CN1884090A - ZnIn2S4 nano materials and their synthesis method and application - Google Patents
ZnIn2S4 nano materials and their synthesis method and application Download PDFInfo
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Abstract
The invention discloses a Znln2S4 nanometer material and synthesizing method and application, which is characterized by the following: adopting bivalent zinc salt, trivalent indium salt and organic sulfide as raw material; proceeding solvent heating or water heating reaction at 100-220 deg.c in the sealing reactor; setting surface activist as addictive; synthesizing Znln2S4 nanometer pipe, nanometer band and nanometer line selectively through controlling solvent kind, reacting temperature and reacting time. The invention belongs to layer-shaped hexagonal crystal phase with kind's direction of specific property, which is fit for relative domains of solar battery, optical catalyst, high-energy battery, and heat-conversion.
Description
Technical Field
The invention relates to ZnIn2S4Preparation of, in particular, ZnIn2S4Nano material and its synthesis process and application. It is a hexagonal phase ZnIn2S4The nano tube, the nano belt and the nano wire have wide application prospect in the related fields of energy, catalysis, photoelectric devices and the like.
Background
ZnIn2S4The ternary chalcogenide semiconductor is an important ternary chalcogenide semiconductor, has structural diversity and unique photoelectric properties, and is widely applied to the fields of photoelectric device materials, thermoelectric materials, catalysts for photolyzing water and the like.
The performance test and application development of the material directly depend on the preparation thereof. ZnIn currently produced by solution chemistry2S4Both have a cubic spinel structure (M.A.Sriram, P.H.McMichael, A.WangHray, et al, J.Mater.Sci.1998, 33, 43334339.; Z.B.Lei, W.S.you, M.Y.Liu, et al, chem.Commun.2003, 2142. Zong. 2143.; R.B.Zong, X.G.Yang, H.M.Hu, et al, Mater.Res.Bull.2004, 39, 933.), and a hexagonal phase ZnIn2S4Still prepared mainly by high temperature high pressure reaction methods (T.Tinoco, A.Polian, J.P.Iti é, Phys.Stat.Sol. (b)1999, 211, 385-387.). ZnIn synthesized by various methods so far2S4The morphology of the product (including cubic and hexagonal phases) is mostly bulk material or nanoparticles. The shape of the substance on the nanometer scale is controlled and synthesized, in particular to the selective control synthesis of ZnIn2S4The research on one-dimensional materials such as nanotubes, nanobelts, nanowires and the like is not reported at home and abroad.
It is well known that the properties of a material depend on factors such as its crystal structure, shape and size, for example, hexagonal phase ZnIn2S4The thermoelectric properties of the material are significantly better than those of cubic phases (w.seo, r.otsuka, h.okuno, m.ohta, et al, j.mater.res.1999, 14, 41764181.), and thus, systematically controlling the crystal phase and morphology of the material is an important goal of modern chemistry and material science.
Disclosure of Invention
The object of the present invention is to provide a ZnIn2S4Nano material and its synthesis process and application. It adopts mild solution chemical method to synthesize hexagonal phase ZnIn2S4The material has excellent photoelectric property and wide application prospect. In a milder reactionRealizing the controlled synthesis of the shape and the crystal phase of the ZnIn under the condition to fill up the ZnIn2S4The blank in the preparation of one-dimensional nano materials so as to test the performance and research the application of the one-dimensional nano materialsAnd laying a foundation. Has wide application prospect in the related fields of energy, catalysis, photoelectric devices and the like.
The ZnIn provided by the invention2S4The crystal structure of the nano material is a hexagonal phase, and the nano material is a one-dimensional nano tube, a one-dimensional nano belt or a one-dimensional nano wire, wherein the inner diameter of the nano tube is 17-25 nm, the outer diameter is 40-60 nm, and the length is 500 nm-600 mu m; the width of the nanoribbon is 40-100 nm, the thickness is about 10nm, and the length is 500 nm-2 mm; the diameter of the nanowire is 15-30 nm, and the length of the nanowire is 500 nm-5 mm.
The ZnIn provided by the invention2S4The synthesis process of one-dimensional nanotube includes the following steps:
(1) adding zinc salt, indium salt and excessive organic sulfide (the molar ratio of the zinc salt to the indium salt to the organic sulfide is 0.5-5: 1-10: 2.5-40) into pyridine in a stoichiometric ratio, fully stirring, and sealing in a self-boosting reaction kettle;
(2) the system reacts for 16 to 24 hours at the temperature of 180 to 220 ℃, is cooled to room temperature, is filtered, washed and dried to obtain ZnIn2S4A nanotube.
