CN110078031B - Te nanowire three-dimensional aerogel, and preparation method and application thereof - Google Patents
Te nanowire three-dimensional aerogel, and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a Te nanowire three-dimensional aerogel, a preparation method and application thereof, wherein the method comprises the following steps: dispersing one-dimensional Te nano-wires in an alcohol solvent, pre-assembling the one-dimensional Te nano-wires with lead nitrate, and then carrying out hydrothermal reaction in a high-pressure reaction kettle to obtain three-dimensional Te nano-wire hydrogel; and (3) carrying out supercritical drying on the Te nanowire three-dimensional hydrogel to obtain the Te nanowire three-dimensional aerogel. The one-dimensional Te nano-wire is pre-assembled under the induction of lead ions; and heating to enable the assembled nanowires to form a two-dimensional nanobelt, and forming a cross-linked network structure in the three-dimensional direction to finally obtain the macroscale three-dimensional Te nanowire hydrogel. The method is simple, and isotropic three-dimensional Te nano-wires with uniform size can be assembled.
Description
Technical Field
The invention belongs to the technical field of nano material assembly, and particularly relates to a Te nanowire three-dimensional aerogel, and a preparation method and application thereof.
Background
The controllable synthesis and effective assembly of metal or semiconductor nano materials, and the design and performance research of devices based on the nano materials are one of the premises and guarantees of the devices towards the use. German applied chemistry (angew. Chem. Int. Ed.2015, 13101, 54) states that nanomaterial assemblies in the form of macroscopic aerogel frames are of great interest for the nanotechnology revolution due to their extremely high porosity and large specific surface area. Advanced Materials (advanced Materials, 30 th 2018) states that aerogels assembled from colloidal metal or semiconductor Nanocrystals (NCs) have large surface areas, ultra-low densities and high porosities, and are therefore attractive in a variety of applications, such as catalysis, sensors, energy storage and electronics.
Currently, the following reports can be found for preparing metal or semiconductor nanomaterial aerogel by assembly induction: journal of the american chemical society (j.am. Chem.soc.2014, page 7993 in 136) reports that nanoparticles are induced to self-assemble by oxidation of Ag nanoparticle surface ligands, thereby forming a silver nanoparticle hydrogel. The basic process of the method is as follows: centrifugally cleaning the synthesized silver nanoparticles, re-dispersing the silver nanoparticles in water, performing rotary evaporation to prepare high-concentration silver nanoparticle sol, adding a proper amount of acetone solution of tetranitromethane, violently shaking, standing for a period of time in a dark environment to obtain silver nanoparticle hydrogel, and finally performing supercritical drying by carbon dioxide to obtain the silver nanoparticle aerogel. The method has complicated steps, and the prepared gel is fragile and has low mechanical strength.
German applied chemistry (angew.chem.int.ed.2016, 55 th 6334) reports that a chemical bond is formed between a cation and an anionic ligand on the surface of a nanoparticle, so that the nanoparticle is induced to assemble, and a cadmium selenide three-dimensional hydrogel is formed. The basic process of the method comprises the following steps: and (3) carrying out ligand exchange on the cadmium selenide particles synthesized by the oil phase to exchange surface ligands for iodide ions. And (2) re-dispersing the ligand-exchanged nanoparticles into MFA, adding a certain amount of cadmium acetate, standing at normal temperature for a period of time to form cadmium selenide hydrogel, and finally performing supercritical drying by carbon dioxide to form the cadmium selenide aerogel. The method has complicated steps and long time consumption.
Disclosure of Invention
In view of the above, the present invention aims to provide a three-dimensional aerogel containing Te nanowires, a preparation method and applications thereof, wherein the method is simple and can assemble isotropic three-dimensional aerogel containing Te nanowires with uniform size.
The invention provides a preparation method of Te nanowire three-dimensional aerogel, which comprises the following steps:
dispersing one-dimensional Te nano-wires in an alcohol solvent, pre-assembling the one-dimensional Te nano-wires with lead nitrate, and then carrying out hydrothermal reaction in a high-pressure reaction kettle to obtain three-dimensional Te nano-wire hydrogel;
and (3) carrying out supercritical drying on the Te nanowire three-dimensional hydrogel to obtain the Te nanowire three-dimensional aerogel.
