CN102086302B - Preparing method for molybdenum oxide - polyaniline composite nanowire and nanotube - Google Patents
Preparing method for molybdenum oxide - polyaniline composite nanowire and nanotube Download PDFInfo
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- CN102086302B CN102086302B CN2009101997488A CN200910199748A CN102086302B CN 102086302 B CN102086302 B CN 102086302B CN 2009101997488 A CN2009101997488 A CN 2009101997488A CN 200910199748 A CN200910199748 A CN 200910199748A CN 102086302 B CN102086302 B CN 102086302B
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Abstract
The invention belongs to the nano-material technical field, and relates to a preparing method for molybdenum oxide - polyaniline composite nanowire and nanotube. Molybdena - aniline hybrid nano wire precursor is obtained by using molybdate as the source of molybdenum and interacting with aniline,,and the molybdenum oxide - polyaniline composite nanowire and nanotube are obtained by respectively adjusting system pH value under the initiation of oxidizing agent. The nanowire and the nanotube prepared by the method of the invention have the characteristics of a composite construction of nanometer scale, controllable physical and chemical features, large specific surface area, uniform one-dimensional morphology and controllable thickness and length. The prepared composite molybdenum oxide - polyaniline composite nanowire and nanotube have important application value in many fields such as designing of advanced catalyst, electrocatalysis, electrochemical super capacitor, electrode material, sensor, thermoelectric material, the synthesis and application of advanced optics, electrical material and magnetism material.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of method for preparing molybdenum oxide-polyaniline composite nano-line and nanotube.
Background technology
The compound research on nanoscale of inorganic materials and conductive polymer polymkeric substance is noticeable day by day, and research shows that both are compound can to combine its good physical and chemical performance, improves each other, makes the more easy to control and modulation of performance of mixture.Prior art discloses polyaniline and has had surface of good stability, thermostability and electroconductibility, and it is widely used in electrochemical capacitor, battery, transmitter, the corrosion inhibitor.Molybdenum oxide has peculiar electrochemical properties, electrocatalysis characteristic etc.Compound that molybdenum oxide and polyaniline material is compound on nanoscale through organic and inorganic will combine both good physical and chemical performances undoubtedly, and derive numerous special physicochemical property; Strengthen its application (Y.P.Li, Y.X.Xiang, X.W.Dong in various fields such as lithium ion battery, ultracapacitor, fuel cell, gas sensors; J.Q.Xu, F.Ruan, Q.Y.Pan; J.Solid State Chem.2009,182,2041; K.Shao, S.P.Liao, H.M.Luo, M.L.Wang, J.Solid StateElectrochem, 2007,11,1279; C.J.Song, M Khanfar, J.Appl.Electrochem, 2006,36,339; T.Itoh, I.Matsubara, W.Shin, N.Izu, M.Nishibori, Sens.ActuatorsB, 2008,128,512.).For example molybdenum oxide-polyaniline mixture nano material embodies higher capacity and good cyclicity in anode material for lithium-ion batteries.Hybrid unidimensional nanotopography is owing to have high outer surface area, good assembling performance, thereby improved molybdenum oxide-above-mentioned character of polyaniline hybridized thing.
At present; About the molybdenum oxide-research of polyaniline mixture mainly concentrates on the research of molybdenum oxide and polyaniline composite film, main compound method has IX polymerization, original position interpolation, independently adorns method and electrochemical deposition method (K.Shao, Y.Ma; Z.H.Chen; Chem Letters, 2002,322; J.Wang, IchiroMatsubara, Thin Solid Films, 2006,514,329; K.Shao, S.P.Liao, J.ColloidInterface Sci, 2008,320,445; Zhitomirsky I, Adv Colloid Interface Sci, 2002,97,279.).What aforesaid method obtained all is molybdenum oxide-polyaniline composite films, and complex operation, and the IX forerunner is difficult to preparation and preservation, synthesis condition limit harsh.
Therefore, for the physico-chemical property that promotes this composite nano materials with in the application in fields such as electrochemistry, sensing, embedded photoluminescent material, simultaneously for meeting scale operation, the compound method that seek new convenience, is prone to control becomes this area researchist's focus.
