CN103950890B - A kind of FeS 2the preparation method of pyrite microballoon and application thereof - Google Patents

A kind of FeS 2the preparation method of pyrite microballoon and application thereof Download PDF

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CN103950890B
CN103950890B CN201410211032.6A CN201410211032A CN103950890B CN 103950890 B CN103950890 B CN 103950890B CN 201410211032 A CN201410211032 A CN 201410211032A CN 103950890 B CN103950890 B CN 103950890B
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fes
pyrite
microballoon
preparation
mixed solution
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CN103950890A (en
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许俊
孙联领
谢超
罗林保
史正添
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Hefei University of Technology
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Abstract

The invention discloses a kind of FeS 2the preparation method of pyrite microballoon and application thereof, is characterized in that: source of iron be dissolved in triethylene glycol, then adds sulphur powder, be stirred to dissolving, obtains mixed solution; Mixed solution is reacted 4 ~ 20h under 170-220 DEG C of condition, obtains reaction mixture; Reaction mixture is centrifugal, cleaning, dry, obtain target product FeS 2pyrite microballoon.Preparation method's technique of the present invention is simple, easy to operate, and product has that stable performance, uniformity are good, phase purity advantages of higher; By changing source of iron and reaction time, FeS can be improved 2the degree of crystallinity of pyrite microballoon, and regulate and control its size and pattern.FeS 2pyrite shows very outstanding electro catalytic activity to electrolytical catalytic regeneration in semiconductor sensitization solar battery, can replace precious metals pt as sensitization solar battery to electrode material, make battery have higher photoelectric transformation efficiency.

Description

A kind of FeS 2the preparation method of pyrite microballoon and application thereof
Technical field
The present invention relates to a kind of FeS 2the preparation method of pyrite microballoon, belongs to technical field of nano material.
Background technology
In recent years, due to electricity and the optical property of nano structural material excellence, it gradually becomes the study hotspot of domestic and international advanced material and field of functional materials.Nano-structured solar cell is emerging third generation solar cell, has the advantages such as theoretical efficiency is high, manufacturing process is simple, with low cost.Wherein, due to many exciton effects of nano material, the theoretical light photoelectric transformation efficiency of quantum dot sensitized solar cell, up to 44%, is a kind of nanostructured battery device had wide application prospects.Quantum dot sensitized solar cell by working electrode, electrolyte solution and electrode three part is formed; Wherein, electrode is played in sensitization solar battery to the electrolytical effect of oxidation state in catalytic reduction electrolyte.In order to improve the photoelectric transformation efficiency of battery, larger specific area, good electric conductivity and higher catalytic activity should be had to electrode, promoting that electrolyte is at the reducing/regenerating to electrode surface.Therefore, exploration and development of new nano structural material have important Research Significance and practical value as efficient to electrode material.
Pyrite FeS 2be a kind of cheap, raw material output abundant, eco-friendly sulfide compound semiconductor material, its energy gap is that 0.95eV, light absorption range are wide, absorption coefficient is up to α ≈ 5 × 10cm -1, carrier mobility is high, is a kind of semiconductor photovoltaic material had wide application prospects.Such as, the people FeS such as Alec Kirkeminde 2nano square and CdS quantum dot structure heterojunction solar battery, battery open circuit voltage is 1.1% (Nanoscale, 2012,4,7649 – 7654) up to 0.79V, photoelectric transformation efficiency.Up to the present, FeS is prepared 2pyritous method has: the methods such as magnetic-field-assisted gas colloidal sol pyrolysis synthesis, electrochemical deposition, chemical vapour deposition (CVD), Hydrothermal Synthesis, solvent-thermal process and Microwave synthesize.But, these preparation method's ubiquity preparation conditions require higher as chemical vapour deposition (CVD) need high temperature high vacuum condition, partial solvent process for thermosynthesizing needs problem such as use organic surface active agent etc., prepared FeS 2more there is the mutually impure and pattern of the mutually pyritous impurity of non-cubic, product in pyrite nanostructured product uneven etc.