Preferably, the temperature of the hydrothermal reaction is 110-140 ℃; the time of the hydrothermal reaction is 30 to 40 hours.
Preferably, the mass ratio of the lead nitrate to the one-dimensional Te nanowire is 1.50-0.55.
Preferably, the alcoholic solvent is selected from ethylene glycol.
Preferably, the diameter of the one-dimensional Te nanowire is 5-20 nm.
Preferably, the supercritical drying is carbon dioxide supercritical drying.
Preferably, the one-dimensional Te nanowire is prepared by the following method:
mixing sodium tellurite, polyvinylpyrrolidone and water, adding ammonia water and hydrazine hydrate, and reacting to obtain the one-dimensional Te nanowire.
Preferably, the reaction temperature is 175-190 ℃, and the reaction time is 2.5-3.5 h.
The invention provides a Te nanowire three-dimensional aerogel which is prepared by the preparation method of the technical scheme.
The invention provides the application of the Te nanowire three-dimensional aerogel prepared by the preparation method in the technical scheme or the application of the Te nanowire three-dimensional aerogel in catalysis, sensors, energy storage or electronic devices in the technical scheme.
The invention provides a preparation method of Te nanowire three-dimensional aerogel, which comprises the following steps: dispersing one-dimensional Te nano-wires in an alcohol solvent, pre-assembling the one-dimensional Te nano-wires with lead nitrate, and then carrying out hydrothermal reaction in a high-pressure reaction kettle to obtain three-dimensional Te nano-wire hydrogel; and (3) carrying out supercritical drying on the Te nanowire three-dimensional hydrogel to obtain the Te nanowire three-dimensional aerogel. The one-dimensional Te nano-wire is pre-assembled under the induction of lead ions; and heating to form a two-dimensional nanobelt by the assembled nanowires, and forming a cross-linked network structure in the three-dimensional direction to finally obtain the macroscale three-dimensional Te nanowire hydrogel. The method is simple, and isotropic three-dimensional Te nano-wires with uniform size can be assembled.
Drawings
FIG. 1 is a TEM image of 7nmTe nanowires in example 1 of the present invention;
FIG. 2 is a TEM image of pre-assembly of Te nanowires in example 1 of the present invention;
FIG. 3 is a transmission electron microscope image of a Te nanowire hydrogel in example 1 of the present invention;
fig. 4 is an optical photograph of the Te nanowire hydrogel in example 1 of the present invention;
fig. 5 is an optical photograph of the Te nanowire aerogel after carbon dioxide supercritical drying in example 1 of the present invention;
fig. 6 is a scanning electron microscope photograph of the three-dimensional Te nanowire aerogel in example 1 of the present invention.
Detailed Description
The invention provides a preparation method of Te nanowire three-dimensional aerogel, which comprises the following steps:
dispersing one-dimensional Te nano-wires in an alcohol solvent, pre-assembling the one-dimensional Te nano-wires with lead nitrate, and then carrying out hydrothermal reaction in a high-pressure reaction kettle to obtain three-dimensional Te nano-wire hydrogel;
and (3) carrying out supercritical drying on the Te nanowire three-dimensional hydrogel to obtain the Te nanowire three-dimensional aerogel.
The method comprises the steps of firstly providing one-dimensional Te nanowires, then dispersing the one-dimensional Te nanowires into ethylene glycol again, adding lead nitrate to pre-assemble the nanowires, then pouring the solution into a reaction kettle substrate, reacting for a period of time at high temperature and high pressure to form the macroscale three-dimensional Te wire hydrogel, and drying the hydrogel through carbon dioxide supercritical to obtain the macroscale three-dimensional Te wire aerogel. The method is simple and short in time consumption.
The one-dimensional Te nano-wire is dispersed in an alcohol solvent, and is subjected to hydrothermal reaction in a high-pressure reaction kettle after being pre-assembled with lead nitrate to obtain the three-dimensional Te nano-wire hydrogel.
In the invention, the one-dimensional Te nanowire is prepared by the following method:
mixing sodium tellurite, polyvinylpyrrolidone and water, adding ammonia water and hydrazine hydrate, and reacting to obtain the one-dimensional Te nanowire.
