CN110078031A - A kind of Te nano wire three-dimensional aeroge, preparation method and its application - Google Patents
A kind of Te nano wire three-dimensional aeroge, preparation method and its application Download PDFInfo
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- CN110078031A CN110078031A CN201910446022.3A CN201910446022A CN110078031A CN 110078031 A CN110078031 A CN 110078031A CN 201910446022 A CN201910446022 A CN 201910446022A CN 110078031 A CN110078031 A CN 110078031A
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Abstract
The present invention provides a kind of Te nano wire three-dimensional aeroge, preparation method and its applications, method is the following steps are included: one-dimensional Te nano wire is dispersed in alcohols solvent, with with plumbi nitras it is pre-assembled after carry out hydro-thermal reaction in a high pressure reaction kettle, obtain Te nano wire three dimensional hydrogel；By the Te nano wire three dimensional hydrogel supercritical drying, Te nano wire three-dimensional aeroge is obtained.The present invention carries out one-dimensional Te nano wire pre-assembled under the induction of lead ion；Heating makes the nano wire of assembling form two-dimensional nano band, forms cross-linked structure on three-dimensional, finally obtains macro-scale three-dimensional Te nano wire hydrogel.This method is simple, and being capable of the uniform isotropic three-dimensional Te nano wire of package size.
Description
Technical field
The invention belongs to nanomaterial assembly technical field more particularly to a kind of Te nano wire three-dimensional aeroges, its preparation
Method and its application.
Background technique
The controlledly synthesis of metal or semiconductor nano material effectively assembles, and the design of the device based on nano material
It is one of its premise for moving towards useization and guarantee with performance study." German applied chemistry "
(54 phase of Angew.Chem.Int.Ed.2015 page 13101) points out with nano material group existing for macroscopical aeroge frame form
Part causes the great interest of nanotechnology revolution due to its high porosity and big specific surface area." advanced material "
(Advance Materials, the 30th phase in 2018) points out, the gas assembled by colloidal metal or semiconductor nanocrystal (NCs)
Gel has big surface area, extremely-low density and high porosity, therefore attractive in various applications, such as is catalyzed, and passes
Sensor, energy storage and electronic device.
Metal or semiconductor nano material aeroge are prepared about assembling induction at present, it is seen that following some reports: " beauty
State's Society will " (136 phase of J.Am.Chem.Soc.2014 page 7993) report through Ag nano grain surface ligand
Oxidation, induction nano particle carries out self assembly, and then forms silver nano-grain hydrogel.The basic process of the method is: will close
It is dispersed in water again at good silver nano-grain eccentric cleaning, the silver nano-grain for then carrying out revolving preparation high concentration is molten
Glue, then in the acetone soln that suitable tetranitromethane is wherein added, a period of time is stood under dark surrounds after acutely rocking,
Silver nano-grain hydrogel can be obtained, be dried to obtain silver nano-grain aeroge finally by CO 2 supercritical.The party
Method complex steps, and manufactured gel is frangible, mechanical strength is low.
" German applied chemistry " (55 phase of Angew.Chem.Int.Ed.2016 page 6334) report by cation with
The anion ligand of nano grain surface forms chemical bond, induction nano particle assembling, and then forms cadmium selenide three dimensional hydrogel.
The basic process of the method: the cadmium selenide particle that oil is combined to carries out ligand exchange, and surface ligand is made to change iodide ion into.It will match
Nano particle after body exchange is re-dispersed into MFA, and a certain amount of cadmium acetate is added, and stands a period of time at normal temperature, i.e.,
Cadmium selenide hydrogel can be formed, forms cadmium selenide aeroge finally by CO 2 supercritical drying.This method complex steps,
It takes a long time.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of Te nano wire three-dimensional aeroge, preparation method and its answering
With this method is simple, and being capable of the uniform isotropic three-dimensional Te nano wire aeroge of package size.
