通过化学键和物理吸附作用，在PA层表面上的逐层自组装TiO和GO，当接枝层数等于6时效果最好。

2但仅靠物理作用进行掺杂的机纳米材料容易浸出或脱落[6]，还容易在膜内发生局部聚集。

1.1.2 有机纳米颗粒有机物之间常具有良好的相容性，界面聚合时可以通过化学键进行交联。

有机材料与PA层的交联往往比无机材料更紧密，Wang等人[7]在制模过程中，分别利用相同尺寸的有机材料氨基苯酚/甲醛树脂聚合物纳米球（APFNSs）与其完全碳化后的无机产物氮掺杂纳米球（N-CNSs）进行掺杂，有机的APFNSs能与均苯三甲酰氯（TMC）形成稳定的酰胺键，使其与PA层聚合更加紧密，而无机的N-CNS无法扩散到PA层中，只能留在PA层底部的支撑或半嵌入。