CN102786038A - Hydro-thermal synthesis method of cubic phase InSe nano sheet - Google Patents
Hydro-thermal synthesis method of cubic phase InSe nano sheet Download PDFInfo
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Abstract
The invention belongs to the technical field of synthesis of environment-friendly nano material, relates to a synthesis method of the nano material, and particularly relates to a hydro-thermal synthesis method of cubic phase InSe nano sheet. The hydro-thermal synthesis method of cubic phase InSe nano sheet comprises the followings steps of: using a ternary hybrid solution of diethylenetriamine, hydrazine hydrate and water as solvent, carrying out hydro-thermal synthesis reaction on hydro-thermal synthesis aqueous solution and sodium selenite aqueous solution in a reaction kettle at 180 DEG C, rinsing by absolute ethyl alcohol, centrifugally separating, drying, and roasting, so as to obtain the nano material. Inferred from the growth mechanism, the method is suitable for the preparation of other selenium and tellurium metal compound nano materials. From the scanning electron microscope (SEM), after roasting, the nano sheet has high crystallinity, smooth surface and even size, and is 0.6-1.3microns in length, 0.5-1micron in width and 60nm in thickness, and most nano sheets are square. The preparation method has the following characteristics of simplicity, low cost, high controllability, high crystallinity of product, high yield, green and environmental protection.
Description
Technical field
The invention belongs to environmentally friendly nano material synthesis technical field, relate to the compound method of nano material, relate in particular to the hydrothermal synthesis method of a kind of cube of crystalline phase InSe nanometer sheet.
Background technology
In a broad sense, nano material just is meant in three-dimensional space, to have at least one dimension to be in the material in the nanoscale scope, or assembles the structured material that forms as elementary cell by them.If divide according to dimension, nano material can be divided into four types substantially: (i) zero dimension refers at the space three-dimensional yardstick all at nanoscale, like the particle of nanoscale, Nano microsphere, elementide etc.; (ii) one dimension, referring to has bidimensional to be in nanoscale in the space, like nano wire, nanometer rod, nanotube, nano belt and nanofiber etc.; (iii) two dimension refers in three-dimensional space, have one dimension at nanoscale, like ultrathin membrane, nanometer sheet, superlattice etc.(v) three-dimensional, refer to the material that forms according to the certain rule assembling by one dimension or two-dimensional nano material, like nanometer flower, nanometer sea urchin etc.
And nanometer sheet has significant physico-chemical property in flourish day by day nanostructure, to play the part of important role as a kind of important two-dimensional nano material, can be widely used in various important researchs and production field.For example: single nanometer sheet can be used as elementary cell and is assembled into nanometer flower and nanometer ball, is widely used on button cell, solar cell, catalyzer and the macromolecular material.Multiple different nanometer sheet can be formed various semi-conductors, catalyzer, magnet and plasma nano particle and can be applied in many devices such as optomagnetic catalyzer and the hydrogen manufacturing of photoelectrolysis water.Graphene is exactly an instance, and the electrical properties of two-dimentional graphene nanometer sheet is better than other nanostructures.The dimension of a large amount of sulfur family inorganic nano materials is determining its application performance, and the inorganic materials that therefore obtains the two-dimensional nano sheet is very important.
Indium selenide is as important III-VI main group compound; The laminate structure of forming by the Se-In-In-Se key; Intensive covalent linkage and faint Van der Waals force make it have the performances such as anisotropy, electricity, optics and magnetics, catalysis and air-sensitive of height between layer and the layer, thereby make indium selenide on devices such as polarized radiation, photovoltaic solar cells, lithium cell, fluorescent apparatus, dielectric medium, field-effect transistor, cause numerous people's attention.Simultaneously, indium selenide also can be used as the raw material that structural unit is used to prepare different ternary systems, for example CuInSe
2And AgInSe
2, be widely used on the photovaltaic material device and these materials have good photoelectric property.In addition, indium selenide is the photovaltaic material that a kind of direct band gap is 1.36eV, because photoelectronic anisotropy has very high uptake factor in visible light wave scope, can be electric energy with conversion of solar energy effectively, is a kind of photovoltaic energy material of excellence.Simultaneously, compare with lead selenide with cadmium selenide, indium selenide also has hypotoxicity and environment friendly in the low band-gap nano material.
