Retarded Charge Recombination in Dye-Sensitized Nitrogen-Doped TiO2 Solar Cells

Retarded Charge Recombination in Dye-Sensitized Nitrogen-Doped TiO2Solar Cells Huajun Tian,Linhua Hu,Changneng Zhang,Weiqing Liu,Yang Huang,Lie Mo,Lei Guo,

Jiang Sheng,and Songyuan Dai*

Key Laboratory of No V el Thin Film Solar Cells,Institute of Plasma Physics,Chinese Academy of Sciences,

P.O.Box1126,Hefei,Anhui230031,PR China

Recei V ed:October30,2009;Re V ised Manuscript Recei V ed:December14,2009

In this paper,the photovoltaic performance and charge recombination of the dye-sensitized solar cells(DSCs)

based on nitrogen-doped TiO2electrodes were investigated in detail.A negative shift of the?atband potential

(V fb)of nitrogen-doped TiO2?lm was attributed to the formation of an O-Ti-N bond,and it was indicated

that the position of the edge of the V fb is shifted to negative,resulting in the improvement of the open circuit

voltage for DSC with nitrogen doping.The UV-vis spectrum of the nitrogen-doped?lm exhibited a visible

absorption in the wavelength range from400to500nm.The back electron transfer of the nitrogen-doped

DSC was studied by measuring the electrochemistry impedance spectra(EIS),and the EIS for DSCs showed

that the enhanced electron lifetime for nitrogen-doped TiO2solar cells could be attributed to the formation of

O-Ti-N in the TiO2electrode to retard the recombination reaction at the TiO2photoelectrode/electrolyte

interface as compared to the undoped TiO2solar cells.The photovoltaic performance of the DSC under high

temperature conditions and one soaking in sun light for more than1000h indicated that the nitrogen-doped

TiO2solar cells exhibited better stability.It indicated that the formation of O-Ti-N in the TiO2electrode

in?uences the performance of the DSC.Especially,the introduction of nitrogen into the DSC can stabilize

the DSC system due to the replacement of oxygen-de?cient titania by nitrogen-doped TiO2.

1.Introduction

Dye-sensitized solar cells(DSCs)based on nanoporous TiO2 electrodes have received much attention for the development of low-cost,high-ef?ciency solar energy conversion.1-8Under light irradiation,the sensitizers become photoexcited and rapidly inject electrons into the TiO2conduction band.The oxidized sensitizer is effectively scavenged by the redox system,which itself is regenerated at the counter electrode by passing electrons through the external load.The injected conduction-band elec-trons can recombine with oxidized dye molecules or react with redox species in electrolyte.Many methods for retarding the charge recombination of DSC have been attempted such as the use of some novel dyes,9core-shell structure,10,11and doping nonmetal to improve the performance of DSCs.12

As one crucial component in DSCs,the nanostructure TiO2 electrode has some oxygen de?ciency in the crystal structure.13-15The oxygen de?ciency could create electron-hole pairs.The oxidizing holes can react with the dye or be scavenged by iodide ions.16Those de?ciencies result in shortening the lifetime of the DSC,and doping nitrogen into the TiO2crystal structure can just perfect the oxygen de?ciency and decrease the back reaction mentioned above. Since2001,Asahi et al.reported that improved photocatalytic acting of TiO2under visible irradiation can be achieved by nitrogen doping,and much research about nitrogen doping in TiO2?lm has been investigated extensively.17-19Recently, research about nitrogen-doped TiO2electrodes,especially that reported by Ma et al.,has obtained some achievements,12 but there is no detailed study about the charge recombination of DSCs based on nitrogen-doped TiO2electrodes.

In this paper,a simple and useful technology of preparing nitrogen-doped TiO2pastes based on a modi?ed sol-gel method is introduced,and the mechanism of charge recombination of DSCs based on nitrogen-doped TiO2electrodes is discussed in detail.The photovoltaic performance and photostability of a DSC after the addition of nitrogen into the TiO2electrode is also researched.

