CN103613759A - Preparation method of MoO3/polyaniline coaxial nano heterojunction - Google Patents

Preparation method of MoO3/polyaniline coaxial nano heterojunction Download PDF

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CN103613759A
CN103613759A CN201310658871.8A CN201310658871A CN103613759A CN 103613759 A CN103613759 A CN 103613759A CN 201310658871 A CN201310658871 A CN 201310658871A CN 103613759 A CN103613759 A CN 103613759A
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moo
polyaniline
solution
deionized water
stirring
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CN103613759B (en
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胡俊青
蒋扉然
李文尧
邹儒佳
徐开兵
李博
安磊
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Donghua University
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Abstract

The invention relates to a preparation method of a MoO3/polyaniline coaxial nano heterojunction. The preparation method comprises the following steps: (1) dropwise adding H2O2 into metal molybdenum powder under a condition of an ice water bath, and stirring and fixing the volume to obtain precursor liquor; (2) adding deionized water into the precursor liquor, stirring at room temperature and carrying out a hydrothermal reaction, after reaction, naturally cooling to room temperature, and washing the product by excessive ethanol, and finally, carrying out centrifugal separation to obtain a MoO3 nano belt; and (3) adding deionized water into the MoO3 nano belt to obtain liquor A; dropwise adding hydrochloric acid liquor of aniline into the liquor A while stirring, and then adding deionized water liquor of ammonium persulfate, and stirring for 1-24 hours at constant temperature; and after reaction, washing, centrifugalizing and vacuum-drying to obtain the MoO3/polyaniline coaxial nano heterojunction. The preparation method provided by the invention is simple to operate, free from complex equipment and relatively easily controlled in components, and the heterojunction can be produced on a large scale and has a wide application prospect.