Indium selenide has cube crystalline phase and hexagonal crystal mutually, and cube crystalline phase is the low temperature phase, and hexagonal crystal is the high temperature phase mutually.Receive the restriction of compound method, cube crystalline phase InSe is difficult to through traditional method synthetic, and synthetic InSe major part all is the hexagonal crystal phase at present, seldom relevant for cube relevant report of crystalline phase InSe.The method of the synthetic InSe that has developed mainly contains field-effect method, solid phase method, organo-metallic hot steam method etc.; But above-mentioned compound method needs the instrument of high-end precision; Temperature of reaction is at 400 ~ 1000 ℃, and energy consumption is big, meeting toxigenicity gas; Human body and environment are caused certain harm, and the sample that these methods obtain also have shortcomings such as heterogeneity and low yield.Therefore seek simple, cheap, green, a controlled method, it is necessary and challenging synthesizing the InSe nanometer structure.
Hydrothermal method has advantages such as equipment is simple, raw material obtains easily, obtain product purity height, good uniformity, chemical constitution precise control, receives many researchers' favor.Hydrothermal method is in special closed reactor (autoclave); With fluids such as water or organic solvents is RM; Through reaction system being heated to critical temperature (or near critical temperature), create a HTHP reflection environment, impel to be reflected in liquid phase or the gas phase and carry out; Make indissoluble or insoluble substance dissolves and recrystallization originally, process separation and thermal treatment obtain a kind of effective ways of product again.Hydrothermal method has the following advantages: temperature (generally between 120 ~ 200 ℃) liquid phase control during adopt (1), and energy consumption is relatively low, and suitability is wide, both can be used for the less nanoparticle preparation of size, also can obtain larger-size monocrystalline; (2) raw material is relatively inexpensive is easy to get, and is reflected in the quick convection current of liquid phase and carries out, and productive rate is high, thing is even mutually, high, the well-crystallized of purity, and the shape controlled amount; (3) in water-heat process, can pass through conditioned reaction temperature, pressure, time, pH value, precursor and tensio-active agent etc., reach the purpose of effective control reaction and crystal growth characteristic; (4) be reflected in the container of sealing and carry out, be applicable to the building-up reactions in the poisonous system, can reduce environmental pollution.
Summary of the invention
To defective that exists in the prior art and deficiency, the invention provides the hydrothermal synthesis method of a kind of cube of crystalline phase InSe nano material.
The hydrothermal synthesis method of a kind of cube of crystalline phase InSe nanometer sheet; Be to be solvent with diethylenetriamine, Hydrazine Hydrate 80 and water ternary mixing solutions; With the aqueous solution of indium chloride and aqueous solution hydrothermal synthesis reaction in 180 ℃ reaction kettle of Sodium Selenite; Use absolute ethanol washing then, spinning is dry also to be made after the calcining.Infer that from growth mechanism this method can be applicable to the preparation of other selenium, tellurium metal compound nano-material.
The hydrothermal synthesis method of a kind of cube of crystalline phase InSe nanometer sheet, concrete steps are following:
Steps A, take by weighing four hydration indium chlorides respectively, Sodium Selenite is dissolved in separately and processes solution in the deionized water, wherein, described indium ion concentration is 0.1mmol/L, concentration of sodium selenite is 0.1mol/L;
Step B, measure above-mentioned solution respectively and mix and stir, add diethylenetriamine, Hydrazine Hydrate 80 and deionized water mix,
Wherein said indium ion: the mol ratio of Sodium Selenite is 2:3,
Described diethylenetriamine, the volume ratio of Hydrazine Hydrate 80 and deionized water are 5:2:12;
Step C, in 180 ℃ of following reaction 72 ~ 96h, be cooled to room temperature then.
The flap that above-mentioned reaction is made with absolute ethanol washing after, make sheet indium selenide precursor after placing 60 ℃ of vacuum drying oven dryings.
In the preferred embodiment of the present invention, described calcining step is under argon shield, 400 ℃ of calcining 4h ~ 8h.
Cube crystalline phase InSe nanometer sheet that is prepared from according to the hydrothermal synthesis method of above-mentioned cube of crystalline phase InSe nanometer sheet is from its X-ray diffraction analysis figure (XRD), the InSe of typical cube of crystalline phase.26.8 °, corresponding (110) crystal face, 44.7 °, corresponding is (220) crystal face, and 52.6 °, be (311) crystal face, 64.9 °, be (400) crystal face, 71.6 °, be (314) crystal face; From its sem photograph (SEM), after calcining, the crystallinity of nanometer sheet strengthens, and the surface is very smooth, and the size of sheet is homogeneous relatively, and length is at 0.6 ~ 1.3 micron, and width is at 0.5 ~ 1 micron, and thickness is 60nm, and major part is cubic sheet.