Summary of the invention
The objective of the invention is for overcoming the deficiency of prior art the molybdenum oxide-polyaniline composite nano-line, the nanotube that provide a kind of method simple and easy to control, economical rationality to enrich with preparation property.
The present invention proposes the method for the synthetic molybdenum oxide of a kind of adjustable-polyaniline composite nano-line and nanotube, molybdenum oxide and polyaniline is compound at nanoscale, and assembling forms one-dimensional composite nano line and nanotube.
Particularly, the method for preparing molybdenum oxide-polyaniline composite nano-line and nanotube of the present invention is characterized in that; With molybdate as the molybdenum source; Through with the interaction of aniline, at first obtain molybdenum oxide-aniline hybridized nanometer line presoma, under the initiation of oxygenant; Through the pH value of regulation system, obtain molybdenum oxide-polyaniline composite nano-line or nanotube respectively.
It comprises the steps:
(1) molybdate is dissolved in the zero(ppm) water, makes molybdate solution;
(2) aniline is injected above-mentioned solution;
(3) dropwise add mineral acid, occur to white precipitate;
(4) above-mentioned reaction be placed in the oil bath react, molybdenum oxide-aniline hybridized nanometer line presoma product;
(5) with the molybdenum oxide that obtains-aniline hybridized nanometer line presoma product washing, suction filtration, oven dry;
(6) above-mentioned presoma product is dissolved in polyelectrolyte solution, centrifugal back adds zero(ppm) water or directly is dissolved in the zero(ppm) water solvent;
(7) add polymerization starter ammonium persulphate or Iron(III) chloride hexahydrate;
(8) mineral acid is regulated above-mentioned pH value of solution value, room temperature reaction, and different pH condition makes molybdenum oxide-polyaniline composite Nano product.
In the step of the present invention (1), molybdate is selected from ammonium molybdate, Sodium orthomolybdate or Potassium orthomolybdate, and described molybdate solution calculates with molybdenum atom, and its volumetric molar concentration is 0.01～3.0mol/L.
In the step of the present invention (2), the mol ratio 12.0～1.0 of aniline and molybdenum atom.
In the step of the present invention (3), mineral acid is selected from hydrochloric acid, nitric acid or sulfuric acid, and pH value of solution 4～5 when white precipitate occurred.
In the step of the present invention (4), 30～60 ℃ of oil bath temperatures, 4～24 hours reaction times.
In the step of the present invention (5), product is with absolute ethanol washing number time, and bake out temperature is a room temperature to 80 ℃.
In the step of the present invention (6), polyelectrolyte is selected from Lewatit (PSS) or sodium apolate (PVS).
In the step of the present invention (7), the mol ratio of described ammonium persulphate and molybdenum atom is 0.4～1; The mol ratio of described Iron(III) chloride hexahydrate and molybdenum atom is 1～10.
In the step of the present invention (8), described mineral acid is selected from hydrochloric acid or sulfuric acid, and the reaction times is 6～24 hours;
When the pH value is 1～2, prepare molybdenum oxide-polyaniline composite nano-line; The pH value is 3～5 o'clock, prepares molybdenum oxide-polyaniline composite nano tube.
Among the present invention, preferred reaction conditions is:
(1) described molybdate is Ammonium Molybdate Tetrahydrate ((NH
4)
6Mo
7O
244H
2O), purity 99.99%;
(2) aniline is analytical pure;
(3) concentration of molybdate solution is 0.4～1.0mol/L (calculating with molybdenum atom), and the mol ratio of organic amine and molybdenum atom is 2.0～4.0; Mineral acid is a hydrochloric acid, and concentration is 0.5～2.5mol/L;
(3) solvent adds zero(ppm) water for adding Lewatit (PSS) after centrifugal again.
(5) initiator is an ammonium persulphate, and the mol ratio of ammonium persulphate and molybdenum atom is 0.4～1.
(6) different-shape product optimal ph: the preferred pH of molybdenum oxide-polyaniline composite nano-line is 1.0; The preferred pH of molybdenum oxide-polyaniline composite nano tube is 3.0.
