CN105692688A - Method for preparing spherical In2S3 nanometer materials by aid of ionic liquid - Google Patents
Method for preparing spherical In2S3 nanometer materials by aid of ionic liquid Download PDFInfo
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- CN105692688A CN105692688A CN201610097952.9A CN201610097952A CN105692688A CN 105692688 A CN105692688 A CN 105692688A CN 201610097952 A CN201610097952 A CN 201610097952A CN 105692688 A CN105692688 A CN 105692688A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The invention discloses a method for preparing spherical In2S3 nanometer materials by the aid of ionic liquid. The method includes adding a certain quantity of water into an inner container of a polytetrafluoroethylene high-pressure reaction kettle and then sequentially adding appropriate quantities of In(NO3)3 4.5H2O, thioacetamide and the 1-butyl-3-methylimidazolium tetrafluoroborate [Bmim]BF4 ionic liquid into the inner container of the polytetrafluoroethylene high-pressure reaction kettle; uniformly stirring the water, the In(NO3)3 4.5H2O, the thioacetamide and the 1-butyl-3-methylimidazolium tetrafluoroborate [Bmim]BF4 ionic liquid to obtain mixtures, arranging the mixtures in the reaction kettle, carrying out reaction on the mixtures at the temperatures of 160 DEG C for a period of time and then naturally cooling precipitates until the temperatures of the precipitates reach the room temperature; repeatedly ultrasonically cleaning the precipitates by the aid of distilled water and absolute ethyl alcohol and drying the precipitates at the temperatures of 60 DEG C under the vacuum conditions for 8 h. The method has the advantages that the ionic liquid which is aqueous solution is used as a reaction medium, and the environment-friendly reaction is carried out; the method is simple and convenient, is free of environmental pollution and good in repeatability, the micro-sphere materials have perfect crystal forms and morphological structures, and accordingly the method has certain application value.
Description
Technical field:
The invention belongs to material chemistry technical field, particularly relate to ionic liquid auxiliary and prepare flower ball-shaped In2S3The chemical method of nano material。
Background technology:
In2S3It is the important type n semiconductor material of a class, is typical III-VI family sulfide, has potential application prospect in fields such as luminescence, photoconduction, photoelectricity and photocatalysis。The physicochemical properties of indium sulfide uniqueness depend not only upon its thing phase, are also largely dependent upon its pattern, size and organizational structure etc.。Regulation and control In2S3Pattern to develop this material practical application significant。So far, the In that research worker has synthesized2S3Pattern has granule, nano wire, nanotube, nanosphere, nanometer sheet and nanometer rods etc.。Although making some progress, but the three-dimensional In of regulation and control2S3The pattern of multilevel hierarchy and size remain a very big challenge。With Conventional nano crystalline phase ratio, three-dimensional manometer multilevel hierarchy is more suitable for being used as the construction material of photonic crystal。At present about In2S3The report of multilevel hierarchy is few, and Qi Kezhen etc. delivers the scientific paper being entitled as " liquid phase synthesis of flower-shaped indium sulfide nanometer hierarchical structure and Morphological control mechanism " on " advanced chemical journal ", with In (NO3)3And C2H5NS is predecessor, adopts liquid phase synthesizing method to be prepared for the three-dimensional flower-shaped β-In being made up of two-dimensional nano sheet2S3Multilevel hierarchy。But hydro-thermal method and solvent-thermal method operation are easier。Zhao etc. deliver the article being entitled as " Fabricationofindiumsulfidehollowspheresandtheirconversio ntoindiumoxidehollowspheresconsistingofmultiporenanoflak es " on " JPhysChemC " magazine, with biomolecule cysteine and InCl3·4H2O is raw material, and dodecyl alcohol is adjuvant, adopts 180 ° of C constant temperature 12h of hydro-thermal method to synthesize the In of nanometer sheet self assembly2S3Tiny balloon。Chen etc. deliver on " Chem.Phys.Lett. " magazine and are entitled as " Single-sourceapproachtothesynthesisofIn2S3andIn2O3Crystallitesandtheiropticalproperties " article, with the metallorganic In (S of indium2CNEt2)3For raw material, employing hydro-thermal method, in 180 ° of C constant temperature 12h, obtains the In that nanometer sheet assembles2S3Microsphere。It is raw material as the organic indium compound that template or use are expensive that above method needs to use biomolecule。