So far, pyrite FeS 2as to the application of electrode material in the quantum dot sensitized solar cell of low-cost high-efficiency, there is not been reported.Therefore, exploration and development low temperature synthesis technique prepare low cost FeS 2pyrite microballoon, and as a kind of high-efficiency quantum dot sensitization solar battery to electrode material come alternative precious metals pt electrode reduce further solar cell cost, improve battery efficiency, there is important Practical significance.
Summary of the invention
The present invention is the weak point for avoiding existing for above-mentioned prior art, provides a kind of cubic system FeS 2the preparation method of pyrite microballoon, the technical problem of solution is existing FeS 2pyrite preparation method needs high-temperature process, complex process, and products therefrom is mutually impure, and pattern is uneven limits its application, invention further provides the application to electrode material of this preparation method's products therefrom as quantum dot sensitized solar cell.
Technical solution problem of the present invention adopts following technical scheme:
FeS of the present invention 2the preparation method of pyrite microballoon, is characterized in that carrying out as follows:
A, 0.5mmol source of iron is dissolved in 40mL triethylene glycol, then adds 1.25mmol sulphur powder, be stirred to dissolving, obtain mixed solution;
B, then described mixed solution is reacted 4 ~ 20h under 170-220 DEG C of condition, obtain reaction mixture;
C, described reaction mixture is cooled to room temperature after, centrifugal acquisition sediment, cleaning, dry, obtain target product FeS 2pyrite microballoon.
FeS of the present invention 2the preparation method of pyrite microballoon, its feature is also: by the reaction time in set-up procedure b, the degree of crystallinity of adjustment aim product and diameter.Along with the growth of time, the diameter of product presents the trend of increase.Confirm through many experiments, when being when reacted 4h, products therefrom is mesoporous cellular microballoon, and when being 20h when reacted, products therefrom is solid microsphere.And along with the growth of time, FeS 2the degree of crystallinity of pyrite microballoon is also improving gradually.
Described in step a, source of iron is selected from FeSO 4, FeCl 2or Fe (NO 3) 2.
Described in step c, deionized water and washes of absolute alcohol are used in cleaning successively.
Drying described in step c is dry 6-15h at 20-60 DEG C.
At 170-220 DEG C of solvent heat condition S powder simultaneously as reagent and drop template, at FeS 2microballoon forming process in played key effect.Have in high boiling solvent triethylene glycol, S powder, at 170-220 DEG C, can be melted into spherical droplets, ensure that monodispersity and the uniform form of end product well.Fe simultaneously 2+ion and melting S drop react and form FeS 2pyrite nano particle.When the reaction time is shorter, these nanometer Fe S 2crystallite assembling forms cellular FeS 2pyrite microballoon, due to slaking effect, along with the reaction time extends, less cellular FeS 2pyrite microballoon can be assembled further and grow into larger microballoon.
FeS of the present invention 2the application of pyrite microballoon, its feature is: described FeS 2pyrite microballoon be used for as sensitization solar battery to electrode material.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the invention provides a kind of FeS 2the preparation method of pyrite microballoon, technique is simple, reaction condition is gentle, without the need to process such as high temperature, with low cost, be easy to promote; And products therefrom is cubic system, electrical and optical properties is excellent, overcomes FeS prepared by conventional method 2the shortcoming that pyrite nanostructured crystal is mutually impure;
2, the present invention is by controlling reaction time, source of iron etc. in preparation, can prepare the FeS of different-shape and degree of crystallinity 2microballoon;
3, the product monodispersity that obtains of preparation method of the present invention is good, stable performance, as semiconductor sensitization solar battery to electrode material, improve its photoelectric transformation efficiency.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 1 and embodiment 4 prepare FeS 2the XRD figure of pyrite microballoon:
Fig. 2 is cellular FeS prepared by the embodiment of the present invention 1 2the morphology characterization figure of pyrite microballoon: (a-d) is SEM figure, (e) is TEM figure, and (f) is HRTEM figure;
Fig. 3 is cellular FeS prepared by the embodiment of the present invention 1 2the Raman spectrogram of pyrite microballoon (Fig. 3 a), high-resolution Fe (Fig. 3 b) and S (Fig. 3 c) xps energy spectrum figure;
Fig. 4 is cellular FeS prepared by the embodiment of the present invention 1 2the SEM figure of pyrite microballoon (Fig. 4 a), EDS power spectrum (Fig. 4 b), and corresponding Fe (Fig. 4 c) and S (Fig. 4 d) EDS mapping schemes;
Fig. 5 is solid FeS prepared by the embodiment of the present invention 4 2morphology characterization figure: Fig. 5 a and Fig. 5 b of pyrite microballoon is the SEM figure of different amplification, and Fig. 5 c is TEM figure, Fig. 5 d is HRTEM figure;
Fig. 6 is FeS prepared by the embodiment of the present invention 2 and embodiment 3 2the SEM figure of pyrite microballoon;
Fig. 7 is solid FeS prepared by the embodiment of the present invention 4 2the SEM figure of pyrite microballoon (Fig. 7 a), EDS spectrogram (Fig. 7 b), and the EDS Mapping of corresponding Fe (Fig. 7 c) and S (Fig. 7 d) schemes;
Fig. 8 is FeS prepared by the embodiment of the present invention 5 2the SEM figure of pyrite microballoon;
The sample of Fig. 9 prepared by embodiment 1 and embodiment 4 is as to electrode material and using Pt as the J-V curve map to the sensitization solar battery prepared by electrode material.
