CN103721708B - A kind of Silver/titanium dioxide composite heterostructure and preparation method thereof - Google Patents
A kind of Silver/titanium dioxide composite heterostructure and preparation method thereof Download PDFInfo
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- CN103721708B CN103721708B CN201410008189.9A CN201410008189A CN103721708B CN 103721708 B CN103721708 B CN 103721708B CN 201410008189 A CN201410008189 A CN 201410008189A CN 103721708 B CN103721708 B CN 103721708B
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Abstract
The invention discloses a kind of Silver/titanium dioxide composite heterostructure, including nano silver wire and titanium dioxide content, wherein being covered with layer of titanium dioxide shell on nano silver wire and can form hud typed heterojunction structure, titanium dioxide ball string can form pelletron type heterojunction structure on nano silver wire.Heterojunction structure of the present invention i.e. has the good conductive and heat-conductive character of silver itself, define again the heterojunction structure of noble metal and semiconductor light-catalyst, be conducive to efficiently separating of electronics and hole, enhance photocatalytic degradation Organic substance performance, compensate for again the poor chemical stability of silver, the shortcoming that is oxidized easily of surface, have broad application prospects in photocatalysis and new energy field.The invention also discloses its preparation method, the method is simple to operate, and controllability is strong, reproducible, can obtain the heterojunction structure of different-shape by adjusting reagent collocation, can adjust TiO by the amount adjusting titanium source2The diameter of ball and the thickness of titanium dioxide shell, have the strongest practicality.
Description
Technical field
The present invention relates to the composite heterogenous junction structure of a kind of nano silver wire and titanium dioxide with and preparation method thereof, belong to metal
With semiconductors coupling heterogeneous structure material preparing technical field.
Background technology
In recent years, all had latent due to hud typed nanostructured in research fields such as optoelectronics, catalysis and photocatalysis
Advantage, get more and more people's extensive concerning.In these materials, Ag and TiO2Coreshell type structure research especially prominent,
Not only due to TiO2At Optical Electro-Chemistry activity, solar energy conversion and photocatalyst, there is potential using value, Er Qieyin
The surface-enhanced Raman effects of nano material, local surface plasma resonance and fluorescent effect, in chemistry and bio-sensing side
To the performance illustrating some uniquenesses.Additionally, individually noble metal granule is susceptible to corrosion and decomposes, noble metal light can be limited
The application of catalytic degradation effect, and Ag and TiO2After material forms hud typed heterojunction structure, the stability of material can be made to obtain
To improving, and the photocatalysis performance of material after being combined, can be effectively improved.
At present, to Ag and TiO2The research of nano-particles reinforcement is mostly gathered in and noble metal nano particles is deposited on TiO2
The surface of nano-particle forms heterojunction structure, is seldom found to have TiO2Material is deposited on the heterojunction structure report on nano silver wire surface
Road, wherein, nano silver wire and TiO2The bead chain shape heterojunction structure formed have not been reported.
Summary of the invention
The invention discloses a kind of Silver/titanium dioxide composite heterostructure, this heterojunction structure combines silver and titanium dioxide
Advantage, overcome unstable, the most oxidized shortcoming of silver, catalytic effect is more preferably.
The invention also discloses the preparation method of this composite heterogenous junction structure, the method can be obtained by the adjustment of technological parameter
To hud typed and pelletron type composite heterogenous junction structure, it is also possible to adjust diameter and the thickness of titanium dioxide shell of titanium dioxide ball,
There is good practicality.
The present invention is using nano silver wire as carrier, and to be mixed to form presoma molten with dispersion solvent, alcohol, bridging agent and titanium source
Liquid, precursor solution is at high temperature reacted make titanium dioxide deposition on nano silver wire surface, thus obtain nano silver wire with
TiO2Compound heterojunction structure, by adjusting solvent and the collocation of alcohol of dispersion nano silver wire, it is possible to obtain pelletron type and nucleocapsid
The heterojunction structure of two kinds of different-shapes of type.By changing preparation condition, it is also possible to the diameter of regulation pelletron type titanium dioxide ball is big
Little, and the thickness of hud typed titanium dioxide shell, there is the strongest practicality.One-dimensional nano silver wire structure has excellence
Optics and electrical properties, therefore, form TiO on the surface of nano silver wire2The hud typed heterojunction structure with two kinds of patterns of pelletron type,
There is potential using value.