2.Experimental Section

2.1.Synthesis of Nitrogen-Doped Nanoporous TiO2.Ni-trogen-doped TiO2material was synthesized via a modi?ed sol-gel method using urea as the nitrogen source.An appropri-ate mount of urea was dissolved in90mL of deionized water prior to hydrolysis of titanium isopropoxide(Fluka)under vigorous stirring.Titanium isopropoxide(50mL,Fluka)was added dropwise to the prepared solution containing urea.The whole procedure is slow under vigorous stirring.The formed precipitate solution was stirred vigorously for2-3h,and then stirred for8-15h at80°C to form transparent sol and heated at200°C in an autoclave for10h to obtain gelatin.The remaining procedures were the same as those described in ref20.

2.2.Fabrication of Dye-Sensitized TiO2Photoanode and DSC Assembly.Nanocrystalline TiO2?lms were fabricated by a screen-printing technique.The TiO2(nitrogen-doped and undoped TiO2)pastes were deposited on the conducting glass substrates(F-doped SnO2),followed by sintering at450°C for 30min.The thicknesses of the three different?lms were18, 17.7,and19.4μm,respectively,which was determined by a pro?lometer(XP-2,AMBIOS Technology,Inc.,USA).After being cooled to120°C,the?lms were immersed into an ethanol solution(0.5mM)of dye N719[cis-dithiocyanate-N,N′-bis-(4-carboxylate-4′-tetrabutylamonium-carboxylate-2,2′-ipyridine)ru-thenium(II)].The counter electrode was platinized by spraying

*Corresponding author.Tel:+86-551-5591377.Fax:+86-551-5591377.

E-mail:sydai@https://www.sodocs.net/doc/599027012.html,.

J.Phys.Chem.C2010,114,1627–16321627

10.1021/jp9103646 2010American Chemical Society

Published on Web01/05/2010

H 2PtCl 6solution onto transparent conductive oxide (TCO)glass and ?red in air at 410°C for 20min.The platinized counter electrode was placed directly on the top of the dyed TiO 2?lm sealed with thermal adhesive ?lms (Surlyn,Dupont).And the electrolyte was ?lled from a hole made on the counter electrode,which was later sealed by a cover glass and thermal adhesive ?lms.The electrolyte consists of anhydrous lithium iodide,iodine,3-methoxypropionitrile (MePN)purchased from Fluka,and 1,2-dimethyl-3-propylimidazolium iodide (DMPII),meth-ylbenzimidazole (MBI)obtained from Aldrich.3.Characterization

The crystallite size of nitrogen-doped TiO 2and the electrode microstructure were studied using a ?eld emission scanning electron microscope (FE-SEM,sirion200,FEI Corp).The crystallinity of the nitrogen-doped TiO 2?lm was determined using X-ray diffraction analysis (XRD,MXPAHF,Mark Corp.,Japan)measurement with Cu K R (γ)0.1541nm).The crystallite size D was calculated by the Sherrer equation.The substitution of the oxygen sites with nitrogen atoms in the titania structure was con?rmed by X-ray photoelectron spectroscopy (XPS,Thermo Electron Corp.,US).The UV -visible (UV -vis)absorption spectra were obtained from a UV -vis spectropho-tometer (TU-1901,PGeneral Instrument Inc.,China).The ?atband potential (V fb )of the nanostructure TiO 2electrode was performed by measuring absorbance at 780nm as a function of the applied potential.The optical absorption comes from intraband transitions or from free carrier absorption,and the absorbance in the experiment is proportional to the density of electrons in the conduction band.21For spectroscopic electro-chemistry measurement,a 4μm-thick TiO 2?lm formed the working electrode (2cm 2surface area)of a three-electrode photoelectrochemical cell employing a platinum wire counter