Detailed description of the invention
Embodiment 1 ~ 4
The present embodiment prepares FeS as follows 2pyrite microballoon:
A, to take by table 1 or to measure each raw material: wherein S powder is selected from (Shanghai Run Jie chemical reagent Co., Ltd), analyzes pure (>99.9%); FeSO 47H 2o selects from (Shanghai Run Jie chemical reagent Co., Ltd), analyzes pure (>99.5%); Triethylene glycol is selected from (Shanghai Run Jie chemical reagent Co., Ltd), chemical pure (>98%);
Table 1
Embodiment S powder FeSO 4·7H 2O Triethylene glycol Temperature Time
1 1.25mmol 0.5mmol 40ml 200℃ 4h
2 1.25mmol 0.5mmol 40ml 200℃ 6h
3 1.25mmol 0.5mmol 40ml 200℃ 10h
4 1.25mmol 0.5mmol 40ml 200℃ 20h
B, by FeSO 47H 2o is dissolved in the middle of triethylene glycol, and adds 1.25mmol sulphur powder, magnetic agitation after 10 minutes ultrasonic process within 20 minutes, fully disperse to make sulphur powder, obtain mixed solution.
C, then gained mixed solution is transferred to reactor, being positioned in thermostatic drying chamber and remaining on 200 DEG C, the reaction time is respectively 4h, 6h, 10h and 20h.
D, taking-up reactor naturally cool to room temperature, centrifugal collecting precipitate, and with deionized water and washes of absolute alcohol several, then at 60 DEG C of vacuum drying 15h, obtain target product FeS 2pyrite microballoon.
Embodiment 5
The present embodiment prepares FeS as follows 2pyrite microballoon:
A, to take by table 2 or to measure each raw material: wherein S powder is selected from (Shanghai Run Jie chemical reagent Co., Ltd), analyzes pure (>99.9%); FeCl 24H 2o selects from (Shanghai Run Jie chemical reagent Co., Ltd), analyzes pure (>99.5%); Triethylene glycol is selected from (Shanghai Run Jie chemical reagent Co., Ltd), chemical pure (>98%);
Table 2
Embodiment S powder FeCl 2·4H 2O Triethylene glycol Temperature Time
5 1.25mmol 0.5mmol 40ml 170℃ 10h
B, by FeCl 24H 2o is dissolved in the middle of triethylene glycol, and adds 1.25mmol sulphur powder, magnetic agitation after 10 minutes ultrasonic process within 20 minutes, fully disperse to make sulphur powder, obtain mixed solution.
C, then gained mixed solution is transferred to reactor, being positioned in thermostatic drying chamber and remaining on 170 DEG C, the reaction time is 10h.
D, taking-up reactor naturally cool to room temperature, centrifugal collecting precipitate, and with deionized water and washes of absolute alcohol several, then at 60 DEG C of vacuum drying 6h, obtain target product FeS 2pyrite microballoon.