Substituting solvent as green, ionic liquid at room temperature is subject to the extensive concern of region of chemistry every field。Ionic liquid refers to and presents liquid, the complete salt being made up of zwitterion in room temperature or under room temperature condition, also referred to as low temperature molten salt or organic ion liquid。And present ionic liquid not only has the advantage of conventional organic solvents, and show many excellent properties compared with organic solvent, for instance almost without vapour pressure, without flammable, there is wider electrochemical window, height and stable electrical conductivity, non-volatile。Therefore, ionic liquid becomes the welcome green solvent of new century, and the application in catalysis, electrochemistry, separation etc. causes the interest of research worker。In the process that many inorganic material synthesize, the architectural characteristic of material can be controlled with ionic liquid for medium, be characterized as being the size of granule, structure and pattern, according to this effect of ionic liquid, it is possible to prepare the inorganic material of different-shape。
Chen Hui admires to wait to deliver in " fine chemistry industry " and is entitled as " different structure, pattern In2S3The ion thermal synthesis of nano material and sign " article, with InCl3·4H2O and Na2S is raw material, respectively with 1-ethyl 3-Methylimidazole. bromine salt [Emim] Br ionic liquid and 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF4Ion full-boiled process synthesis flake, flower ball-shaped indium sulfide nano material。But solvent is all with ionic liquid, and cost is too high。Chai etc. deliver on " Nanoscale " magazine and are entitled as " Walnut-likeIn2S3Microspheres:ionicliquid-assistedsolvothermalsynthesis, characterizationandformationmechanism " article, with In (NO3)3And Na2S·9H2O is raw material, is the indium sulfide microsphere etc. that solvent has synthesized walnut wood shape with the aqueous solution of ionic liquid 1-butyl-3-methyl imidazolium bromine salt [Bmim] Br。But Na2S·9H2O is prone to hydrolysis。Therefore, find the preparation method that a kind of operation is easier, prepare a kind of reproducible, perfect flower ball-shaped In of pattern2S3Nano material, is problem in the urgent need to address。
Summary of the invention
Problem to be solved by this invention is: overcomes and prepares In at present2S3The dependence biomolecule existed in crystal method is raw material, Na as the organic indium compound that template or use are expensive2S·9H2O is prone to the shortcomings such as hydrolysis。A kind of ionic liquid auxiliary is provided to prepare flower ball-shaped In2S3The method chemical method of nano material。This method adopts with ionic liquid [Bmim] BF4Aqueous solution be that medium with water full-boiled process prepares flower ball-shaped In2S3。The method is simple to operate, environmentally friendly, without loaded down with trivial details post-processing operation, only need to be co-located in having in the stainless steel cauldron of polytetrafluoroethylliner liner by reactant, take out after reaction, respectively with distilled water and the repeated multiple times ultrasonic centrifuge washing of dehydrated alcohol, 60 DEG C of vacuum drying 8h。
The problem to solve is adopted the technical scheme that by the present invention:
Flower ball-shaped In2S3The preparation method of nano material, with ionic liquid aqueous solution for medium, adopting water heat transfer diameter is about 2 μm In2S3Microsphere, is formed by the flake-assembly mode of receiving of 20nm left and right thickness, and nanometer sheet thickness uniformity is high。The ionic liquid auxiliary of the present invention prepares flower ball-shaped In2S3The method of nano material, what it was prepared concretely comprises the following steps:
(1) add water in a reservoir, be then sequentially added into In (NO3)3·4.5H2O, thioacetamide and ionic liquid, the mass range adding ionic liquid is 2.5g ~ 7g。Mixed solution is stirred；
(2) being placed on by container at 160 DEG C reaction a period of time, reaction time range is 12h ~ 96h, and namely reaction prepares flower ball-shaped In after terminating2S3Nano material；
(3) naturally cool to room temperature, it is thus achieved that precipitate respectively with distilled water and the repeated multiple times ultrasonic centrifuge washing of dehydrated alcohol, 60 DEG C of vacuum drying 8h。
In technical scheme, In (NO in reactant3)3It is 1:4 with the mol ratio of thioacetamide。
In (NO in reactant3)3It is 1:4 with the mol ratio of thioacetamide。
The medium of reaction is the aqueous solution of ionic liquid, and described ionic liquid refers to 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF4。
Described container is the stainless steel cauldron (volume is 100mL) with polytetrafluoroethylliner liner, and it respectively washs repeatedly with tap water, distilled water before using successively, dries。
In technical scheme, the medium of reaction is the aqueous solution of ionic liquid, and described ionic liquid refers to [Bmim] BF4。The effect adding ionic liquid is the pattern controlling end product。
In technical scheme, described container is the stainless steel cauldron (volume is 100mL) with polytetrafluoroethylliner liner, and it respectively washs repeatedly with tap water, distilled water before using successively, dries。
Advantages of the present invention:
1, preparation method is simple。With ionic liquid aqueous solution for medium, adopt water heat transfer In2S3Microsphere；
2, the effect adding ionic liquid is the pattern controlling end product；
3, reacting reproducible, product pattern is perfect, and nanometer sheet thickness uniformity is high；
4, environmentally friendly reaction, applied range are belonged to。Ionic liquid used by course of reaction, In (NO3)3·4.5H2O and thioacetamide are all nontoxic, it is possible to reduce environmental pollution, reduce the harm to human body；And without using biomolecule, and can large area prepare, it is simple to industrialized production and Technique Popularizing。
Accompanying drawing illustrates:
The flower ball-shaped In of Fig. 1-1, embodiment 1 preparation2S3X-ray diffraction (XRD) spectrogram of nano material；
The flower ball-shaped In of Fig. 1-2, embodiment 1 preparation2S3The field emission scanning electron microscope figure of nano material；
The flower ball-shaped In of Fig. 2-1, embodiment 2 preparation2S3X-ray diffraction (XRD) spectrogram of nano material；
The flower ball-shaped In of Fig. 2-2, embodiment 2 preparation2S3The field emission scanning electron microscope figure of nano material；
The flower ball-shaped In of Fig. 3-1, embodiment 3 preparation2S3X-ray diffraction (XRD) spectrogram of nano material；
The flower ball-shaped In of Fig. 3-2, embodiment 3 preparation2S3The field emission scanning electron microscope figure of nano material；
The flower ball-shaped In of Fig. 4-1, embodiment 4 preparation2S3X-ray diffraction (XRD) spectrogram of nano material；
The flower ball-shaped In of Fig. 4-2, embodiment 4 preparation2S3The field emission scanning electron microscope figure of nano material；
In figure, diffraction maximum is compared with standard diagram, corresponding to Emission in Cubic In2S3(PDFNumber:32-456), θ=20.42 °, main diffraction peak position 2,27.49 °, 47.85 °, 56.08 °, corresponding crystal face indexes is followed successively by: (211), (311), (531), (622)。
Detailed description of the invention:
Further illustrate flower ball-shaped In by the examples below2S3The preparation method of nano material。
Flower ball-shaped In2S3The preparation method of nano material, with ionic liquid aqueous solution for medium, adopting water heat transfer diameter is about 2 μm In2S3Microsphere, is formed by the flake-assembly mode of receiving of 20nm left and right thickness, and nanometer sheet thickness uniformity is high。The ionic liquid auxiliary of the present invention prepares flower ball-shaped In2S3The method of nano material, what it was prepared concretely comprises the following steps:
(1) add water in a reservoir, be then sequentially added into In (NO3)3·4.5H2O, thioacetamide and ionic liquid, the mass range adding ionic liquid is 2.5g ~ 7g。Mixed solution is stirred；
(2) being placed on by container at 160 DEG C reaction a period of time, reaction time range is 12h ~ 96h, and namely reaction prepares flower ball-shaped In after terminating2S3Nano material；
(3) naturally cool to room temperature, it is thus achieved that precipitate respectively with distilled water and the repeated multiple times ultrasonic centrifuge washing of dehydrated alcohol, 60 DEG C of vacuum drying 8h。
In technical scheme, In (NO in reactant3)3It is 1:4 with the mol ratio of thioacetamide。
In (NO in reactant3)3It is 1:4 with the mol ratio of thioacetamide。
The medium of reaction is the aqueous solution of ionic liquid, and described ionic liquid refers to 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF4。
Described container is the stainless steel cauldron (volume is 100mL) with polytetrafluoroethylliner liner, and it respectively washs repeatedly with tap water, distilled water before using successively, dries。
In technical scheme, the medium of reaction is the aqueous solution of ionic liquid, and described ionic liquid refers to [Bmim] BF4。The effect adding ionic liquid is the pattern controlling end product。
In technical scheme, described container is the stainless steel cauldron (volume is 100mL) with polytetrafluoroethylliner liner, and it respectively washs repeatedly with tap water, distilled water before using successively, dries。
Embodiment 1
1, preparation: politef reactor (volume is 100mL) is respectively washed 3 times with tap water, distilled water successively, stand-by after drying；
2, reactions steps: add 50mL water in the reactor that step 1 processed, be then sequentially added into 0.4mmolIn (NO3)3·4.5H2[Bmim] BF of O, 1.6mmol thioacetamide and 7.5g4。After uniform for above-mentioned solution stirring, put in reactor, at 160 DEG C, react 48h；
3, post processing: then reaction naturally cools to room temperature after terminating。The precipitate obtained cleans with distilled water and dehydrated alcohol repeated ultrasonic centrifuge washing respectively, 60 DEG C of vacuum drying 8h。Then carefully proceed in sample cell, preserve in lucifuge, dry environment。The outward appearance of product is uniform yellow, determines that it only has In with x-ray powder diffraction instrument (XRD)2S3, it does not have impurity, XRD figure spectrum is shown in Fig. 1-1。Observing its microstructure under field emission scanning electron microscope be diameter is about 2 μm In2S3Microsphere, is formed by the flake-assembly mode of receiving of 20nm left and right thickness, and nanometer sheet thickness uniformity is high。Flied emission scanning electron micrograph is shown in Fig. 1-2。
Embodiment 2
1, preparation: with embodiment 1；
2, reactions steps: add 50mL water in the reactor that step 1 processed, is then sequentially added into 0.4mmolIn (NO3)3·4.5H2[Bmim] BF of O, 1.6mmol thioacetamide and 5g4。After uniform for above-mentioned solution stirring, put in reactor, at 160 DEG C, react 48h；
3, post processing: with embodiment 1。The outward appearance of product is uniform yellow, and XRD figure spectrum is shown in Fig. 1-1, and Flied emission scanning electron micrograph is shown in Fig. 2-2。
Embodiment 3
1, preparation: with embodiment 1；
2, reactions steps: add 50mL water in the reactor that step 1 processed, is then sequentially added into 0.4mmolIn (NO3)3·4.5H2[Bmim] BF of O, 1.6mmol thioacetamide and 2.5g4。After uniform for above-mentioned solution stirring, put in reactor, at 160 DEG C, react 48h；
3, post processing: be uniform yellow with the outward appearance of embodiment 1 product, XRD figure spectrum is shown in Fig. 3-1, and Flied emission scanning electron micrograph is shown in Fig. 3-2。
Embodiment 4
1, preparation: with embodiment 1；
2, reactions steps: add 50mL water in the reactor that step 1 processed, is then sequentially added into 0.4mmolIn (NO3)3·4.5H2[Bmim] BF of O, 1.6mmol thioacetamide and 5g4。After uniform for above-mentioned solution stirring, put in reactor, at 160 DEG C, react 24h；
3, post processing: be uniform yellow with the outward appearance of embodiment 1 product, XRD figure spectrum is shown in Fig. 4-1, and Flied emission scanning electron micrograph is shown in Fig. 4-2。