The ZnIn provided by the invention2S4The synthesis method of the one-dimensional nanobelt takes divalent zinc salt, trivalent indium salt and organic sulfide as reaction raw materials, pyridine (py) as a solvent, and the solvothermal reaction is carried out at the temperature of 120-160 ℃. The method comprises the following steps:
(1) adding zinc salt, indium salt and excessive organic sulfide (the molar ratio of the zinc salt to the indium salt to the organic sulfide is 0.5-5: 1-10: 2.5-40) into pyridine in a stoichiometric ratio, fully stirring, and sealing in a self-boosting reaction kettle;
(2) the system reacts for 16-24 h at 120-160 ℃, is cooled to room temperature, filtered and washedWashing and drying to obtain ZnIn2S4A nanoribbon.
The ZnIn provided by the invention2S4The synthesis method of the one-dimensional nanowire takes divalent zinc salt, trivalent indium salt and organic sulfide as reaction raw materials, takes a surfactant as an additive, and generates hydrothermal reaction in a closed container. The method comprises the following steps:
(1) dissolving zinc salt, indium salt and excessive organic sulfide in stoichiometric ratio in water, adding a surfactant (the molar ratio of the zinc salt to the indium salt to the organic sulfide to the surfactant is 0.5-5: 1-10: 2.5-40: 0.005-0.4), and stirring to completely dissolve the zinc salt, the indium salt and the excessive organic sulfide;
(2) transferring the solution into a closed reaction kettle, reacting for 12-24 h at 100-180 ℃, cooling to room temperature, filtering, washing and drying to obtain ZnIn2S4Hollow fiber spheres;
(3) the hollow fiber ball is ultrasonically dispersed in ethanol or water (40 min-1.5 h, common ultrasonic cleaner) to obtain ZnIn2S4A nanowire.
The divalent zinc salt is zinc sulfate, zinc nitrate, zinc chloride or zinc acetate, and Zn is used2+Represents; the trivalent indium salt is indium trichloride In3+Represents; the organic sulfide is Thioacetamide (TAA); the surfactant is polyethylene glycol (PEG, the molecular weight is 1000-10000).
The above reaction is expressed by the following chemical equation:
the invention selects and controls the synthesis of hexagonal ZnIn under mild reaction conditions by reasonably selecting an organic sulfur source and combining a solvothermal/hydrothermal synthesis method and a surfactant template technology2S4ZnIn such as nanotube, nanoribbon and nanowire2S4A one-dimensional nanomaterial. The method is simple, strong in controllability and wide in applicability, and the obtained productThe one-dimensional nano material has excellent photoelectric property and is expected to be used in the related fields of solar cells, photocatalysis, high-energy cells, thermoelectric conversion and the like.
Drawings
FIG. 1 shows ZnIn prepared in example 12S4X-ray powder diffraction pattern of nanotubes.
FIG. 2 shows ZnIn prepared in example 12S4TEM images of nanotubes.
FIG. 3 shows ZnIn prepared in example 22S4X-ray powder diffraction pattern of the nanoribbons.
FIG. 4 shows ZnIn prepared in example 22S4TEM images of the nanobelts.
FIG. 5 shows ZnIn prepared in example 32S4X-ray powder diffraction pattern of nanowires.
FIG. 6 shows ZnIn prepared in example 32S4SEM image of hollow fiber spheres.
FIG. 7 shows ZnIn prepared in example 32S4TEM images of nanowires.
FIG. 8 shows ZnIn in example 42S4Ultraviolet-visible absorption spectrum of one-dimensional nano material.
FIG. 9 is the ZnIn described in example 52S4The structure schematic diagram of the one-dimensional nano material used for the dye-sensitized solar cell.
Detailed Description
The preparation of ZnIn described in the invention2S4In the one-dimensional nanomaterial method, zinc salt [ Zn]2+]And indium salt [ In3+]The ratio of (A) to (B) is controlled to be 1: 2, [ Zn]2+]The concentration is optimized to 0.25-0.1 mol/L, and the organic sulfide is fed according to 1-2 times of the required stoichiometric ratio. The preparation of ZnIn by the process of the invention is as follows2S4Some examples of one-dimensional nanomaterials are nanotubes, nanoribbons and nanowires. In the examples, ZnSO was used as a raw material4·7H2O、InCl3·4H2O and Thioacetamide (TAA), with whichThe preparation method of the raw materials is the same as that of the raw materials.