Fig. 1 is that the embodiment of the present invention 1 and embodiment 4 prepare FeS 2the XRD collection of illustrative plates of microballoon, as can be seen from the figure, all diffraction peak energy of each sample index the pyritous FeS of Emission in Cubic well 2(JCPDF01-1295), and do not observe other iron sulfide relevant peaks, disclose the FeS of pure Emission in Cubic 2pyritous formation.The collection of illustrative plates of contrast two products is known, and increase the reaction time, the diffraction peak intensity of gained sample is increased, and this also reveal that the increase in reaction time makes product have better degree of crystallinity.
Fig. 2 is cellular FeS prepared by the embodiment of the present invention 1 2(d), TEM schemes (Fig. 2 e) to Fig. 2 a to Fig. 2 to the SEM figure of pyrite microballoon, and HRTEM schemes (Fig. 2 f); Can find out that product is the nearly monodisperse particles of diameter at 500-800nm from Fig. 2 a and Fig. 2 b.Fig. 2 c and Fig. 2 d discloses FeS 2pyrite microsphere surface and inside are mesoporous bead, and form cellular microballoon, its aperture is within the scope of 25-30nm.HRTEM figure in the TEM figure and Fig. 2 f of Fig. 2 e confirms the mesoporous characteristic of microballoon further.And cellular FeS 2pyrite microballoon has good crystallinity.0.24nm fringe spacing matched well pyrite FeS in figure 2f 2{ the interplanar distance of 210} crystal face.
Fig. 3 is cellular FeS prepared by the embodiment of the present invention 1 2the Raman spectrum of pyrite microballoon (Fig. 3 a) and Fe (Fig. 3 b) and S (Fig. 3 c) high-resolution xps energy spectrum figure; Fig. 3 a demonstrates cellular FeS 2the Raman spectrum of pyrite microballoon has and is positioned at 338 and 374cm -1two strong characteristic peaks and at 424cm -1weak peak be observed, respectively corresponding pyrite FeS 2e g, A g, T gvibration mode.At 200-300cm -1there is no vibration peak in scope, show without FeS or Fe xo ygenerate Deng impurity phase, show that prepared is high-purity FeS further 2pyrite microballoon.Fig. 3 b shows cellular FeS 2the xps energy spectrum figure of the Fe2p of pyrite microballoon, wherein 719.94eV corresponds to Fe2p1/2,707.18eV and corresponds to Fe2p3/2, is FeS 2pyritous characteristic peak.Have also been observed the weak peak being positioned at 711.19eV in the drawings, this causes surperficial Fe because sample is exposed in air 2+by slight oxidation.Fig. 3 c is depicted as the XPS spectrum figure of the 2p of S, lays respectively at two peaks of 162.45eV (S2p3/2) and 163.60eV (S2p1/2) as we can see from the figure, this also with report pyrite FeS 2the combination of middle sulphur can match.
Fig. 4 is cellular FeS prepared by the embodiment of the present invention 1 2pyritous SEM figure (Fig. 4 a), EDS power spectrum (Fig. 4 b), and the EDS mapping of corresponding Fe (Fig. 4 c) and S (Fig. 4 d) schemes; In Fig. 4 b, EDS power spectrum discloses microballoon and contains Fe and S two kinds of elements, and its atomic ratio is 33:67, describes FeS 2formation.Fig. 4 c and Fig. 4 d shows that Fe and S is evenly distributed in whole cellular microballoon.
Fig. 5 is solid FeS prepared by the embodiment of the present invention 4 2pyrite microballoon SEM schemes (Fig. 5 a, Fig. 5 b), and TEM schemes (Fig. 5 c), and HRTEM figure (Fig. 5 d); 20h is extended to, FeS between can finding out when reacted 2the diameter of pyrite microballoon is increased to about 2 μm.The surface of pyrite microballoon also becomes smooth (Fig. 5 b).The TEM figure of Fig. 5 c also demonstrate that the formation of microspheres with solid.The fringe spacing of the 0.24nm demonstrated in HRTEM figure (Fig. 5 d), with pyritous FeS 2crystal structure { interplanar distance of 210} crystal face is consistent.
Fig. 6 (a) and Fig. 6 (b) is respectively the solid FeS of the embodiment of the present invention 2 and embodiment 3 preparation 2the SEM figure of pyrite microballoon, the SEM in conjunction with several embodiment schemes, the known growth found out along with the reaction time, and product is from less cellular FeS 2pyrite microballoon is to larger solid FeS 2the evolutionary process of pyrite microballoon.