The nano wire of the inventive method preparation, the composite structure that nanotube has nanoscale, regulatable physico-chemical property, big specific surface area, one dimension pattern and the thickness and the regulatable characteristic of length of homogeneous, the compound molybdenum oxide-polyaniline nano-line that makes, nanotube have important use to be worth in the numerous areas such as synthetic and application of advanced catalyst design, electrocatalysis, electric chemical super capacitor, electrode materials, transmitter, thermoelectric material and advanced optics, electricity and magnetics material.
The inventive method productive rate is up to more than 95%.Preparation condition is simple and easy to control, and the processing condition cost is low, and preparation efficiency is high, and quality product and yield rate are high, and good application and industrialization prospect are arranged.
Description of drawings
Fig. 1 is ESEM (SEM) figure of molybdenum oxide-polyaniline composite nano-line A.
Fig. 2 is transmission electron microscope (TEM) figure of product A.
Fig. 3 is infrared (IR) figure of product A.
Fig. 4 is thermogravimetric (TGA) figure of product A.
Fig. 5 is x-ray photoelectron power spectrum (XPS) figure of product A.
Fig. 6 is ESEM (SEM) figure of product B.
Fig. 7 is transmission electron microscope (TEM) figure of product B.
Fig. 8 is transmission electron microscope (TEM) figure of product B.
Fig. 9 is infrared (IR) figure of product B.
Figure 10 is thermogravimetric (TGA) figure of product B.
Figure 11 is x-ray photoelectron power spectrum (XPS) figure of product B.
Figure 12 is ESEM (SEM) figure of product B.
Embodiment
With 1.24g (NH
4)
6Mo
7O
244H
2O is dissolved in the 20mL zero(ppm) water, injects 1.67g aniline, and (pH 4 ~ 5) appear in hydrochloric acid to the white precipitate that dropwise adds 1.0mol/L then.Be transferred among 50 ℃ the oil bath, reacted 6 hours, will obtain the product washing with alcohol for several times and suction filtration, 50 ℃ of dryings, product is called precursor.0.355g precursor is dissolved in 10mLPSS, centrifugal back adds zero(ppm) water, and 0.5mol/L hydrochloric acid regulation system pH is 1.0, adds the 0.143g ammonium persulphate, and reaction is 12 hours under the room temperature, obtains molybdenum oxide-polyaniline composite nano-line A.
Embodiment 2
Method with embodiment 1 experimentizes, and changes wherein ammonium molybdate into Sodium orthomolybdate, makes nanowire product A
1
Embodiment 3
Method with embodiment 1 experimentizes, and changes wherein ammonium molybdate concentration into 0.01mol/L (calculating with molybdenum atom), makes nanowire product A
2
Embodiment 4
Method with embodiment 1 experimentizes, and changes wherein ammonium molybdate concentration into 3.0mol/L (calculating with molybdenum atom), makes nanowire product A
3
Method with embodiment 1 experimentizes, and changes wherein the organic amine and the mol ratio of molybdenum atom into 12.0, makes nanowire product A
4
Embodiment 6
Method with embodiment 1 experimentizes, and changes wherein the organic amine and the mol ratio of molybdenum atom into 1.0, makes nanowire product A
5
Embodiment 7
Method with embodiment 1 experimentizes, and does not wherein add PSS, and zero(ppm) water is directly added precursor, makes nanowire product A
6
Embodiment 8
Method with embodiment 1 experimentizes, and changes wherein PSS into PVS, makes nanowire product A
7
Embodiment 9
Method with embodiment 1 experimentizes, and wherein using 0.5mol/L hydrochloric acid regulation system pH is 2.0, makes nanowire product A
8
Embodiment 10
Method with embodiment 1 experimentizes, and wherein, changes the mol ratio of precursor and Ammonium Persulfate 98.5 into 1, makes nanowire product A
9
Embodiment 11
With 1.24g (NH
4)
6Mo
7O
244H
2O is dissolved in the 20mL zero(ppm) water, injects 1.67g aniline, and (pH 4 ~ 5) appear in hydrochloric acid to the white precipitate that dropwise adds 1.0mol/L then.Be transferred among 50 ℃ the oil bath, reacted 6 hours, will obtain product for several times and suction filtration with washing with alcohol, 50 ℃ of dryings, product is called precursor.0.355g precursor is dissolved in 10mLPSS, centrifugal back adds zero(ppm) water, adds the 0.143g ammonium persulphate, and 1.0mol/L hydrochloric acid regulation system pH is 3.0, and reaction is 12 hours under the room temperature, obtains molybdenum oxide-polyaniline and can get the nanotube product B.