The present invention provides a kind of preparation methods of Te nano wire three-dimensional aeroge, comprising the following steps:
One-dimensional Te nano wire is dispersed in alcohols solvent, with plumbi nitras it is pre-assembled after carry out water in a high pressure reaction kettle
Thermal response obtains Te nano wire three dimensional hydrogel；
By the Te nano wire three dimensional hydrogel supercritical drying, Te nano wire three-dimensional aeroge is obtained.
Preferably, the temperature of the hydro-thermal reaction is 110~140 DEG C；The time of hydro-thermal reaction is 30~40h.
Preferably, the mass ratio of the plumbi nitras and one-dimensional Te nano wire is 1:0.50~0.55.
Preferably, the alcohols solvent is selected from ethylene glycol.
Preferably, the diameter of the one-dimensional Te nano wire is 5~20nm.
Preferably, the supercritical drying is dry using CO 2 supercritical.
Preferably, the one-dimensional Te nano wire is made by following methods:
After sodium tellurite, polyvinylpyrrolidone and water are mixed, ammonium hydroxide and hydrazine hydrate is added, reaction obtains one-dimensional Te
Nano wire.
Preferably, the temperature of the reaction is 175~190 DEG C, and the time of reaction is 2.5~3.5h.
The present invention provides a kind of Te nano wire three-dimensional aeroge, the preparation method as described in above-mentioned technical proposal is made.
The present invention provides Te nano wire three-dimensional aeroge made from preparation method described in a kind of above-mentioned technical proposal or on
State application of the Te nano wire three-dimensional aeroge in catalysis, sensor, energy storage or electronic device described in technical solution.
The present invention provides a kind of preparation methods of Te nano wire three-dimensional aeroge, comprising the following steps: receives one-dimensional Te
Rice noodles are dispersed in alcohols solvent, with plumbi nitras it is pre-assembled after carry out hydro-thermal reaction in a high pressure reaction kettle, obtain Te nanometers
Line three dimensional hydrogel；By the Te nano wire three dimensional hydrogel supercritical drying, Te nano wire three-dimensional aeroge is obtained.The present invention
One-dimensional Te nano wire is carried out under the induction of lead ion pre-assembled；Heating make assembling nano wire formed two-dimensional nano band, three
Dimension side is upwardly formed cross-linked structure, finally obtains macro-scale three-dimensional Te nano wire hydrogel.This method is simple, and can
The uniform isotropic three-dimensional Te nano wire of package size.
Detailed description of the invention
Fig. 1 is the transmission electron microscope figure of 7nmTe nano wire in the embodiment of the present invention 1；
Fig. 2 is the pre-assembled transmission electron microscope figure of Te nano wire in the embodiment of the present invention 1；
Fig. 3 is the transmission electron microscope figure of Te nano wire hydrogel in the embodiment of the present invention 1；
Fig. 4 is the optical photograph of Te nano wire hydrogel in the embodiment of the present invention 1；
Fig. 5 is the optical photograph of the Te nano wire aeroge in the embodiment of the present invention 1 after CO 2 supercritical drying；
Fig. 6 is the electron scanning micrograph of three-dimensional Te nano wire aeroge in the embodiment of the present invention 1.
Specific embodiment
The present invention provides a kind of preparation methods of Te nano wire three-dimensional aeroge, comprising the following steps:
One-dimensional Te nano wire is dispersed in alcohols solvent, with plumbi nitras it is pre-assembled after carry out water in a high pressure reaction kettle
Thermal response obtains Te nano wire three dimensional hydrogel；
By the Te nano wire three dimensional hydrogel supercritical drying, Te nano wire three-dimensional aeroge is obtained.
The present invention first provides one-dimensional Te nano wire, and then one-dimensional Te nano wire is re-dispersed into ethylene glycol, and nitre is added
Lead plumbate carries out the pre-assembled of nano wire, then pours solution into reaction kettle substrate, after reacting a period of time at high temperature under high pressure, shape
At macro-scale three-dimensional Te line hydrogel, hydrogel is dry by CO 2 supercritical, and macro-scale three-dimensional Te can be obtained
Line aeroge.This method is simple, time-consuming shorter.