The concrete technical scheme of the present invention is as follows:
Nano silver wire of the present invention and titanium dioxide can form two kinds of composite heterogenous junction structure, and one is hud typed,
One is pelletron type, specific as follows:
Hud typed Silver/titanium dioxide composite heterostructure, is characterized in that: described silver is nano silver wire, on nano silver wire
It is covered with layer of titanium dioxide shell, nano silver wire and titanium dioxide and forms hud typed composite heterogenous junction structure.
In hud typed heterojunction structure, described nano silver wire can be mono-crystalline structures, it is also possible to for polycrystalline structure, nano silver wire
A diameter of 10-60 nm.In this diameter range, gained composite heterogenous junction structure performance is the most fine.
In hud typed heterojunction structure, described titanium dioxide is uniformly coated on nano silver wire substantially, by nano silver wire bag
Being rolled in titanium dioxide shell, titanium dioxide thickness of the shell is 5-100 nm.
Pelletron type Silver/titanium dioxide composite heterostructure, is characterized in that: include nano silver wire, and described nano silver wire is gone here and there
There are at least one titanium dioxide ball, described nano silver wire to be chained together by all titanium dioxide balls, form pelletron type and be combined different
Matter structure.
In pelletron type composite heterogenous junction structure, nano silver wire runs through titanium dioxide ball along titanium dioxide ball diametric(al).
In pelletron type composite heterogenous junction structure, every nano silver wire can contain one or more titanium dioxide balls, typically
All contain multiple titanium dioxide ball, the concrete number of titanium dioxide ball and the length of nano silver wire, the diameter of titanium dioxide ball, two
Between individual titanium dioxide ball, the factor such as spaced apart is relevant.
In pelletron type composite heterogenous junction structure, closely coupled or there is certain interval between each titanium dioxide ball；Two titanium dioxide
The gap location (i.e. not having at the nano silver wire of titanium dioxide ball) of titanium ball is also covered with layer of titanium dioxide, but the thickness of this titanium dioxide
Spend relatively thin, less than bulb diameter.
In pelletron type composite heterogenous junction structure, described nano silver wire is only the nano silver wire of polycrystalline structure, and nano silver wire is straight
Footpath is 10-60 nm.In this diameter range, gained composite heterogenous junction structure performance is the most fine.
In pelletron type composite heterogenous junction structure, string titanium dioxide ball on nano silver wire varies, and there is certain difference
Different, general, the average diameter of titanium dioxide ball is 200-600 nm.
The above-mentioned hud typed or preparation of pelletron type Silver/titanium dioxide composite heterostructure, can be by nano silver wire table
The form of face deposition of titanium oxide forms hud typed or pelletron type composite heterogenous junction structure.Specifically include following steps:
(1) being disperseed in a solvent by nano silver wire, time of infusion makes solvent carry out moistening on the surface of nano silver wire,
Obtain nano silver wire suspension；
(2) stir under addition alcohol and bridging agent, room temperature in nano silver wire suspension；
(3) in the suspension of step (2), add titanium source, stir under room temperature；
(4) temperature of the suspension of ascending step (3), makes titanium dioxide deposition on nano silver wire surface, is centrifuged after reaction
Separate, wash, obtain Silver/titanium dioxide composite heterostructure.
In step (1), the purpose of dipping is that the solvent having made peptizaiton carries out moistening on the surface of nano silver wire, makes molten
Agent molecule adsorbs on surface or grain boundaries.The solvent of dispersion nano silver wire can be deionized water, methanol, ethanol, propanol or fourth
Alcohol etc..The time of dipping is generally 4 hours-7 days.
In step (2), described alcohol is monohydric alcohol；Described bridging agent is TGA or mercaptopropionic acid.
In step (3), described titanium source is butyl titanate, metatitanic acid orthocarbonate or isopropyl titanate.
In step (4), suspension being risen to 120-200 DEG C and reacts, the response time is 4-20 h, preferably at 150 DEG C
React 10 h.
In above-mentioned preparation method, in order to obtain titanium dioxide shell and the titanium dioxide of corresponding pattern, respective thickness or diameter
Ball, the consumption of the reagent such as titanium source to be controlled, bridging agent, nano silver wire and concentration.