Beneficial effect
Preparing method of the present invention is simple, with low cost, controllability is strong, product good crystallinity, output are high, environmental protection.
Description of drawings
Fig. 1 is the sheet indium selenide forerunner's of preparation X-ray diffraction analysis figure (XRD);
Fig. 2 is the sheet indium selenide forerunner's of preparation a sem photograph (SEM);
Fig. 3 is the sheet indium selenide forerunner's of preparation a transmission electron microscope picture (TEM);
Fig. 4 is the calcining X-ray diffraction analysis figure (XRD) of InSe nanometer sheet later;
Fig. 5 is the calcining sem photograph (SEM) of InSe nanometer sheet later;
Fig. 6 is the calcining transmission electron microscope picture (TEM) of InSe nanometer sheet afterwards.
Embodiment
Below in conjunction with embodiment the present invention is elaborated, so that those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
Embodiment 1
The hydrothermal synthesis method of a kind of cube of crystalline phase InSe nanometer sheet, concrete steps are following:
(1) take by weighing the 0.0442g indium chloride respectively with electronic balance, the Sodium Selenite of 0.0519g is in the reaction kettle of 25ml;
(2) use the 5ml transfer pipet respectively, the 2ml transfer pipet, the 10ml transfer pipet is measured diethylenetriamine, Hydrazine Hydrate 80, deionized water 5ml, 2ml, 12ml stirs 3min with glass stick in the 50ml beaker, it is mixed;
(3) measure mixing solutions 15ml reaction kettle in (1) in (2) with transfer pipet, stir 10min, it is mixed;
(4) reaction kettle sealing was put into 180 ℃ of baking oven constant temperature three days, naturally cool to room temperature then, with absolute ethanol washing 5 times, drying obtains the nanometer sheet of yellow indium selenide precursor in 60 ℃ of vacuum drying ovens;
(5) the yellow precursor that obtains in (4) is placed tube furnace, argon shield, 400 ℃ of calcining 6h obtain the InSe nanometer sheet.
Fig. 1 is the sheet indium selenide forerunner's of preparation a XRD figure, and as can be seen from the figure the peak of the inside is many, at 10 ° a strong peak is arranged in the past, and this peak is the peak of typical precursor.
Fig. 2 is the sheet indium selenide forerunner's of preparation SEM figure, as can be seen from the figure, the surperficial smoother of nanometer sheet, long is 0.9-1.5 μ m, and wide is 0.6-1.1 μ m, and thickness is 90nm.
Fig. 3 is the sheet indium selenide forerunner's of preparation TEM figure.As can be seen from the figure, sheet surface smoother, almost near transparent, the plasticity of sheet is fine.
Fig. 4 is the calcining XRD figure of InSe nanometer sheet later.This figure is the InSe of typical cube of crystalline phase, 26.8 °, and corresponding (110) crystal face, 44.7 °, corresponding is (220) crystal face, and 52.6 °, be (311) crystal face, 64.9 °, be (400) crystal face, 71.6 °, be (314) crystal face.
Fig. 5 is the calcining SEM figure of InSe nanometer sheet later.After calcining, the crystallinity of nanometer sheet strengthens, and the surface is very smooth, and the size of sheet is homogeneous relatively, and length is at 0.6 ~ 1.3 micron, and width is at 0.5 ~ 1 micron, and thickness is 60nm, and major part is cubic sheet.
Fig. 6 is the calcining TEM figure of indium selenide afterwards.Smooth degree is not calcined before good, and from projection, can see what slice was made up of small-particle.
Embodiment 2
The hydrothermal synthesis method of a kind of cube of crystalline phase InSe nanometer sheet, concrete steps are following:
(1) take by weighing the 0.0709g indium bromide respectively with electronic balance, the 0.0519g Sodium Selenite is in the 25ml reaction kettle;
(2) use the 5ml transfer pipet respectively, the 2ml transfer pipet, the 10ml transfer pipet is measured diethylenetriamine, Hydrazine Hydrate 80, deionized water 5ml, 2ml, 12ml stirs 3min with glass stick in the 50ml beaker, it is mixed;
(3) measure mixing solutions 15ml reaction kettle in (1) in (2) with transfer pipet, stirring 10min fully dissolves it and mixes;
(4) reaction kettle sealing was put into 180 ℃ of baking oven constant temperature three days, naturally cool to room temperature then, with absolute ethanol washing 5 times, drying obtains the nanometer sheet of yellow indium selenide precursor in 60 ℃ of vacuum drying ovens;
(5) the yellow precursor that obtains in (4) is placed tube furnace, argon shield, 400 ℃ of calcining 6h obtain the InSe nanometer sheet.