Fig. 7 is solid FeS prepared by the embodiment of the present invention 4 2microballoon SEM figure (Fig. 7 a), EDS power spectrum (Fig. 7 b), and the EDS Mapping of corresponding Fe (Fig. 7 c) and S (Fig. 7 d) schemes, can find out that in product, Fe and S is uniformly distributed in whole microballoon, its atomic ratio is 34:66.
Fig. 8 is FeS prepared by the embodiment of the present invention 5 2the SEM figure of pyrite microballoon, observing microballoon is assembled by sheet to form, and diameter is about 2-3 μm.Illustrating by changing source of iron, pattern and the micro-structural of product can be regulated and controled.
The present invention explores prepared FeS further 2the application of pyrite microballoon in semiconductor sensitization solar battery, general existing semiconductor sensitization solar battery is by working electrode, many sulphur electrolyte and form electrode three part.Common, semiconductor sensitization solar battery (SSCs) adopts precious metals pt electrode as to electrode, but selling at exorbitant prices, the defect that is difficult to large-area applications limit its application in sensitization solar battery industrialization.
In the present embodiment, working electrode adopts growth ZnSe/CdSe on FTO glass to be total to the ZnO nano array of sensitization, i.e. ZnO/ZnSe/CdSe nano-array; Electrolyte adopts many sulphur electrolyte (S 2-/ S n 2-), that is: 1M Na 2the aqueous solution of S, 1M S and 0.1MNaOH.With cellular FeS prepared by embodiment 1 2pyrite microballoon and the solid FeS prepared by embodiment 4 2pyrite depositing them (is labeled as m-FeS respectively at FTO sheet glass 2/ FTO and s-FeS 2/ FTO) as replacing conventional P t/FTO to electrode to electrode, its J-V curve is as shown in Figure 9.The photovoltaic parameter of each battery: short-circuit current density (J sC), open-circuit voltage (V oC), fill factor, curve factor (FF) and photoelectric transformation efficiency (PCE) as shown in table 3.As can be seen from Table 3, with Pt/FTO to compared with electrode battery, FeS 2pyrite microballoon is as to electrode material, and the photoelectric transformation efficiency of battery significantly improves.Wherein m-FeS 2/ FTO is about that Pt/FTO is to 2 of electrode battery conversion efficiency times to the photoelectric transformation efficiency of electrode battery.As can be seen from the table, with FeS 2pyrite microballoon as to electrode material at short-circuit current density J sC, fill factor, curve factor FF and photoelectric transformation efficiency PCE is obviously better than traditional using Pt as the semiconductor sensitization solar battery to electrode material.
Table 3 uses the different performance comparison to the photovoltaic parameter of the battery of electrode

Claims (6)

1. a FeS 2the preparation method of pyrite microballoon, is characterized in that carrying out as follows:
A, 0.5mmol source of iron is dissolved in 40mL triethylene glycol, then adds 1.25mmol sulphur powder, be stirred to dissolving, obtain mixed solution;
B, then described mixed solution is reacted 4 ~ 20h under 170-220 DEG C of condition, obtain reaction mixture;
C, described reaction mixture is cooled to room temperature after, centrifugal acquisition sediment, cleaning, dry, obtain target product FeS 2pyrite microballoon.
2. FeS according to claim 1 2the preparation method of pyrite microballoon, is characterized in that: by the reaction time in set-up procedure b, the degree of crystallinity of adjustment aim product and size.
3. FeS according to claim 1 and 2 2the preparation method of pyrite microballoon, is characterized in that: described in step a, source of iron is selected from FeSO 4, FeCl 2or Fe (NO 3) 2.
4. FeS according to claim 1 and 2 2the preparation method of pyrite microballoon, is characterized in that: described in step c, deionized water and washes of absolute alcohol are used in cleaning successively.
5. FeS according to claim 1 and 2 2the preparation method of pyrite microballoon, is characterized in that: bake out temperature described in step c is 20-60 DEG C.
6. the FeS that described in a claim 1-5 any one, preparation method obtains 2the application of pyrite microballoon, is characterized in that: described FeS 2pyrite microballoon be used for as sensitization solar battery to electrode material.
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