In above-mentioned preparation method, nano silver wire is 1:0.7 ~ 14 with the mol ratio in titanium source, preferably nano silver wire (mmol): titanium
Source (ml)=0.1:0.1=1:1.
In above-mentioned preparation method, bridging agent can make titanium source be attached in Ag nanowire surface, prepares the different of pelletron type
Bridging agent must be used during matter structure, can be at nano silver wire in the case of without bridging agent when preparing hud typed heterojunction structure
Surface cover last layer TiO2.Preferably, when preparing pelletron type composite heterogenous junction structure, the volume ratio of titanium source and bridging agent be (1 ~
10): (0.4~2)；When preparing hud typed composite heterogenous junction structure, the volume ratio of titanium source and bridging agent is (1 ~ 10): (0 ~ 2) (because of
Titanium source used and bridging agent are liquid, so mol ratio can embody by volume ratio).
In above-mentioned preparation method, the amount in the suspension in step (3) of titanium source is unsuitable excessive, also unsuitable too small, through experiment
Checking, system volume is mainly provided by dispersion solvent in step (1) and the alcohol in step (2), the volume in titanium source and step (1)
In middle dispersion solvent and step (2), the ratio of the volume sum of alcohol is effective when 0.00125-0.025:1 scope.
In above-mentioned preparation method, the composite heterogenous junction structure of different-shape can be made by controlling the collocation of reagent.Work as step
Suddenly when the alcohol during the solvent in (1) is deionized water, step (2) is methanol, ethanol or propanol, products obtained therefrom be nano silver wire with
The pelletron type composite heterogenous junction structure of titanium dioxide；Alcohol in the solvent in step (1) is deionized water, step (2) is isopropyl
When alcohol or the carbon chain lengths such as n-butyl alcohol, n-amyl alcohol are more than or equal to the monohydric alcohol of four, products obtained therefrom is nano silver wire and titanium dioxide
Hud typed composite heterogenous junction structure；Alcohol in the solvent in step (1) is methanol, ethanol, propanol or butanol, step (2) is
During arbitrary monohydric alcohol, products obtained therefrom is the hud typed composite heterogenous junction structure of nano silver wire and titanium dioxide.
In above-mentioned preparation method, when in step (1), solvent is deionized water, it is 1:200 with the volume ratio of alcohol in step (2)
Left and right.When in step (1), solvent is alcohol, it is about 1:3 with the volume ratio of the alcohol in step (2).
The present invention's it is crucial that is combined nano silver wire with titanium oxide, nano silver wire length not requirement used, can adopt
Prepare required crystal formation and the nano silver wire of diameter by the method disclosed in prior art, such as, can use disclosed in following document
Method prepare nano silver wire:
(1)Changchao Jia, Ping Yang, Aiyu Zhang. Glycerol and ethylene glycol
co-mediated synthesis of uniform multiple crystalline silver nanowires,
Materials Chemistry and Physics, 2014, 143(2), 794-800.
(2)Linfeng Gou, Mircea Chipara, and Jeffrey M. Zaleski, Convenient,
Rapid Synthesis of Ag Nanowires, Chem. Mater. 2007, 19, 1755-1760.
(3)Yugang Sun, Yadong Yin, Brian T. Mayers, Thurston Herricks, and
Younan Xia, Uniform Silver Nanowires Synthesis by Reducing AgNO3 with
Ethylene Glycol in the Presence of Seeds and Poly(Vinyl Pyrrolidone). Chem.
Mater. 2002, 14, 4736-4745.
Composite heterogenous junction structure of the present invention can be as the catalyst of light-catalyzed reaction.During light-catalyzed reaction, silver is not
Only can reduce electronics and the combined efficiency in hole pair as electronics trapping agent, effectively carry out organic light degradation reaction, and
And visible ray can be made full use of, expand TiO2The response range of exciting light, simultaneously because photo-excited electron is at TiO2And between Ag
Carry out electron transfer, improve the photocatalysis efficiency of material.In pearl chain structure, TiO2Bulb diameter is excessive, can affect nano silver wire
Exciting photoelectronic, the utilization rate of light declines and reduces TiO2And the electron transfer effect between Ag, if TiO2The diameter of ball
Too small, make photocatalysis rises the TiO of Degradation2Content reduces relatively, reduces photocatalysis effect.Bulb diameter of the present invention can do
To 200-600 nm, preferably during diameter 450 nm, performance is more preferable.In nucleocapsid structure, the thickness of titanium dioxide shell is to heterojunction structure
Impact that can be good and bad is similar to the impact of bead chain shape structure, and shell thickness can adjust in 5-100 nm scope, preferred thickness 30
During nm, performance is more preferable.