Embodiment 3
The hydrothermal synthesis method of a kind of cube of crystalline phase InSe nanometer sheet, concrete steps are following:
(1) take by weighing the 0.0764g indium nitrate respectively with electronic balance, the 0.0519g Sodium Selenite is in the 25ml reaction kettle;
(2) use the 5ml transfer pipet respectively, the 2ml transfer pipet, the 10ml transfer pipet is measured diethylenetriamine, Hydrazine Hydrate 80, deionized water 5ml, 2ml, 12ml stirs 3min with glass stick in the 50ml beaker, it is mixed;
(3) measure mixing solutions 15ml reaction kettle in (1) in (2) with transfer pipet, stirring 10min fully dissolves it and mixes;
(4) reaction kettle sealing was put into 180 ℃ of baking oven constant temperature three days, naturally cool to room temperature then, with absolute ethanol washing 5 times, drying obtains the nanometer sheet of yellow indium selenide precursor in 60 ℃ of vacuum drying ovens;
(5) the yellow precursor that obtains in (4) is placed tube furnace, argon shield, 400 ℃ of calcining 6h obtain the InSe nanometer sheet.
Embodiment 4
The hydrothermal synthesis method of a kind of cube of crystalline phase InSe nanometer sheet, concrete steps are following:
(1) take by weighing the 0.0884g indium chloride respectively with electronic balance, the Sodium Selenite of 0.1038g is in the reaction kettle of 50ml;
(2) use the 10ml transfer pipet respectively, the 5ml transfer pipet, the 10ml transfer pipet is measured diethylenetriamine, Hydrazine Hydrate 80, deionized water 10ml, 4ml, 24ml stirs 3min with glass stick in the 50ml beaker, it is mixed;
(3) measure mixing solutions 30ml reaction kettle in (1) in (2) with transfer pipet, stir 10min, it is mixed;
(4) reaction kettle sealing was put into 180 ℃ of baking oven constant temperature three days, naturally cool to room temperature then, with absolute ethanol washing 5 times, drying obtains the nanometer sheet of yellow indium selenide precursor in 60 ℃ of vacuum drying ovens;
(5) the yellow precursor that obtains in (4) is placed tube furnace, argon shield, 400 ℃ of calcining 6h obtain the InSe nanometer sheet.
Embodiment 5
The hydrothermal synthesis method of a kind of cube of crystalline phase InSe nanometer sheet, concrete steps are following:
(1) take by weighing the 0.0442g indium chloride respectively with electronic balance, the Sodium Selenite of 0.0519g is in the reaction kettle of 25ml;
(2) use the 5ml transfer pipet respectively, the 2ml transfer pipet, the 10ml transfer pipet is measured diethylenetriamine, Hydrazine Hydrate 80, deionized water 5ml, 2ml, 12ml stirs 3min with glass stick in the 50ml beaker, it is mixed;
(3) measure mixing solutions 15ml reaction kettle in (1) in (2) with transfer pipet, stir 10min, it is mixed;
(4) reaction kettle sealing was put into 180 ℃ of baking oven constant temperature four days, naturally cool to room temperature then, with absolute ethanol washing 5 times, drying obtains the nanometer sheet of yellow indium selenide precursor in 60 ℃ of vacuum drying ovens;
(5) the yellow precursor that obtains in (4) is placed tube furnace, argon shield, 400 ℃ of calcining 6h obtain the InSe nanometer sheet.
Embodiment 6
The hydrothermal synthesis method of a kind of cube of crystalline phase InSe nanometer sheet, concrete steps are following:
(1) take by weighing the 0.0442g indium chloride respectively with electronic balance, the Sodium Selenite of 0.0519g is in the reaction kettle of 25ml;
(2) use the 5ml transfer pipet respectively, the 2ml transfer pipet, the 10ml transfer pipet is measured diethylenetriamine, Hydrazine Hydrate 80, deionized water 5ml, 2ml, 12ml stirs 3min with glass stick in the 50ml beaker, it is mixed;
(3) measure mixing solutions 15ml reaction kettle in (1) in (2) with transfer pipet, stir 10min, it is mixed;
(4) reaction kettle sealing was put into 180 ℃ of baking oven constant temperature three days, naturally cool to room temperature then, with absolute ethanol washing 5 times, drying obtains the nanometer sheet of yellow indium selenide precursor in 60 ℃ of vacuum drying ovens;
(5) the yellow precursor that obtains in (4) is placed tube furnace, argon shield, 400 ℃ of calcining 4h obtain the InSe nanometer sheet.