In the invention, the ratio of the mass of the sodium tellurite, the mass of the polyvinylpyrrolidone, the volume of the water, the volume of the ammonia water and the volume of the hydrazine hydrate is preferably (0.9-1.0) g, (9.5-10.5) g, (310-350) mL, (32-35) mL: (15-18) mL.
Mixing the raw materials in a reaction kettle, mixing for 10min, and placing in an oven for reaction; the reaction temperature is preferably 175-190 ℃, and the reaction time is 2.5-3.5 h. In the specific example, the reaction temperature is 180 ℃ and the reaction time is 3h.
In the invention, the diameter of the one-dimensional Te nanowire is preferably 5-20 nm; the diameter of the one-dimensional Te nano-wire cannot be too thick or too thin, otherwise, a Te nano-wire three-dimensional assembly cannot be obtained.
The invention preferably adds acetone into the one-dimensional Te nano-wire for centrifugal precipitation, and the one-dimensional Te nano-wire is cleaned by ethanol and then dispersed in the alcohol solvent after centrifugation.
In the present invention, the mass ratio of the amount of lead nitrate added to the Te wire is preferably 1.
In the present invention, the alcohol solvent is preferably ethylene glycol; the mass ratio of the volume of the alcohol solvent to the lead nitrate is (35-45) mL:1g; in the specific embodiment, the mass ratio of the volume of the ethylene glycol to the mass of the lead nitrate is 40mL.
In the invention, the temperature of the hydrothermal reaction is preferably 110-140 ℃; the time of the hydrothermal reaction is 30-40 h; in a specific embodiment, the temperature of the hydrothermal reaction is 120 ℃, and the time of the hydrothermal reaction is 36h.
After the Te nanowire three-dimensional hydrogel is obtained, the Te nanowire three-dimensional hydrogel is subjected to supercritical drying to obtain the Te nanowire three-dimensional aerogel. The supercritical drying is preferably carried out by using carbon dioxide.
In order to further illustrate the present invention, the following examples are provided to describe in detail a Te nanowire three-dimensional aerogel, its preparation method and its application, but they should not be construed as limiting the scope of the present invention.
Example 1
Synthesis of tellurium nanowires with diameter of 7nm
Adding 0.922g of sodium tellurite, 10g of polyvinylpyrrolidone and 330mL of deionized water into a 500mL reaction kettle, stirring and dissolving, adding 33.5mL of ammonia water and 16.5mL of hydrazine hydrate, stirring for 10min, placing the mixture into an oven at 180 ℃ for reaction for 3 hours, taking out the reaction kettle, and naturally cooling to room temperature.
Synthesis of three-dimensional Te nanowire hydrogel
And adding acetone into 0.52g of 500mL of Te nanowire obtained by the preparation method for centrifugal precipitation, washing with ethanol once, centrifuging again, dispersing in 40mL of ethylene glycol, adding 1g of lead nitrate, stirring until the lead nitrate is completely dissolved, putting into a 50mL reaction kettle, carrying out hydrothermal treatment at 120 ℃ for 36 hours, cooling, and taking out to obtain the three-dimensional Te nanowire hydrogel. And (4) performing supercritical drying on carbon dioxide to obtain the three-dimensional Te nanowire aerogel.
FIG. 1 is a TEM image of 7nmTe nanowires in example 1 of the present invention; as can be seen from fig. 1: the Te nano-wires are uniform in size.
FIG. 2 is a TEM image of pre-assembly of Te nanowires in example 1 of the present invention; as can be seen in fig. 2: the discrete nanowires are pre-assembled.
FIG. 3 is a transmission electron microscope image of a Te nanowire hydrogel in example 1 of the present invention; as can be seen in fig. 3: the pre-assembled nanowires form nanoribbons.
Fig. 4 is an optical photograph of the Te nanowire hydrogel in example 1 of the present invention;
fig. 5 is an optical photograph of the Te nanowire aerogel after carbon dioxide supercritical drying in example 1 of the present invention;
fig. 6 is a scanning electron microscope photograph of the three-dimensional Te nanowire aerogel in example 1 of the present invention.