The present invention is at the Surface coating TiO of nano silver wire2, synthesized nano silver wire and TiO2Composite heterogenous junction structure, XRD
Characterization result proves, it is thus achieved that TiO2Crystal formation belong to Detitanium-ore-type.This heterojunction structure can present hud typed and two kinds of pelletron type
Different patterns.The method is simple to operate, and controllability is strong, reproducible, can obtain different-shape by adjusting reagent collocation
Heterojunction structure, by adjust titanium source amount can adjust TiO2The diameter of ball and the thickness of titanium dioxide shell, have
The strongest practicality.Surface coating TiO at nano silver wire2, the surface that can effectively protect silver is not oxidized, has excellence
Chemical stability, it addition, TiO2As traditional photocatalyst material, being compounded to form heterojunction structure with nano silver wire, this is different
Photocatalysis and the electrical properties of matter structural advantage have broad application prospects in photocatalysis and new energy field.
Heterojunction structure of the present invention i.e. has the good conductive and heat-conductive character of silver itself, defines again noble metal and semiconductor light
The heterojunction structure of catalyst, beneficially electronics efficiently separate with hole, enhance photocatalytic degradation Organic substance performance, make up again
The shortcoming that the poor chemical stability of silver, surface are oxidized easily.Before photocatalysis and new energy field have wide application
Scape.
Accompanying drawing explanation
The nano silver wire of Fig. 1 (a) embodiment of the present invention 1 synthesis and TiO2(AgNWs@TiO2) X of pelletron type heterojunction structure penetrates
Line diffraction (XRD) collection of illustrative plates.
The nano silver wire of Fig. 1 (b) embodiment of the present invention 1 synthesis and TiO2The scanning electron microscope (SEM) of pelletron type heterojunction structure
Photo.
The nano silver wire of Fig. 2 embodiment of the present invention 5 synthesis and TiO2The scanning electron microscope (SEM) of pelletron type heterojunction structure shines
Sheet.
The nano silver wire of Fig. 3 embodiment of the present invention 6 synthesis and TiO2The scanning electron microscope (SEM) of pelletron type heterojunction structure shines
Sheet.
The nano silver wire of Fig. 4 embodiment of the present invention 11 synthesis and TiO2The scanning electron microscope (SEM) of hud typed heterojunction structure shines
Sheet.
The nano silver wire of Fig. 5 embodiment of the present invention 12 synthesis and TiO2The scanning electron microscope (SEM) of hud typed heterojunction structure shines
Sheet.
The nano silver wire of Fig. 6 embodiment of the present invention 15 synthesis and TiO2The scanning electron microscope (SEM) of hud typed heterojunction structure shines
Sheet.
The nano silver wire of Fig. 7 (a) embodiment of the present invention 16 synthesis and TiO2X-ray diffraction (XRD) figure of coreshell type structure
Spectrum.
The nano silver wire of Fig. 7 (b) embodiment of the present invention 16 synthesis and TiO2The scanning electron microscope (SEM) of coreshell type structure shines
Sheet.
The nano silver wire of Fig. 8 embodiment of the present invention 18 synthesis and TiO2The scanning electron microscope (SEM) of hud typed heterojunction structure shines
Sheet.
The nano silver wire of Fig. 9 embodiment of the present invention 19 synthesis and TiO2The scanning electron microscope (SEM) of hud typed heterojunction structure shines
Sheet.
The nano silver wire of Figure 10 embodiment of the present invention 27 synthesis and TiO2The scanning electron microscope (SEM) of hud typed heterojunction structure shines
Sheet.
Nano silver wire used and TiO in Figure 11 embodiment of the present invention 282(AgNWs@TiO2) pelletron type and hud typed hetero-junctions
The structure degradation effect figure to methyl orange.
Detailed description of the invention
Below by embodiment, the present invention will be further elaborated, it should explanation, the description below merely to
Explain the present invention, its content is not defined.