The present invention uses common ionic liquid [Bmim] BF4Aqueous solution, as reaction medium, directly adopts In (NO under hydrothermal conditions3)3·4.5H2O and thioacetamide, through single step reaction, prepare flower ball-shaped In2S3Nano material。Not using any noxious substance, belong to environmentally friendly reaction, it is not necessary to follow-up purification step, material morphology is perfect, and nanometer sheet thickness uniformity is high。Easy to operate, it is simple to industrialized production and Technique Popularizing。
Claims (4)
1. flower ball-shaped In2S3The preparation method of nano material, it is characterised in that: with ionic liquid aqueous solution for medium, adopting water heat transfer diameter is about 2 μm In2S3Microsphere, is formed by the flake-assembly mode of receiving of 20nm left and right thickness, and nanometer sheet thickness uniformity is high；
The ionic liquid auxiliary of the present invention prepares flower ball-shaped In2S3The method of nano material, what it was prepared concretely comprises the following steps:
(1) add water in a reservoir, be then sequentially added into In (NO3)3·4.5H2O, thioacetamide and ionic liquid, the mass range adding ionic liquid is 2.5g ~ 7g, is stirred by mixed solution；
(2) being placed on by container at 160 DEG C reaction a period of time, reaction time range is 12h ~ 96h, and namely reaction prepares flower ball-shaped In after terminating2S3Nano material；
(3) naturally cool to room temperature, it is thus achieved that precipitate respectively with distilled water and the repeated multiple times ultrasonic centrifuge washing of dehydrated alcohol, 60 DEG C of vacuum drying 8h。
2. flower ball-shaped according to claim 12S3The preparation method of nano material, it is characterised in that: In (NO in reactant3)3It is 1:4 with the mol ratio of thioacetamide。
3. flower ball-shaped according to claim 12S3The preparation method of nano material, it is characterised in that: the medium of reaction is the aqueous solution of ionic liquid, and described ionic liquid refers to 1-butyl-3-methyl imidazolium tetrafluoroborate [Bmim] BF4。
4. flower ball-shaped according to claim 12S3The preparation method of nano material, it is characterised in that: described container is the stainless steel cauldron (volume is 100mL) with polytetrafluoroethylliner liner, and it respectively washs repeatedly with tap water, distilled water before using successively, dries。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106423166A (en) * | 2016-10-20 | 2017-02-22 | 绍兴文理学院 | Compounding method for cuprous oxide visible photocatalyst |
| CN112981447A (en) * | 2021-02-10 | 2021-06-18 | 中国科学技术大学 | Preparation method and application of nanometer flower-like sulfide |
| CN115367785A (en) * | 2022-08-23 | 2022-11-22 | 安徽工程大学 | High-efficiency photocatalyst micro/nano-thorn spherical indium sulfide and preparation method and application thereof, indium sulfide composite membrane and preparation method and application thereof |
| CN115959701A (en) * | 2023-02-20 | 2023-04-14 | 西南交通大学 | Preparation method and application of 3D self-assembly hydrangea-shaped indium sulfide |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106423166A (en) * | 2016-10-20 | 2017-02-22 | 绍兴文理学院 | Compounding method for cuprous oxide visible photocatalyst |
| CN106423166B (en) * | 2016-10-20 | 2019-04-26 | 绍兴文理学院 | A kind of synthetic method of cuprous oxide visible light catalyst |
| CN112981447A (en) * | 2021-02-10 | 2021-06-18 | 中国科学技术大学 | Preparation method and application of nanometer flower-like sulfide |
| CN115367785A (en) * | 2022-08-23 | 2022-11-22 | 安徽工程大学 | High-efficiency photocatalyst micro/nano-thorn spherical indium sulfide and preparation method and application thereof, indium sulfide composite membrane and preparation method and application thereof |
| CN115959701A (en) * | 2023-02-20 | 2023-04-14 | 西南交通大学 | Preparation method and application of 3D self-assembly hydrangea-shaped indium sulfide |
| CN115959701B (en) * | 2023-02-20 | 2024-04-26 | 西南交通大学 | Preparation method and application of 3D self-assembled hydrangea-shaped indium sulfide |
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