One-dimensional Te nano wire is dispersed in alcohols solvent by the present invention, with plumbi nitras it is pre-assembled after in a high pressure reaction kettle
Hydro-thermal reaction is carried out, Te nano wire three dimensional hydrogel is obtained.
In the present invention, the one-dimensional Te nano wire is made by following methods:
After sodium tellurite, polyvinylpyrrolidone and water are mixed, ammonium hydroxide and hydrazine hydrate is added, reaction obtains one-dimensional Te
Nano wire.
In the present invention, the quality of the sodium tellurite, the quality of polyvinylpyrrolidone, the volume of water, ammonium hydroxide body
Long-pending and hydrazine hydrate volume ratio is preferably (0.9~1.0) g:(9.5~10.5) g:(310~350) mL:(32~35) mL:(15
~18) mL.
Above-mentioned raw materials are mixed in a kettle, are placed in baking oven and are reacted again after mixing 10min；The reaction
Temperature is preferably 175~190 DEG C, and the time of reaction is 2.5~3.5h.In specific embodiment, the temperature of reaction is 180 DEG C, instead
The time answered is 3h.
In the present invention, the diameter of the one-dimensional Te nano wire is preferably 5~20nm；The diameter of the one-dimensional Te nano wire
Cannot excessively slightly can not be meticulous, otherwise cannot get Te nano wire three-dimensional assembly.
One-dimensional Te nano wire is preferably added acetone centrifugation by the present invention, ethyl alcohol cleans one time be centrifuged again after be dispersed in alcohols
In solvent.
In the present invention, the mass ratio of the additional amount of the plumbi nitras and Te line is preferably 1:0.50~0.55, more preferably
For 1:0.52.
In the present invention, the alcohols solvent is preferably ethylene glycol；The volume of the alcohols solvent and the quality of plumbi nitras
Than for (35~45) mL:1g；In specific embodiment, the volume of ethylene glycol and the mass ratio of plumbi nitras are 40mL:1g.
In the present invention, the temperature of the hydro-thermal reaction is preferably 110~140 DEG C；The time of hydro-thermal reaction be 30~
40h；In specific embodiment, the temperature of the hydro-thermal reaction is 120 DEG C, and the time of hydro-thermal reaction is 36h.
After obtaining Te nano wire three dimensional hydrogel, the present invention obtains the Te nano wire three dimensional hydrogel supercritical drying
To Te nano wire three-dimensional aeroge.Present invention preferably employs carbon dioxide to carry out supercritical drying.
In order to further illustrate the present invention, below with reference to embodiment to a kind of Te nano wire three-dimensional airsetting provided by the invention
Glue, preparation method and its application are described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
The synthesis of diameter 7nm tellurium nano-wire
0.922g sodium tellurite, 10g polyvinylpyrrolidone, the stirring of 330mL deionized water are added in 500mL reaction kettle
After dissolution, 33.5mL ammonium hydroxide is added, 16.5mL hydrazine hydrate is put into 180 DEG C of baking ovens and reacts 3 hours after stirring 10min, takes out
Reaction kettle, cooled to room temperature.
The synthesis of three-dimensional Te nano wire hydrogel
The Te nano wire 0.52g for the 500mL that the method for being prepared as described above obtains is added into acetone centrifugation, ethyl alcohol cleans one time
It is centrifuged, is dispersed in 40mL ethylene glycol again, the plumbi nitras of 1g is added, stirring is completely dissolved to plumbi nitras, is put into 50mL reaction kettle
In 120 DEG C hydro-thermal 36 hours, taken out after cooling and obtain three-dimensional Te nano wire hydrogel.After CO 2 supercritical is dry, obtain
Three-dimensional Te nano wire aeroge.
Fig. 1 is the transmission electron microscope figure of 7nmTe nano wire in the embodiment of the present invention 1；As seen from Figure 1: Te receives
Rice noodles size uniformity.
Fig. 2 is the pre-assembled transmission electron microscope figure of Te nano wire in the embodiment of the present invention 1；Fig. 2 is it can be seen that at random
Nano wire carried out it is pre-assembled.