Nano silver wire used by the present invention can use any means disclosed in existing method to obtain, the diameter of nano silver wire
Requiring between 10-60nm, the nano silver wire of polycrystalline structure can prepare the heterojunction structure of pelletron type by adjusting process condition,
The nano silver wire of monocrystalline or polycrystalline structure all can prepare hud typed heterojunction structure by adjusting process condition.Following embodiment
In, nano silver wire used is according to document (Changchao Jia, Ping Yang, Aiyu Zhang. Glycerol and
ethylene glycol co-mediated synthesis of uniform multiple crystalline silver
Nanowires, Materials Chemistry and Physics, 2014,143 (2), 794-800.) in listed method
Prepare: by the AgNO of 0.034 g3It is dissolved in 5 mL glycerol, standby；The PVP of 0.067 g is dissolved in 10 mL glycerol and 3
In the mixed solution of mL ethylene glycol, stir standby；Above two solution is mixed, stirs, be then transferred to reaction
Still 200 DEG C reaction 5 h, after reaction terminates, use water centrifuge washing, and 4000 turns every point is washed three times.Under this preparation parameter, gained is put down
The polycrystalline structure nano silver wire of the most a diameter of 40 nm, by adjusting PVP and AgNO3Mol ratio can obtain diameter 10-60
The nano silver wire of nm scope.
Embodiment 1
0.1 mmol nano silver wire is dispersed in 0.1 mL deionized water by 1.1, impregnates 12 h, obtains suspension；
1.2 add 20 mL ethanol, 100 L TGAs in the nano silver wire suspension described in embodiment 1.1, stir
Mix uniformly；
1.3 add 0.5 mL butyl titanate in the mixed liquor described in embodiment 1.2, are uniformly mixed；
Mixed liquor described in embodiment 1.3 is transferred in 50 mL reactors by 1.4,150 DEG C, reacts 10 h.
1.5 by embodiment 1.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Pelletron type heterojunction structure
(as shown in Figure 1), titanium dioxide mean diameter of a ball is 600 nm, a diameter of 40 nm of nano silver wire.
Embodiment 2
0.1mmol nano silver wire is dispersed in 0.1 mL deionized water by 2.1, impregnates 4 h, obtains suspension；
2.2 add 20 mL methanol, 20 L TGAs in the nano silver wire suspension described in embodiment 2.1, stir
Mix uniformly；
2.3 add 0.5 mL metatitanic acid orthocarbonate in the mixed liquor described in embodiment 2.2, are uniformly mixed；
Mixed liquor described in embodiment 2.3 is transferred in 50 mL reactors by 2.4,150 DEG C, reacts 10 h.
2.5 by embodiment 2.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Pelletron type hetero-junctions
Structure, titanium dioxide mean diameter of a ball is 560 nm, a diameter of 10 nm of nano silver wire.
Embodiment 3
0.1mmol nano silver wire is dispersed in 0.1 mL deionized water by 3.1, impregnates 8 h, obtains suspension；
3.2 add 20mL propanol, 50 L TGAs, stirring in the nano silver wire suspension described in embodiment 3.1
Uniformly；
3.3 add 0.025 mL isopropyl titanate in the mixed liquor described in embodiment 3.2, are uniformly mixed；
Mixed liquor described in embodiment 3.3 is transferred in 50 mL reactors by 3.4,150 DEG C, reacts 10 h.
3.5 by embodiment 3.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Pelletron type hetero-junctions
Structure, titanium dioxide mean diameter of a ball is 200 nm, a diameter of 60 nm of nano silver wire.
Embodiment 4
0.1mmol nano silver wire is dispersed in 0.1 mL deionized water by 4.1, impregnates 3 days, obtains suspension；
4.2 add 20 mL ethanol, 50 L mercaptopropionic acids in the nano silver wire suspension described in embodiment 4.1, stir
Mix uniformly；
4.3 add 0.5 mL isopropyl titanate in the mixed liquor described in embodiment 4.2, are uniformly mixed；
Mixed liquor described in embodiment 4.3 is transferred in 50 mL reactors by 4.4,150 DEG C, reacts 10 h.
4.5 by embodiment 4.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Pelletron type hetero-junctions
Structure, titanium dioxide mean diameter of a ball is 580 nm, a diameter of 40 nm of nano silver wire.