electrode and a Ag/AgCl reference electrode.Potential control was carried out on a CHI 660A potentiostat,and the applied potential was scanned at 5mV/s.A 780nm monochromatic light source was obtained from a UV -vis spectrophotometer (TU-1901,PGeneral Instrument Inc.,China).For each deter-mination of V fb ,a new working electrode and freshly prepared electrolyte solution were used.The photovoltaic performance,including short-circuit current (I sc ),open-circuit voltage (V oc ),?ll factor (FF),and energy conversion ef?ciency (η)of the DSC was measured with a Keithley model 2420digital source meter controlled by Test point software under a xenon lamp (100mW/cm 2;uniform illumination is less than 3%in an active area of 30cm ×30cm,Changchun Institute of Optics Fine Mechanic and Physics,Chinese Academy of Sciences)and calibrated with a standard crystalline silicon solar cell (the 18th Research Institute of Electronics Industry Ministry,China).Linear sweep voltammeter (LSV)curves of the DSCs were performed to obtain the dark current with an electrochemical workstation (CHI660A,CH Instruments,Inc.,USA).Impedance measure-ments were carried out with an IM6ex electrochemical worksta-tion (Zahner-Elektrick,Germany)in the frequency range of 20mHz to 1000kHz at room temperature.The working electrode was a dyed TiO 2electrode of DSC,and the auxiliary electrode,and the reference electrode was a platinized counter electrode of DSC.The amplitude of the alternative signal was 5mV.4.Results and Discussion

Nitrogen-doped TiO 2materials prepared by modi?ed sol -gel method using urea as the nitrogen carrier display a pale yellow color and are characterized by various spectroscopic features.The FE-SEM micrographs of the TiO 2electrodes with the corresponding undoped and nitrogen-doped material are shown in Figure 1a,b,respectively.Highly porous nanostructure

could

Figure 1.FE-SEM micrographs of the undoped and nitrogen-doped titania ?lms:(a,c)undoped titania ?lm;(b,d)nitrogen-doped titania ?lm.

1628J.Phys.Chem.C,Vol.114,No.3,2010Tian et al.

be observed for both the thin?lms from the FE-SEM micro-graphs.In Figure1b,d,the average particle size of a nitrogen-doped TiO2nanoparticle is about25nm.The micrographs of the nitrogen-doped TiO2nanoparticles using urea as the nitrogen source and the undoped TiO2nanoparticles indicated that the addition of the urea prior to hydrolysis of titanium isopropoxide has no obvious in?uence on the titania crystallite size compared to the undoped titania.

The XRD spectrum of the nitrogen-doped titania powder is shown in Figure2,which shows that the crystal phases of the nitrogen-doped titania and undoped titania powder were anatase. Additionally,their average crystallite sizes calculated from the broadening of the(101)XRD peak of the anatase phase were 19.1and17.6nm,respectively.From the XRD data,it can be seen that there is a little shift in the(101)peak positions for nitrogen-doped TiO2,as reported in Jagadale’s work on N-doped TiO2by the sol-gel method.22

In particular,the substitution of oxygen sites with nitrogen atoms in the titania structure was con?rmed by XPS.The binding energy peak of N1s for the nitrogen-doped TiO2in Figure3shows that two XPS peaks at about399.6and401.7 eV were observed.These lie in the range(396-404eV) observed by other authors,23-27and are typical of nitrogen-doped titanium dioxide.In most cases,a peak at396eV was detected and attributed to binding energy in Ti-N.28However,in some recent papers,the feature of396eV was completely absent,and peaks at higher binding energies(396-404eV)were observed.23-27Burda et al.indicated that,when nitrogen is substituted for the oxygen in the initial O-Ti-O structure,the electron density around N is reduced,and the N1s binding energy in an O-Ti-N is higher than that in an N-Ti-N environment.26Therefore,the peak at399eV indicated that the nitrogen-doped titania probably has an O-Ti-N structure.22,26 Di Valentin et al.indicated that preparation methods and conditions largely affected nitrogen XPS spectral features.29In the case of the sample described here and prepared via sol-gel, peaks at396eV were never observed.In summary,the signals at399.6and401.7eV observed should be attributed to the O-Ti-N structure and the molecular adsorbed nitrogen species, respectively.

The observed XPS peak for the Ti2p in Figure4a showed signi?cant change upon nitrogen https://www.sodocs.net/doc/599027012.html,pared with the binding energy of undoped TiO2(458.8eV for Ti2p),the binding energy of Ti2p(458.4eV)decreases after nitrogen doping.This suggested that the nitrogen incorporates into the TiO2lattice and substitutes for oxygen.26The O1s XPS spectra in Figure4b also showed signi?cant changes upon nitrogen incorporation.O1s peak at530.1comes from Ti-O-Ti linkages in TiO2,and the undoped sample shows an O1s peak at530.1 eV,versus a shift to529.6eV,which is observed for nitrogen-doped samples.