Fig. 3 is the transmission electron microscope figure of Te nano wire hydrogel in the embodiment of the present invention 1；Fig. 3 is it can be seen that pre- group
The nano wire of dress forms nanobelt.
Fig. 4 is the optical photograph of Te nano wire hydrogel in the embodiment of the present invention 1；
Fig. 5 is the optical photograph of the Te nano wire aeroge in the embodiment of the present invention 1 after CO 2 supercritical drying；
Fig. 6 is the electron scanning micrograph of three-dimensional Te nano wire aeroge in the embodiment of the present invention 1.
As seen from the above embodiment, the present invention provides a kind of preparation methods of Te nano wire three-dimensional aeroge, including with
Lower step: one-dimensional Te nano wire is dispersed in alcohols solvent, with plumbi nitras it is pre-assembled after carry out water in a high pressure reaction kettle
Thermal response obtains Te nano wire three dimensional hydrogel；By the Te nano wire three dimensional hydrogel supercritical drying, Te nano wire is obtained
Three-dimensional aeroge.The present invention carries out one-dimensional Te nano wire pre-assembled under the induction of lead ion；Heating makes the nano wire of assembling
Two-dimensional nano band is formed, cross-linked structure is formed on three-dimensional, finally obtains macro-scale three-dimensional Te nano wire hydrogel.
This method is simple, and being capable of the uniform isotropic three-dimensional Te nano wire of package size.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of Te nano wire three-dimensional aeroge, comprising the following steps:
One-dimensional Te nano wire is dispersed in alcohols solvent, with plumbi nitras it is pre-assembled after to carry out hydro-thermal in a high pressure reaction kettle anti-
It answers, obtains Te nano wire three dimensional hydrogel；
By the Te nano wire three dimensional hydrogel supercritical drying, Te nano wire three-dimensional aeroge is obtained.
2. preparation method according to claim 1, which is characterized in that the temperature of the hydro-thermal reaction is 110~140 DEG C；
The time of hydro-thermal reaction is 30~40h.
3. preparation method according to claim 1, which is characterized in that the mass ratio of the plumbi nitras and one-dimensional Te nano wire
For 1:0.50~0.55.
4. preparation method according to claim 1, which is characterized in that the alcohols solvent is selected from ethylene glycol.
5. preparation method according to claim 1, which is characterized in that the diameter of the one-dimensional Te nano wire is 5~20nm.
6. preparation method according to claim 1, which is characterized in that the supercritical drying uses CO 2 supercritical
It is dry.
7. preparation method according to claim 1, which is characterized in that the one-dimensional Te nano wire is made by following methods:
After sodium tellurite, polyvinylpyrrolidone and water are mixed, ammonium hydroxide and hydrazine hydrate is added, reaction obtains Te nanometers one-dimensional
Line.
8. preparation method according to claim 7, which is characterized in that the temperature of the reaction is 175~190 DEG C, reaction
Time be 2.5~3.5h.
9. a kind of Te nano wire three-dimensional aeroge is made by any one of claim 1~8 preparation method.
10. Te nano wire three-dimensional aeroge or claim 9 made from a kind of any one of claim 1~8 preparation method
Application of the Te nano wire three-dimensional aeroge in catalysis, sensor, energy storage or electronic device.
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| CN201910446022.3A CN110078031B (en) | 2019-05-27 | 2019-05-27 | Te nanowire three-dimensional aerogel, and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111250007A (en) * | 2020-01-17 | 2020-06-09 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Preparation method of pure metal aerogel and flexible composite material |
| CN115432692A (en) * | 2022-05-23 | 2022-12-06 | 复旦大学 | One-dimensional soft interface nanowire and super-assembly preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111250007A (en) * | 2020-01-17 | 2020-06-09 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Preparation method of pure metal aerogel and flexible composite material |
| CN115432692A (en) * | 2022-05-23 | 2022-12-06 | 复旦大学 | One-dimensional soft interface nanowire and super-assembly preparation method thereof |
| CN115432692B (en) * | 2022-05-23 | 2023-12-08 | 复旦大学 | One-dimensional soft interface nanowire and super-assembly preparation method thereof |
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