Description

A kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction
Technical field
The invention belongs to polyaniline nano Material Field, particularly a kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction.
Background technology
Transition metal oxide molybdic oxide has the character such as electrochromism, photochromic, photocatalytic degradation and gas-sensitive property, in fast ion conduction, catalyzer, sensor and electrochemical field, all has widespread use.Molybdic oxide has three kinds of common phases: quadrature phase (α-MoO 3), monoclinic phase (β-MoO 3) and six side's phase (h-MoO 3), the former belongs to thermodynamically stable phase, and both belong to the thermodynamics steady phase that is situated between afterwards.Quadrature phase MoO wherein 3because of its unique one dimension laminate structure, make it be widely used in the electrode materials in electrochemical energy storing device, as lithium ion primary cell, lithium-ion secondary cell, ultracapacitor etc., at present, MoO 3the application aspect electrochemical field such as nanometer rod, nanometer sheet, nano wire, nano belt has corresponding report.But molybdic oxide ion and electronic conduction rate variance, this is just restricted its chemical property, thereby improve the focus that its electroconductibility just becomes research, and the means such as employing is coated, hydridization doping can effectively be improved its electroconductibility.Be combined together to form matrix material with conducting polymer and can solve these defects, and obtain more superior performance by the synergy of each several part.
Since American scientist black square (A.J.Heeger), MacDiarmid (A.G.MacDiamid) and Japanese scientist's Hideki Shirakawa (H.Shirakawa) in 1977 find that doped polyacetylene has metallic conductivity, polymkeric substance can not thoroughly be changed as the concept of electro-conductive material, and from then on conductive polymers has been subject to various countries scientists' extensive concern.Common conductive polymers has Polythiophene, polypyrrole, polyaniline etc., and wherein polyaniline synthesizes simply because it has, and can pass through electrochemical oxidation, chemical syntheses; Raw material is easy to get; The advantages such as high temperature resistant and good in oxidation resistance, become the conducting polymer composite of tool prospect.The performances such as the conduction of polyaniline and catalysis depend on dopant states and the structure of polymkeric substance to a great extent, can be by changing the redox state, doping agent of polyaniline or by improving the performance of polyaniline with inorganic compounding, electrically conductive polyaniline/inorganic materials matrix material combines the premium properties of superpolymer and inorganic materials, thereby can have by compound acquisition the functional materials of the performances such as special optical, electrical, magnetic, catalysis.
At present, generally adopt intercalation polymeric method that aniline monomer is inserted to molybdic oxide interlayer, obtain MoO 3with the hybrid material of polyaniline, because the oxidisability of molybdic oxide own is very weak and there is no tradable ion, therefore polyaniline is inserted into MoO 3interlayer is very difficult, and method is complicated, and therefore complex steps needs a kind of polyaniline-coated MoO for preparing simply efficiently of exploitation 3the preparation method of matrix material.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction, this preparation method is simple to operate, does not need complex apparatus, obtains evenly coated MoO of polyaniline 3nano composite material.
A kind of MoO of the present invention 3the preparation method of/polyaniline co-axial nano heterojunction, comprising:
(1) presoma is synthetic:
By H 2o 2in the metal molybdenum powder being slowly added drop-wise under ice-water bath condition, and constantly stir to avoid overheated, a large amount of heat and gas are emitted in reaction; After dropwising, under normal temperature, continue to stir 2-8 hour, obtain the peroxide molybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume obtains precursor solution;
(2) MoO 3synthesizing of nano belt:
In above-mentioned precursor solution, add deionized water, after stirring and at 60-180 ℃, carry out hydro-thermal reaction 6-24 hour under room temperature, after reaction finishes, naturally cool to room temperature, by excessive washing with alcohol for product, last centrifugation obtains MoO 3nano belt;
(3) polyaniline-coated MoO 3nano belt:
At MoO 3in nano belt, add deionized water, then the ultrasonic 0.5～1h of room temperature, makes MoO 3nano belt is dispersed in water, obtains A solution; According to MoO 3the mol ratio of nano belt and aniline is 1:0.25～2, while stirring the hydrochloric acid soln of aniline is added drop-wise in A solution, and then adds the deionized water solution of ammonium persulphate, stirring at normal temperature 1～24h; After reaction finishes, with excessive washing with alcohol, centrifugation, collecting precipitation thing, last vacuum-drying, obtains MoO 3/ polyaniline co-axial nano heterojunction.
H described in step (1) 2o 2with the amount ratio of metal molybdenum powder be 40mL:0.05mol, H used wherein 2o 2massfraction be 30%; Last constant volume obtains 100mL precursor solution.
MoO in A solution described in step (3) 3the concentration of nano belt is 0.01～0.03g/mL.
The concentration of the deionized water solution of the ammonium persulphate described in step (3) is 0.01～0.03g/mL.
Vacuum drying temperature described in step (3) is 60 ℃.