The UV-vis absorption spectra of undoped TiO2and N-doped TiO2?lms are shown in https://www.sodocs.net/doc/599027012.html,pared with the spectra of undoped TiO2?lm,N-doped TiO2?lm presents a signi?cant absorption in the visible region between400and500 nm,which is the typical absorption feature of N-doped TiO2. In addition,the V fb of TiO2electrodes were studied in this work. It is considered that the presence of O-Ti-N structure in TiO2 could in?uence the performance of the TiO2photoelectrode,and then in?uence the photovoltaic performance of DSC.The V fb of a TiO2electrode can be determined by the absorption spectroscopic method used by Redmond.21The potential was scanned at5mV/s.V fb is considered as the potential from which the two traces begin to depart from each other.Figure6

shows Figure4.Ti2p(a)and O1s(b)XPS spectrum of nitrogen-doped and undoped titania

powder.

Figure2.XRD for nitrogen-doped and undoped titania

powder.

Figure3.N1s XPS spectrum of nitrogen-doped titania

powder.

Figure 5.UV-visible absorption spectra of nitrogen-doped and

undoped titania?lms.

Charge Recombination in Nitrogen-Doped TiO2DSCs J.Phys.Chem.C,Vol.114,No.3,20101629

that V fb shifts to the negative by 0.06and 0.1eV compared with that in the absence of nitrogen TiO 2electrode.

Figure 7shows the current -voltage curves of the DSC based on the nitrogen-doped and undoped TiO 2photoelectrodes.The performance properties of DSCs are summarized in Table 1.In Table 1,it is apparent that V oc and FF shift to the higher values with the concentration of urea increasing.The maximal V oc is found to be 752mV,increasing by 3.8%compared with the minimum V oc of 724mV.Furthermore,the FF increased by 5.2%relative to that of the undoped one.While the J sc and ηdecrease with the increasing quantity of nitrogen source,the V oc increases in the presence of nitrogen compared with that in the absence of nitrogen,which may be explained by the V fb of the TiO 2photoelectrode (Figure 6).Under Fermi level pinning,these two parameters are linked by eq 1.30

where V red is the standard reduction potential of a redox couple,assuming that V red does not vary with the addition of nitrogen.It is expected that V oc should change with V fb ,but the data in Figure 6indicated that V fb shifts to the negative direction appreciably.So the increase of V oc of DSC should be attributed mostly to the addition of the nitrogen into the TiO 2,retarding the dark current shown in Figure 8or to the decrease of the charge recombination.In addition,the addition of the nitrogen into the TiO 2increases the V fb ,and reduces the difference between the higher quasi-Fermi level and the lowest unoccupied molecular orbital (LUMO)of N719dye,which results in the

weakening of the driving force for the photoelectron injecting from the dye excited state into the conduction band of TiO 2,and the increase of the titania crystallite size also in?uences the dye N719absorption of TiO 2?lm.This could explain why the short-circuit photocurrent density J sc decreases appreciably.It is well-known that charge recombination is still one of the most limiting factors for DSC performance.The addition of nitrogen into the titania can suppress the production of dark current.The results are shown in Figure 8.It is known that when a negative potential is applied between the photoanode and counter electrode,the electrons transfer under the electric ?eld force and also are trapped by different recombination pathways.By comparison of doped DSCs and bare DSCs,it illustrates that nitrogen-doped DSCs exhibit smaller dark current,which indicates that nitrogen doping could successfully retard the charge recombination at the TiO 2/dye/electrolyte interface.Thus,the nitrogen-doped titania-introduced formation of O -Ti -N structure can suppress the reduction of I 3-on the TiO 2electrode.In addition,the resistance to the back electron transfer was characterized by measuring the impedance spectra (Figure 9).The equivalent circuit model of DSC is shown as in Figure 10.If the back electron transfer is suppressed,V oc and FF can be improved.In Figure 9,three arcs are distinguished in

the

Figure 6.Absorbance measured at 780nm as a function of applied potential for a nanostructured undoped and nitrogen-doped TiO 2elec-

trode.

Figure 7.Current -voltage curves of DSCs based on nitrogen-doped and undoped TiO 2electrodes.