Example 1:
weighing 0.25mmol of ZnSO4·7H2O，0.5mmol InCl3·4H2O and 1mmol TAA are put into a 25mL polytetrafluoroethylene liner, 12mL pyridine is added, after magnetic stirring is carried out for 1h, the reaction kettle is sealed and heated at 180 ℃ for 16 h. After naturally cooling, filtering, washing with water and absolute ethyl alcohol for several times in sequence, and vacuum drying at 60 ℃ for 4h to obtain yellow powder. The product is identified as hexagonal ZnIn by X-ray powder diffraction2S4(FIG. 1). The morphology of the product is characterized by a Transmission Electron Microscope (TEM), and the result shows that the obtained product is a multi-wall nanotube (shown in figure 2), the inner diameter of the multi-wall nanotube is 17-25 nm, the outer diameter of the multi-wall nanotube is 40-60 nm, and the length of the multi-wall nanotube is about 500 nm-5 microns.
Example 2:
reducing the temperature of the reaction system to 160-120 ℃ while keeping other conditions unchanged to obtain ZnIn2S4A nanoribbon. The product is identified as hexagonal ZnIn by X-ray powder diffraction2S4(FIG. 3). The TEM represents the morphology of the product, and the result shows that the obtained product is a nanobelt (shown in figure 4), the width of the nanobelt is 40-100 nm, the thickness of the nanobelt is about 10nm, and the length of the nanobelt reaches 10 micrometers.
Example 3:
weighing 1mmol of ZnSO4·7H2O and 2mmol of InCl3·4H2And placing the O into a small beaker, adding 20mL of deionized water, and magnetically stirring to completely dissolve the O. Then 0.45g PEG-6000 (polyethylene glycol, molecular weight 6000) is added, after the PEG-6000 is completely dissolved, 4mmol TAA is finally added, and stirring is continued for 30min, so that colorless clear solution is obtained. The mixed solution was transferred to a 50mL teflon lined stainless steel self-pressurizing autoclave, sealed, and heated continuously at 160 ℃ for 16 h. And naturally cooling to room temperature, filtering, washing and drying to obtain yellow powder. The product is identified as hexagonal ZnIn by X-ray powder diffraction2S4(FIG. 5). The Scanning Electron Microscope (SEM) represents the appearance of the product, and the result shows that the obtained product is a hollow fiber ball (attached withFig. 6). Ultrasonically dispersing the powder in ethanol for 1h to obtain ZnIn2S4Nanowires (FIG. 7) with a diameter of about 20nm and a length of up to 500 μm.
Example 4:
ZnIn prepared by the method of the invention2S4The ultraviolet-visible absorption spectra of the one-dimensional nano materials such as the nano tube, the nano belt and the nano wire are tested on a JASCOV-550 ultraviolet-visible spectrophotometer (producing area: Japan), and the results show that the materials have strong absorption in an ultraviolet-visible region (shown in figure 8), and the optical band gap energies are respectively 2.38, 2.25 and 2.40eV, thereby indicating the potential application prospect in the field of photoelectric devices such as solar cells.
Example 5:
ZnIn prepared by the method of the invention2S4The one-dimensional nano materials such as the nano tube, the nano belt and the nano wire are used for the dye-sensitized solar cell (DSSC), and the specific implementation process is as follows:
(1) preparation of a photoanode
Adding TiO into the mixture2(Solaxronix SA, phi 13nm) and ZnIn produced by this method2S4Mixing one-dimensional nanometer material (mass ratio 4: 1) with small amount of ethanol, ultrasonically dispersing into paste, and coating the paste mixture on fluorine-doped conductive glass (F: SnO) with glass rod2Asahi, square resistance 10 Ω). After the mixture is naturally dried, the mixture is sintered for 6 hours at 400 ℃ in Ar (99.999%) atmosphere. Naturally cooling to room temperature, and adding TiO2/ZnIn2S4A thin film (thickness about 10 μm) of conductive glass was dipped in 0.1mM RuL2(NCS)2(chemical name: cis-bis (isothiocyanate) bis (2, 2-dipyridyl-4, 4-dicarboxylat) -ruthenaum (II) bis-tetrabutyllamonium, Johnson Matthey Ltd.) in a solution of tert-butanol dye (volume ratio 1: 1). Soaking at room temperature for 12 hr, taking out the conductive glass, washing with anhydrous ethanol to remove unadsorbed dye, and cutting the dye-sensitized film into film with active area of 1cm2And storing the photo-anode in a glove box filled with high-purity Ar gas for later use.
(2) Preparation of photocathode
A platinum film (about 2nm thick) was chemically deposited on another piece of conductive glass using a 0.05M solution of chloroplatinic acid in isopropanol (Aldrich) as a raw material to prepare a photocathode.
(3) Assembly of DSSC solar cells
The photoanode and cathode were separated by a 25 μm thick Surlyn thermoring (DuPont) and heat sealed. A small hole was drilled in the plastic seal between the electrodes and electrolyte (composition: 0.3M tetrabutylammonium iodide, 0.05M LiI, 0.05M 0.05M I) was injected through this hole20.25M 4-tert-butyl-pyridine), then sealed with Surlyn to prevent the electrolyte from leaking, and finally assembled into a sandwich type solar cell, the structure of which is shown in fig. 9.