The present invention directly uses metal molybdenum powder for molybdenum source, and does not adopt under any template condition and prepare MoO 3nano belt.
Beneficial effect:
The present invention can prepare MoO with simple experimental installation 3/ polyaniline co-axial nano heterojunction; This reaction has the advantages such as environmental friendliness, required starting material are easy to get, cheap, operating process is easy, and can relatively largely prepare, and is preparation MoO 3a kind of new and effective method of/polyaniline co-axial nano heterojunction.
Accompanying drawing explanation
Fig. 1 is the MoO preparing in the present invention 3nano belt and MoO 3the SEM picture of/polyaniline co-axial nano heterojunction; Wherein (a) is MoO 3nano belt, (b) is MoO 3/ polyaniline co-axial nano heterojunction;
Fig. 2 is the MoO preparing in the present invention 3the TEM figure of/polyaniline co-axial nano heterojunction;
Fig. 3 is the MoO preparing in the present invention 3nano belt and MoO 3the FTIR collection of illustrative plates of/polyaniline co-axial nano heterojunction; Wherein (a) is MoO 3nano belt, (b) is MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
(1) presoma is synthetic: by 40mL H 2o 2under ice-water bath condition, be slowly added drop-wise in the metal molybdenum powder of 0.05mol, and constantly stir to avoid overheated.After dropwising, under normal temperature, continue to stir 4 hours, obtain the peroxide molybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, standby.
(2) measure 5mL peroxide molybdic acid precursor solution in beaker, add 15mL deionized water, room temperature lower magnetic force goes in autoclave after stirring 1h, and hydro-thermal reaction is 12 hours at 180 ℃, naturally cools to room temperature.By the white MoO of gained 3excessive washing with alcohol for precipitation, centrifugation, obtains MoO 3nano belt.
(3) take 0.1g MoO 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.01g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is A solution; 0.1g ammonium persulphate is added in 10mL deionized water, is made into the aqueous solution that concentration is 0.01g/ml, ultrasonic being uniformly dispersed, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:1, while stirring the hydrochloric acid soln of aniline is added drop-wise in A solution, obtains C solution, then B solution is joined in C solution to stirring at normal temperature 4h.After reaction finishes, with excessive washing with alcohol, centrifugation, collecting precipitation thing, is vacuum-drying at 60 ℃ in temperature, obtains MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment 2
(1) presoma is synthetic: by 40mL H 2o 2under ice-water bath condition, be slowly added drop-wise in the metal molybdenum powder of 0.05mol, and constantly stir to avoid overheated.After dropwising, under normal temperature, continue to stir 4 hours, obtain the peroxide molybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, standby.
(2) measure 10mL peroxide molybdic acid precursor solution in beaker, add 10mL deionized water, room temperature lower magnetic force goes in autoclave after stirring 1h, and hydro-thermal reaction is 12 hours at 180 ℃, naturally cools to room temperature.By the white MoO of gained 3excessive washing with alcohol for precipitation, centrifugation, obtains MoO 3nano belt.
(3) take 0.1g MoO 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.01g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is A solution; 0.1g ammonium persulphate is added in 10mL deionized water, is made into the aqueous solution that concentration is 0.01g/ml, ultrasonic being uniformly dispersed, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:1, while stirring the hydrochloric acid soln of aniline is added drop-wise in A solution, obtains C solution, then B solution is joined in C solution to stirring at normal temperature 4h.After reaction finishes, with excessive washing with alcohol, centrifugation, collecting precipitation thing, is vacuum-drying at 60 ℃ in temperature, obtains MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment 3
(1) presoma is synthetic: by 40mL H 2o 2under ice-water bath condition, be slowly added drop-wise in the metal molybdenum powder of 0.05mol, and constantly stir to avoid overheated.After dropwising, under normal temperature, continue to stir 4 hours, obtain the peroxide molybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, standby.
(2) measure 20mL peroxide molybdic acid precursor solution in beaker, room temperature lower magnetic force goes in autoclave after stirring 1h, and hydro-thermal reaction is 12 hours at 180 ℃, naturally cools to room temperature.By the white MoO of gained 3excessive washing with alcohol for precipitation, centrifugation, obtains MoO 3nano belt.
(3) take 0.1g MoO 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.01g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is A solution; 0.1g ammonium persulphate is added in 10mL deionized water, is made into the aqueous solution that concentration is 0.01g/ml, ultrasonic being uniformly dispersed, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:1, while stirring the hydrochloric acid soln of aniline is added drop-wise in A solution, obtains C solution, then B solution is joined in C solution to stirring at normal temperature 4h.After reaction finishes, with excessive washing with alcohol, centrifugation, collecting precipitation thing, is vacuum-drying at 60 ℃ in temperature, obtains MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment 4