TABLE 1:Performance Characteristics of DSCs Based on Nitrogen-Doped and Undoped Titania Electrodes

DSC

V oc (mV)J sc (mA/cm 2)FF (%)η(%)undoped

72412.061.5 5.34nitrogen-doped (TiO2:Urea )1:0.5)74511.062.3 5.10nitrogen-doped (TiO2:Urea )1:1)

752

10.1

64.7

4.90

V oc )|V fb -V red |

(1)

Figure 8.LSV curves of nitrogen-doped DSCs and bare DSCs in the

dark.

Figure 9.Nyquist plots and Bode plots for DSC based on undoped and nitrogen-doped TiO 2photoanodes,measured at a forward bias of -0.71V in the dark.The lines show the ?tted results in Nyquist plots.

1630J.Phys.Chem.C,Vol.114,No.3,2010Tian et al.

frequency regime of 103-105(ω1/ω2),1-103(ω3)and 0.1-1Hz (ω4),from left to right.These arcs are assigned to resistances at the conducting layer/TiO 2(ω1),Pt/electrolyte (ω2),and TiO 2/dye/electrolyte (ω3)interface and diffusion of the I 3s /I s redox electrolyte (ω4).31

In Figure 9,it is noted that the doping of nitrogen into the TiO 2increased the impedance component corresponding to ω3.The increase in the resistance at the TiO 2/dye/electrolyte interface is as much as 10%,while the change in other impedance components was negligible.The increase in the resistance of ω3indicated that the addition of nitrogen increases the surface resistance of TiO 2photoelctrodes and suppresses the back transfer of photogenerated electrons from nitrogen-doped TiO 2nanoparticles to the electrolyte at TiO 2/dye/electrolyte (ω3)interface.

In the Bode plots,it can be seen that the addition of nitrogen into the TiO 2shifts the midfrequency peak to lower frequencies,increasing at the same time its amplitude,as seen in Figure 9.The result of the midfrequency peak shifts to lower frequencies,corresponding to an increase of the electron lifetime calculated from the 32.7to 44.5ms.It con?rms that the nitrogen doping into the TiO 2photoanode can improve the performance of DSC.The effect of Xe-light and high-temperature (70°C)aging on the performance of nitrogen-doped and undoped TiO 2photoanode DSCs is shown in Figure 11.However,high temperature in?uences device performance.The FF of the N-doped DSC could nearly keep its initial value,and the V oc also could retain nearly 90%.Compared with the undoped DSC,

the J sc of the nitrogen-doped DSC can remain nearly unchanged.It is well-known that the oxidizing holes created by oxygen de?ciency,which exists in pure TiO 2,can react with the dye,and the doping nitrogen could replace the oxygen de?ciency.12So the excellent performance J sc of DSC could be explained by the fact that the doping nitrogen in the TiO 2photoanode could retard the dye degradation,attributing to the formation of O -Ti -N in TiO 2.Additionally,the ηof the nitrogen-doped DSC remained at nearly 80%compared with the 72%of the undoped DSC under high temperature (70°C)conditions after over 1000h.It can be seen that the formation of O -Ti -N in the TiO 2electrode in?uences the performance of the DSC.Especially,the introduction of nitrogen into the DSC can stabilize the DSC system as a result of the replacement of oxygen-de?cient titania by nitrogen-doped titania.Research on the improved ef?ciency of nitrogen-doped DSCs is in progress.5.Conclusions

In this paper,the charge recombination in dye-sensitized TiO 2solar cells based on nitrogen-doped TiO 2photoanodes was investigated.Nitrogen-doped TiO 2thin ?lms were prepared with a modi?ed sol -gel process in order to develop a simple and novel method for preparing a nitrogen-doped TiO 2photoanode of DSC.The TiO 2photoanode with nitrogen doping could successfully retard the charge recombination,and the introduc-tion of nitrogen replaced the oxygen de?ciency in the titania crystal lattice.The enhanced electron lifetime for doped TiO 2solar cells could be attributed to the formation of O -Ti -N in the TiO 2electrode to retard the recombination reaction at the TiO 2photoelectrode/electrolyte interface,as compared to the undoped TiO 2solar cells.Additionally,the V fb of TiO 2is also affected slightly by the presence of the doping nitrogen.As a result,the position of the edge of the V fb is shifted to the negative direction as the content of urea addition increases.During the stability test under one sun light soaking and a high temperature condition (70°C)for more than 1000h,the DSC based on the nitrogen-doped TiO 2photoanode is more stable.Other methods of preparing a nitrogen-doped TiO 2photoanode of DSC are still being researched.