(4) DSSC solar cell performance test and results
The current-voltage curve of the solar cell is applied to a solar simulation system (Yamashita Denso YSS-50, Am1.5, 100 mW. cm)-2) And (4) testing. Short-circuit current (J) thereofSC) Open circuit voltage (V)oc) The Fill Factor (FF) and the energy conversion efficiency (η) are respectively 9-11 mA-cm-2、650～670mV、0.60～0.70、8.5～10.2％。
Claims (10)
1. ZnIn2S4Nanomaterial characterized in that it is ZnIn of hexagonal crystalline phase crystal structure2S4Is ZnIn2S4One-dimensional nanotube, ZnIn2S4One-dimensional nanoribbons or ZnIn2S4A one-dimensional nanowire; the inner diameter of the nanotube is 17-25 nm, the outer diameter is 40-60 nm, and the length is 500 nm-600 mu m; the width of the nanoribbon is 40-100 nm, the thickness is about 10nm, and the length is 500 nm-2 mm; the diameter of the nanowire is 15-30 nm, and the length of the nanowire is 500 nm-5 mm.
2. The ZnIn of claim 12S4The synthesis process of one-dimensional nanotube features that bivalent zinc salt, trivalent indium salt and soluble organic sulfide as reaction material and pyridine (py) as solvent at 180 deg.cThe solvent thermal reaction is carried out under the conditions, and the steps are as follows:
(1) adding zinc salt, indium salt and excessive organic sulfide in stoichiometric ratio into pyridine, fully stirring, and sealing in a self-elevating reaction kettle;
(2) the system reacts for 16 to 24 hours at the temperature of 180 to 220 ℃, is cooled to room temperature, is filtered, washed and dried to obtain ZnIn2S4A nanotube.
3. ZnIn according to claim 22S4The synthesis method of the one-dimensional nanotube is characterized in that the molar ratio of the zinc salt, the indium salt and the organic sulfide is 0.5-5: 1-10: 2.5-40.
4. The ZnIn of claim 12S4The synthesis method of the one-dimensional nanobelt is characterized in that divalent zinc salt, trivalent indium salt and organic sulfide are used as reaction raw materials, pyridine (py) is used as a solvent, and the solvothermal reaction is carried out at the temperature of 120-160 ℃. The method comprises the following steps:
(1) adding zinc salt, indium salt and excessive organic sulfide in stoichiometric ratio into pyridine, fully stirring, and sealing in a self-elevating reaction kettle;
(2) the system reacts for 16 to 24 hours at the temperature of 120 to 160 ℃, is cooled to room temperature, is filtered, washed and dried to obtain ZnIn2S4A nanoribbon.
5. ZnIn according to claim 42S4The synthesis method of the one-dimensional nanobelt is characterized in that the molar ratio of zinc salt to indium salt to organic sulfide is as follows: 0.5-5: 1-10: 2.5-40.
6. The ZnIn of claim 12S4The synthesis process of one-dimensional nanometer line features that bivalent zinc salt, trivalent indium salt and organic sulfide as reaction material and surfactant as additive are hydrothermally reacted in a sealed container.
The method comprises the following steps:
(1) dissolving zinc salt, indium salt and excessive organic sulfide in stoichiometric ratio in water, adding a surfactant, and stirring to completely dissolve the surfactant;
(2) transferring the solution into a closed reaction kettle, reacting for 12-24 h at 100-180 ℃, cooling to room temperature,filtering, washing and drying to obtain ZnIn2S4Hollow fiber spheres;
(3) the hollow fiber ball is ultrasonically dispersed in ethanol or water (40 min-1.5 h, common ultrasonic cleaner) to obtain ZnIn2S4A nanowire.
7. ZnIn according to claim 62S4The synthesis method of the one-dimensional nanowire is characterized in that the molar ratio of the zinc salt, the indium salt, the organic sulfide and the surfactant is 0.5-5: 1-10: 2.5-40: 0.005-0.4.
8. A synthesis process according to claim 2, 4 or 6, characterized in that the divalent zinc salt is zinc sulphate, zinc nitrate, zinc chloride or zinc acetate; the trivalent indium salt is indium trichloride; the organic sulfide is thioacetamide.
9. ZnIn according to claim 62S4The synthesis method of the one-dimensional nanowire is characterizedin that the surfactant is polyethylene glycol, and the molecular weight is 1000-10000.
10. The ZnIn of claim 12S4Use of a nanomaterial characterized in that it is used in a solar cell, a photo-catalysis, a high-energy cell or a device for thermoelectric conversion.
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