Embodiment 12
Method with embodiment 11 experimentizes, and does not wherein add PSS, and zero(ppm) water is directly added precursor, makes the nanotube product B
1
Embodiment 13
Method with embodiment 11 experimentizes, and wherein regulation system pH is 4-5, makes the nanotube product B
2
Embodiment 14
Method with embodiment 11 experimentizes, and wherein the mol ratio with precursor and Ammonium Persulfate 98.5 changes 1 into, makes the nanotube product B
3
Embodiment 15
Method with embodiment 11 experimentizes, and wherein initiator is changed to Iron(III) chloride hexahydrate, and the mol ratio of Iron(III) chloride hexahydrate and molybdenum atom is 6, makes the nanotube product B
4
Embodiment 16
Method with embodiment 11 experimentizes, and wherein using 0.5mol/L hydrochloric acid regulation system pH is 0.5, makes product C.
The stereoscan photograph of said product (SEM) all absorbs on Philips XL30D6716 instrument, and lens photo (TEM) absorbs on JEOL JEM-2010 instrument.
Fig. 1 has shown the stereoscan photograph of molybdenum oxide-polyaniline composite nano-line A that embodiment 1 makes, demonstrates product A and has the one dimension linear structure.
It is composite Nano wire structure that Fig. 2 (lens photo) further illustrates product A.
Product A to gained characterizes (as shown in Figure 3) with IR (Nicolet 360FT-IR spectrometer), and wave number is 1579.2,1497.7,1303.5,1239.9,1143.6 and 864.2cm
-1The peak be the characteristic peak of polyaniline, wave number is 944.21,902.4,739.3 and 682.3cm
-1The vibration peak of corresponding oxidation state molybdenum shows that this material is the organic inorganic hybridization mixture that is made up of the polyaniline molybdenum oxide.
Weightlessness between the thermogravimetric analysis of product A (Perkin-Elmer TGA7) (as shown in Figure 4), room temperature to 100 ℃ mainly be since the removing of the deionized water of absorption, the weightlessness between 300 ℃ to 410 ℃ mainly due to the decomposition of polyaniline.
The x-ray photoelectron power spectrum XPS of product A (Perkin-Elmer PHI5000c XPS) characterizes (as shown in Figure 5), shows that Mo is a sexavalence in the product.
The SEM photo (as shown in Figure 6) of product B proves that embodiment 11 makes is molybdenum oxide-polyaniline composite nano tube, and size is even.
The TEM photo of product B (shown in Fig. 7 and 8) further demonstrates the tubular structure of product of nano.
The IR collection of illustrative plates (as shown in Figure 9) of B proves that the nanotube product shown in Fig. 7 and 8 is similarly polyaniline-molybdenum oxide mixture.
Weightlessness between the thermogravimetric analysis of product B (shown in figure 10) room temperature to 100 ℃ mainly is mainly due to the decomposition of polyaniline owing to the removing of adsorption deionizing water, weightlessness between 260 ℃ to 430 ℃.
With XPS the sign (shown in figure 11) of product B is shown that Mo is similarly sexavalence in the product.
Figure 12 demonstrates the product S EM figure that embodiment 16 methods obtain; Show when reaction system pH is 0.5; What obtain is not molybdenum oxide-polyaniline composite nano-line or nanotube pattern, further specifies in the inventive method the conditional request to different-shape product pH value.
Molybdenum oxide-polyaniline nano-line that the present invention makes, nanotube have novel composite structure, big outer surface area and the one dimension pattern of homogeneous; The good physico-chemical property that embodies in fields such as electrode materials, ultracapacitor, catalysis, sensings simultaneously based on molybdenum oxide and polyaniline; Described al oxide-polyaniline composite nano-line and nanotube will be applied to like, the synthetic field of nano-device design and assembling, electrode materials, lithium ion battery, ultracapacitor, fuel cell, gas sensor and advanced optics, electricity and magnetics material.