Embodiment 7
The hydrothermal synthesis method of a kind of cube of crystalline phase InSe nanometer sheet, concrete steps are following:
(1) take by weighing the 0.0442g indium chloride respectively with electronic balance, the Sodium Selenite of 0.0519g is in the reaction kettle of 25ml;
(2) use the 5ml transfer pipet respectively, the 2ml transfer pipet, the 10ml transfer pipet is measured diethylenetriamine, Hydrazine Hydrate 80, deionized water 5ml, 2ml, 12ml stirs 3min with glass stick in the 50ml beaker, it is mixed;
(3) measure mixing solutions 15ml reaction kettle in (1) in (2) with transfer pipet, stir 10min, it is mixed;
(4) reaction kettle sealing was put into 180 ℃ of baking oven constant temperature three days, naturally cool to room temperature then, with absolute ethanol washing 5 times, drying obtains the nanometer sheet of yellow indium selenide precursor in 60 ℃ of vacuum drying ovens;
(5) the yellow precursor that obtains in (4) is placed tube furnace, argon shield, 400 ℃ of calcining 8h obtain the InSe nanometer sheet.
Claims (5)
1. the hydrothermal synthesis method of one kind of cube of crystalline phase InSe nanometer sheet; Be to be solvent with diethylenetriamine, Hydrazine Hydrate 80 and water ternary mixing solutions; With the aqueous solution of indium chloride and aqueous solution hydrothermal synthesis reaction in 180 ℃ reaction kettle of Sodium Selenite; Use absolute ethanol washing then, spinning is dry also to be made after the calcining.
2. the hydrothermal synthesis method of according to claim 1 cube of crystalline phase InSe nanometer sheet is characterized in that, described solvent thermal building-up reactions comprises the steps:
Steps A, take by weighing four hydration indium chlorides respectively, Sodium Selenite is dissolved in separately and processes solution in the deionized water, wherein, described indium ion concentration is 0.1mmol/L, concentration of sodium selenite is 0.1mol/L;
Step B, measure above-mentioned solution respectively and mix and stir, add diethylenetriamine, Hydrazine Hydrate 80 and deionized water mix,
Wherein said indium ion: the mol ratio of Sodium Selenite is 2:3,
Described diethylenetriamine, the volume ratio of Hydrazine Hydrate 80 and deionized water are 5:2:12;
Step C, in 180 ℃ of following reaction 72h ~ 96h, be cooled to room temperature then.
3. the hydrothermal synthesis method of according to claim 1 cube of crystalline phase InSe nanometer sheet is characterized in that, described calcining step is under argon shield, 400 ℃ of calcining 6h.
4. cube crystalline phase InSe nanometer sheet that is prepared from according to the said method of claim 1.
5. according to claim 4 cube of crystalline phase InSe nanometer sheet, the length that it is characterized in that nanometer sheet are at 0.6 ~ 1.3 micron, and width is at 0.5 ~ 1 micron, and thickness is 60nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106179406A (en) * | 2016-07-11 | 2016-12-07 | 福州大学 | A kind of single layer structure MnSb2s4the preparation method of catalysis material |
| CN107086321A (en) * | 2017-05-25 | 2017-08-22 | 莆田学院 | A kind of lithium battery |
| CN109459137A (en) * | 2018-09-12 | 2019-03-12 | 深圳大学 | Polarize the detection method of optical detector and polarised light |
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| CN101913575A (en) * | 2010-08-31 | 2010-12-15 | 武汉理工大学 | Method for preparing In4Se3 thermoelectric compound powder |
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Patent Citations (2)
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| WO1996020943A1 (en) * | 1995-01-06 | 1996-07-11 | President And Fellows Of Harvard College | Liquid precursor for cubic-phase passivating/buffer film |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106179406A (en) * | 2016-07-11 | 2016-12-07 | 福州大学 | A kind of single layer structure MnSb2s4the preparation method of catalysis material |
| CN106179406B (en) * | 2016-07-11 | 2018-06-15 | 福州大学 | A kind of single layer structure MnSb2S4The preparation method of catalysis material |
| CN107086321A (en) * | 2017-05-25 | 2017-08-22 | 莆田学院 | A kind of lithium battery |
| CN109459137A (en) * | 2018-09-12 | 2019-03-12 | 深圳大学 | Polarize the detection method of optical detector and polarised light |
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