(1) presoma is synthetic: by 40mL H 2o 2under ice-water bath condition, be slowly added drop-wise in the metal molybdenum powder of 0.05mol, and constantly stir to avoid overheated.After dropwising, under normal temperature, continue to stir 4 hours, obtain the peroxide molybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, standby.
(2) measure 10mL peroxide molybdic acid precursor solution in beaker, add 10mL deionized water, room temperature lower magnetic force goes in autoclave after stirring 1h, and hydro-thermal reaction is 12 hours at 180 ℃, naturally cools to room temperature.By the white MoO of gained 3excessive washing with alcohol for precipitation, centrifugation, obtains MoO 3nano belt.
(3) take 0.1g MoO 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.01g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is A solution; 0.1g ammonium persulphate is added in 10mL deionized water, is made into the aqueous solution that concentration is 0.01g/ml, ultrasonic being uniformly dispersed, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:1, while stirring the hydrochloric acid soln of aniline is added drop-wise in A solution, obtains C solution, then B solution is joined in C solution to stirring at normal temperature 12h.After reaction finishes, with excessive washing with alcohol, centrifugation, collecting precipitation thing, is vacuum-drying at 60 ℃ in temperature, obtains MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment 5
(1) presoma is synthetic: by 40mL H 2o 2under ice-water bath condition, be slowly added drop-wise in the metal molybdenum powder of 0.05mol, and constantly stir to avoid overheated.After dropwising, under normal temperature, continue to stir 4 hours, obtain the peroxide molybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, standby.
(2) measure 10mL peroxide molybdic acid precursor solution in beaker, add 10mL deionized water, room temperature lower magnetic force goes in autoclave after stirring 1h, and hydro-thermal reaction is 12 hours at 180 ℃, naturally cools to room temperature.By the white MoO of gained 3excessive washing with alcohol for precipitation, centrifugation, obtains MoO 3nano belt.
(3) take 0.1g MoO 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.01g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is A solution; 0.1g ammonium persulphate is added in 10mL deionized water, is made into the aqueous solution that concentration is 0.01g/ml, ultrasonic being uniformly dispersed, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:1, while stirring the hydrochloric acid soln of aniline is added drop-wise in A solution, obtains C solution, then B solution is joined in C solution to stirring at normal temperature 24h.After reaction finishes, with excessive washing with alcohol, centrifugation, collecting precipitation thing, is vacuum-drying at 60 ℃ in temperature, obtains MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment 6
(1) presoma is synthetic: by 40mL H 2o 2under ice-water bath condition, be slowly added drop-wise in the metal molybdenum powder of 0.05mol, and constantly stir to avoid overheated.After dropwising, under normal temperature, continue to stir 4 hours, obtain the peroxide molybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, standby.
(2) measure 10mL peroxide molybdic acid precursor solution in beaker, add 10mL deionized water, room temperature lower magnetic force goes in autoclave after stirring 1h, and hydro-thermal reaction is 12 hours at 180 ℃, naturally cools to room temperature.By the white MoO of gained 3excessive washing with alcohol for precipitation, centrifugation, obtains MoO 3nano belt.
(3) take 0.2g MoO 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.02g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is A solution; 0.2g ammonium persulphate is added in 10mL deionized water, is made into the aqueous solution that concentration is 0.02g/ml, ultrasonic being uniformly dispersed, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:0.25, while stirring the hydrochloric acid soln of aniline is added drop-wise in A solution, obtains C solution, then B solution is joined in C solution to stirring at normal temperature 8h.After reaction finishes, with excessive washing with alcohol, centrifugation, collecting precipitation thing, is vacuum-drying at 60 ℃ in temperature, obtains MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment 7
(1) presoma is synthetic: by 40mL H 2o 2under ice-water bath condition, be slowly added drop-wise in the metal molybdenum powder of 0.05mol, and constantly stir to avoid overheated.After dropwising, under normal temperature, continue to stir 4 hours, obtain the peroxide molybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, standby.
(2) measure 10mL peroxide molybdic acid precursor solution in beaker, add 10mL deionized water, room temperature lower magnetic force goes in autoclave after stirring 1h, and hydro-thermal reaction is 12 hours at 180 ℃, naturally cools to room temperature.The white MoO of gained just 3excessive washing with alcohol for precipitation, centrifugation, obtains MoO 3nano belt.
(3) take 0.3g MoO 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.03g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is A solution; 0.3g ammonium persulphate is added in 10mL deionized water, is made into the aqueous solution that concentration is 0.03g/ml, ultrasonic being uniformly dispersed, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:2, while stirring the hydrochloric acid soln of aniline is added drop-wise in A solution, obtains C solution, then B solution is joined in C solution to stirring at normal temperature 12h.After reaction finishes, with excessive washing with alcohol, centrifugation, collecting precipitation thing, is vacuum-drying at 60 ℃ in temperature, obtains MoO 3/ polyaniline co-axial nano heterojunction.