From the above embodiments, the invention provides a preparation method of a Te nanowire three-dimensional aerogel, which comprises the following steps: dispersing one-dimensional Te nano-wires in an alcohol solvent, pre-assembling the Te nano-wires with lead nitrate, and then carrying out hydrothermal reaction in a high-pressure reaction kettle to obtain three-dimensional Te nano-wire hydrogel; and (3) carrying out supercritical drying on the Te nanowire three-dimensional hydrogel to obtain the Te nanowire three-dimensional aerogel. The one-dimensional Te nano-wire is pre-assembled under the induction of lead ions; and heating to enable the assembled nanowires to form a two-dimensional nanobelt, and forming a cross-linked network structure in the three-dimensional direction to finally obtain the macroscale three-dimensional Te nanowire hydrogel. The method is simple, and isotropic three-dimensional Te nano-wires with uniform size can be assembled.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A preparation method of Te nanowire three-dimensional aerogel comprises the following steps:
dispersing one-dimensional Te nano-wires in an alcohol solvent, pre-assembling the one-dimensional Te nano-wires with lead nitrate, and then carrying out solvothermal reaction in a high-pressure reaction kettle to obtain Te nano-wire three-dimensional gel; the alcohol solvent is selected from ethylene glycol;
performing supercritical drying on the Te nanowire three-dimensional gel to obtain the Te nanowire three-dimensional aerogel;
the one-dimensional Te nanowire is prepared by the following method:
mixing sodium tellurite, polyvinylpyrrolidone and water, adding ammonia water and hydrazine hydrate, and reacting to obtain a one-dimensional Te nanowire; the diameter of the one-dimensional Te nano-wire is 5-20nm;
the temperature of the solvothermal reaction is 110 to 140 ℃; the solvothermal reaction time is 30 to 40h.
2. The preparation method according to claim 1, wherein the mass ratio of the lead nitrate to the one-dimensional Te nanowire is 1.
3. The production method according to claim 1, wherein the supercritical drying is carbon dioxide supercritical drying.
4. The preparation method according to claim 1, wherein the reaction temperature is 175 to 190 ℃ after the ammonia water and hydrazine hydrate are added; the reaction time is 2.5 to 3.5 hours.
5. A Te nanowire three-dimensional aerogel prepared by the method of any of claims 1~4.
6. Use of the Te nanowire three-dimensional aerogel prepared by the preparation method of any one of claims 1~4 in catalysis, sensors, energy storage or electronic devices.
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| CN102086025A (en) * | 2011-01-07 | 2011-06-08 | 中国科学技术大学 | Preparation method of one-dimensional (1D) flexible nano-material assembly body |
| CN102910595A (en) * | 2012-10-31 | 2013-02-06 | 中国科学技术大学 | Macro preparation method for superfine tellurium nanowires |
| CN102985359A (en) * | 2010-04-23 | 2013-03-20 | 普度研究基金会 | Ultrathin nanowire-based and nanoscale heterostructure-based thermoelectric conversion structures and method of making same |
| CN109179340A (en) * | 2018-09-18 | 2019-01-11 | 西安交通大学 | Lead base chalcogenide alloy particle with nanostructure and preparation method thereof |
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| TWI610463B (en) * | 2016-07-11 | 2018-01-01 | 國立清華大學 | Method for forming tellurium/telluride nanowire arrays on a conductive substrate and tellurium/telluride nanowire thermoelectric device |
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| CN102985359A (en) * | 2010-04-23 | 2013-03-20 | 普度研究基金会 | Ultrathin nanowire-based and nanoscale heterostructure-based thermoelectric conversion structures and method of making same |
| CN102086025A (en) * | 2011-01-07 | 2011-06-08 | 中国科学技术大学 | Preparation method of one-dimensional (1D) flexible nano-material assembly body |
| CN102910595A (en) * | 2012-10-31 | 2013-02-06 | 中国科学技术大学 | Macro preparation method for superfine tellurium nanowires |
| CN109179340A (en) * | 2018-09-18 | 2019-01-11 | 西安交通大学 | Lead base chalcogenide alloy particle with nanostructure and preparation method thereof |
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