Claims (13)
1. method for preparing molybdenum oxide-polyaniline composite nano-line and nanotube; It is characterized in that, with molybdate as the molybdenum source, through with the interaction of aniline; Obtain molybdenum oxide-aniline hybridized nanometer line presoma; Under the initiation of oxygenant,, make molybdenum oxide-polyaniline composite nano-line or nanotube respectively through the pH value of regulation system; It comprises the steps:
(1) molybdate is dissolved in the zero(ppm) water, makes molybdate solution,
(2) aniline is injected above-mentioned solution;
(3) dropwise add mineral acid, occur to white precipitate;
(4) above-mentioned reaction be placed in the oil bath react, molybdenum oxide-aniline hybridized nanometer line presoma product;
(5) with the molybdenum oxide that obtains-aniline hybridized nanometer line presoma product washing, suction filtration, oven dry;
(6) the presoma product with above-mentioned (5) is dissolved in polyelectrolyte solution, and centrifugal back adds zero(ppm) water or directly is dissolved in the zero(ppm) water solvent;
(7) add polymerization starter;
(8) use mineral acid to regulate above-mentioned pH value of solution value, room temperature reaction, the pH value be 1～2 or the pH value be to make molybdenum oxide-polyaniline composite Nano product at 3～5 o'clock;
Described molybdate is selected from ammonium molybdate, Sodium orthomolybdate or Potassium orthomolybdate.
2. method according to claim 1 is characterized in that described molybdate solution calculates with molybdenum atom, and its volumetric molar concentration is 0.01～3.0mol/L.
3. method according to claim 1 is characterized in that, in said step (2) solution, the mol ratio of aniline and molybdenum atom is 12.0～1.0.
4. method according to claim 1 is characterized in that, the mineral acid in the said step (3) is selected from hydrochloric acid, nitric acid or sulfuric acid, and pH value of solution 4～5 when described white precipitate occurred.
5. method according to claim 1 is characterized in that, the oil bath temperature in the said step (4) is 30～60 ℃, and the reaction times is 4～24 hours.
6. method according to claim 1 is characterized in that, the molybdenum oxide in the said step (5)-aniline hybridized nanometer line presoma product is with absolute ethanol washing number time, suction filtration, and oven dry, temperature is a room temperature to 80 ℃.
7. method according to claim 1 is characterized in that, the polyelectrolyte in the said step (6) is selected from Lewatit or sodium apolate.
8. method according to claim 1 is characterized in that, the initiator in the said step (7) is ammonium persulphate or Iron(III) chloride hexahydrate.
9. method according to claim 8 is characterized in that, the mol ratio of described ammonium persulphate and molybdenum atom is 0.4～1.
10. method according to claim 8 is characterized in that, the mol ratio of described Iron(III) chloride hexahydrate and molybdenum atom is 1～10.
11. method according to claim 1 is characterized in that, the mineral acid in the said step (8) is hydrochloric acid or sulfuric acid.
12., it is characterized in that the room temperature reaction time in the said step (8) is 6～24 hours according to claim 1 or 11 described methods.
13. method according to claim 1 is characterized in that, in the said step (8), when the pH value was 1～2, product was molybdenum oxide-polyaniline composite nano-line, and when the pH value was 3～5, product was molybdenum oxide-polyaniline composite nano tube.
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| EP2960302A1 (en) * | 2014-06-26 | 2015-12-30 | Instytut Elektrotechniki | Method of synthesis of hybrid compounds of polyaniline and application of hybrid compounds of polyaniline |
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| CN103613759B (en) * | 2013-12-06 | 2015-10-28 | 东华大学 | A kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction |
| CN106065180B (en) * | 2016-06-08 | 2018-02-16 | 东华大学 | A kind of preparation method of molybdenum trioxide polypyrrole polyaniline trielement composite material |
| CN109427981B (en) * | 2017-08-28 | 2020-11-10 | Tcl科技集团股份有限公司 | QLED device and preparation method thereof |
| CN113750987A (en) * | 2021-09-16 | 2021-12-07 | 南京信息工程大学 | Quadrature phase MoO3Electrocatalyst and preparation method and application thereof |
| 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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