Claims (5)

1. a MoO 3the preparation method of/polyaniline co-axial nano heterojunction, comprising:
(1) by H 2o 2in the metal molybdenum powder being slowly added drop-wise under ice-water bath condition, after dropwising, continue to stir 2-8 hour under normal temperature, obtain the peroxide molybdic acid colloidal sol of orange, constant volume obtains precursor solution;
(2) in above-mentioned precursor solution, add deionized water, after stirring, carry out hydro-thermal reaction 6-24 hour at 60-180 ℃ under room temperature, after reaction finishes, naturally cool to room temperature, by excessive washing with alcohol for product, last centrifugation obtains MoO 3nano belt;
(3) at MoO 3in nano belt, add deionized water, then the ultrasonic 0.5～1h of room temperature, obtains A solution; According to MoO 3the mol ratio of nano belt and aniline is 1:0.25～2, while stirring the hydrochloric acid soln of aniline is added drop-wise in A solution, and then adds the deionized water solution of ammonium persulphate, stirring at normal temperature 1～24h; After reaction finishes, with excessive washing with alcohol, centrifugation, collecting precipitation thing, last vacuum-drying, obtains MoO 3/ polyaniline co-axial nano heterojunction.
2. a kind of MoO according to claim 1 3the preparation method of/polyaniline co-axial nano heterojunction, is characterized in that: the H described in step (1) 2o 2with the amount ratio of metal molybdenum powder be 40mL:0.05mol, H used wherein 2o 2massfraction be 30%; Last constant volume obtains 100mL precursor solution.
3. a kind of MoO according to claim 1 3the preparation method of/polyaniline co-axial nano heterojunction, is characterized in that: MoO in the A solution described in step (3) 3the concentration of nano belt is 0.01～0.03g/mL.
4. a kind of MoO according to claim 1 3the preparation method of/polyaniline co-axial nano heterojunction, is characterized in that: the concentration of the deionized water solution of the ammonium persulphate described in step (3) is 0.01～0.03g/mL.
5. a kind of MoO according to claim 1 3the preparation method of/polyaniline co-axial nano heterojunction, is characterized in that: the vacuum drying temperature described in step (3) is 60 ℃.
CN201310658871.8A 2013-12-06 2013-12-06 A kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction Expired - Fee Related CN103613759B (en)

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CN108728674A (en) * 2018-04-20 2018-11-02 中南大学 A method of it extracting molybdenum from thick molybdic acid and prepares molybdenum product
CN109427981A (en) * 2017-08-28 2019-03-05 Tcl集团股份有限公司 QLED device and preparation method thereof
CN109928427A (en) * 2019-03-21 2019-06-25 暨南大学 A kind of double ion intercalation molybdenum oxide nanometer sheet, hetero-junctions and preparation method thereof
CN113054116A (en) * 2019-12-28 2021-06-29 Tcl集团股份有限公司 Light emitting diode
CN113380555A (en) * 2021-06-08 2021-09-10 辽宁大学 Hexadecylamine intercalated alpha-MoO3Material, preparation method thereof and application of material as super capacitor electrode material
CN115160564A (en) * 2022-07-19 2022-10-11 湖北大学 Molybdenum oxide composite polyaniline nanofiber paper and preparation method thereof

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CN102086302A (en) * 2009-12-04 2011-06-08 复旦大学 Preparing method for molybdenum oxide - polyaniline composite nanowire and nanotube
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Publication number Priority date Publication date Assignee Title
CN109427981A (en) * 2017-08-28 2019-03-05 Tcl集团股份有限公司 QLED device and preparation method thereof
CN108728674A (en) * 2018-04-20 2018-11-02 中南大学 A method of it extracting molybdenum from thick molybdic acid and prepares molybdenum product
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CN109928427A (en) * 2019-03-21 2019-06-25 暨南大学 A kind of double ion intercalation molybdenum oxide nanometer sheet, hetero-junctions and preparation method thereof
CN113054116A (en) * 2019-12-28 2021-06-29 Tcl集团股份有限公司 Light emitting diode
CN113380555A (en) * 2021-06-08 2021-09-10 辽宁大学 Hexadecylamine intercalated alpha-MoO3Material, preparation method thereof and application of material as super capacitor electrode material
CN115160564A (en) * 2022-07-19 2022-10-11 湖北大学 Molybdenum oxide composite polyaniline nanofiber paper and preparation method thereof

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