Acknowledgment.This work was ?nancially supported by the National Basic Research Program of China under Grant No.2006CB202600,the National High Technology Research and Development Program of China under Grant No.2009AA050603,and Funds of the Chinese Academy of Sciences for Key Topics in Innovation Engineering under Grant No.KGCX2-YW-326.References and Notes

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Charge Recombination in Nitrogen-Doped TiO 2DSCs J.Phys.Chem.C,Vol.114,No.3,20101631

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简单的四则运算计算器程序

简单的四则运算计算器程序

注：1、报告内的项目或内容设置，可根据实际情况加以调整和补充。 2、教师批改学生实验报告时间应在学生提交实验报告时间后10日内。

附件：程序源代码 // sizheyunsuan.cpp : Defines the entry point for the console application. #include #include const int MAX=100; class Operand{ private: double operS; public: Operand(){} Operand(double opers){ operS=opers; } void set(double opers){ operS=opers; } double get() { return operS;} }; class Operator{ private: char operF; int priority; public: Operator(){} Operator(char operf) { operF=operf; switch(operf) { case'(':priority=-1;break; case'+':priority=0;break; case'-':priority=0;break; case'*':priority=1;break; case'/':priority=1;break; case')':priority=2;break; } } void set(char operf){ operF=operf; } char get(){ return operF;} int getpriority(){ return priority; } };

一元函数微分学习题

第二部分 一元函数微分学 [选择题] 容易题 1—39，中等题40—106，难题107—135。 1．设函数)(x f y =在点0x 处可导，)()(00x f h x f y -+=?，则当0→h 时，必有( ) (A) y d 是h 的同价无穷小量. (B) y y d -?是h 的同阶无穷小量。 (C) y d 是比h 高阶的无穷小量. (D) y y d -?是比h 高阶的无穷小量. 答D 2．已知)(x f 是定义在),(+∞-∞上的一个偶函数，且当0'x f x f ， 则在),0(+∞内有（ ） （A ）0)(,0)(<''>'x f x f 。 （B ）0)(,0)(>''>'x f x f 。 （C ）0)(,0)(<''<'x f x f 。 （D ）0)(,0)(>''<'x f x f 。 答C 3．已知)(x f 在],[b a 上可导，则0)(<'x f 是)(x f 在],[b a 上单减的（ ） （A ）必要条件。 (B) 充分条件。 （C ）充要条件。 （D ）既非必要，又非充分条件。 答B 4．设n 是曲线x x x y arctan 2 2 2 -=的渐近线的条数，则=n （ ） (A) 1． (B) 2 (C) 3 (D) 4 答D 5．设函数)(x f 在)1,1(-内有定义，且满足)1,1(,)(2-∈?≤x x x f ，则0=x 必是

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图1 程序主流程图 说明：所以流程图由深圳市亿图软件有限公司的流程图绘制软件（试用版）绘制，转 存PDF后导出为图片加入到word中的，所以可能会打印效果不好，但确实为本人绘制。

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1、部署VDP模板 (57) 2、配置VDP (62) 3、创建备份作业 (68) 十三、附录 (72)

vmwarevsphere6.7虚拟化配置手册

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按F2，登录。

常用的操作就两块，网络和troubleshooting。 其中troubleshooting中的restart management agents选项，用在vcenter无法管理ESXi主机时。

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3、使用Acronis BR迁移linux物理机 (66) 十一、vmotion迁移测试 (81) 十二、HA高可用测试 (83) 十三、VMware vSphere FT双机热备 (84) 十四、vSphere Data Protection配置部署 (86) 1、部署VDP模板 (86) 2、配置VDP (90) 3、创建备份作业 (96) 十五、部署vRealize Operations Manager (101) 1、部署ova模版 (101) 2、配置vRealize Operations Manager (104) 十六、部署VMware-vRealize-Log-Insight (110) 1、部署OVF模版 (110) 十七、附录 (117)

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