Embodiment 5
0.1mmol nano silver wire is dispersed in 0.1 mL deionized water by 5.1, impregnates 12 h, obtains suspension；
5.2 add 20 mL ethanol, 20 L TGAs in the nano silver wire suspension described in embodiment 5.1, stir
Mix uniformly；
5.3 add 0.1 mL butyl titanate in the mixed liquor described in embodiment 5.2, are uniformly mixed；
Mixed liquor described in embodiment 5.3 is transferred in 50 mL reactors by 5.4,150 DEG C, reacts 10 h.
5.5 by embodiment 5.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Pelletron type heterojunction structure
(as shown in Figure 2), titanium dioxide mean diameter of a ball is 450 nm, a diameter of 40 nm of nano silver wire.
Embodiment 6
0.1mmol nano silver wire is dispersed in 0.1 mL deionized water by 6.1, impregnates 12 h, obtains suspension；
6.2 add 20 mL ethanol, 20 L TGAs in the nano silver wire suspension described in embodiment 6.1, stir
Mix uniformly；
6.3 add 0.05 mL butyl titanate in the mixed liquor described in embodiment 6.2, are uniformly mixed；
Mixed liquor described in embodiment 6.3 is transferred in 50 mL reactors by 6.4,150 DEG C, reacts 10 h.
6.5 by embodiment 6.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Pelletron type heterojunction structure
(as shown in Figure 3), titanium dioxide mean diameter of a ball is 300 nm, a diameter of 40 nm of nano silver wire.
Embodiment 7
0.1mmol nano silver wire is dispersed in 0.1 mL deionized water by 7.1, impregnates 7 days, obtains suspension；
7.2 add 20 mL ethanol, 20 L TGAs in the nano silver wire suspension described in embodiment 7.1, stir
Mix uniformly；
7.3 add 0.15 mL butyl titanate in the mixed liquor described in embodiment 7.2, are uniformly mixed；
Mixed liquor described in embodiment 7.3 is transferred in 50 mL reactors by 7.4,150 DEG C, reacts 10 h.
7.5 by embodiment 7.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Pelletron type hetero-junctions
Structure, titanium dioxide mean diameter of a ball is 480 nm, a diameter of 40 nm of nano silver wire.
Embodiment 8
0.1mmol nano silver wire is dispersed in 0.1 mL deionized water by 8.1, impregnates 2 days, obtains suspension；
8.2 add 20 mL n-butyl alcohol in the nano silver wire suspension described in embodiment 8.1,20 L TGAs,
Stir；
8.3 add 0.5 mL butyl titanate in the mixed liquor described in embodiment 8.2, are uniformly mixed；
Mixed liquor described in embodiment 8.3 is transferred in 50 mL reactors by 8.4,150 DEG C, reacts 10 h.
8.5 by embodiment 8.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure, titanium dioxide thickness of the shell is 100 nm, a diameter of 20 nm of nano silver wire.
Embodiment 9
0.1mmol nano silver wire is dispersed in 0.1 mL deionized water by 9.1, impregnates 3 days, obtains suspension；
9.2 add 20 mL isopropanols in the nano silver wire suspension described in embodiment 9.1,20 L TGAs,
Stir；
9.3 add 0.5 mL butyl titanate in the mixed liquor described in embodiment 9.2, are uniformly mixed；
Mixed liquor described in embodiment 9.3 is transferred in 50 mL reactors by 9.4,150 DEG C, reacts 10 h.
9.5 by embodiment 9.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure, titanium dioxide thickness of the shell is 95 nm, a diameter of 30 nm of nano silver wire.
Embodiment 10
0.1mmol nano silver wire is dispersed in 0.1 mL deionized water by 10.1, impregnates 4 days, obtains suspension；
10.2 add 20 mL n-amyl alcohols, 20 L sulfydryl second in the nano silver wire suspension described in embodiment 10.1
Acid, stirs；
10.3 add 0.5 mL butyl titanate in the mixed liquor described in embodiment 10.2, are uniformly mixed；
Mixed liquor described in embodiment 10.3 is transferred in 50 mL reactors by 10.4,150 DEG C, reacts 10 h.
10.5 by embodiment 10.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure, titanium dioxide thickness of the shell is 90 nm, a diameter of 50 nm of nano silver wire.
Embodiment 11
0.1mmol nano silver wire is dispersed in 0.1 mL deionized water by 11.1, impregnates 12 h, obtains suspension；
11.2 add 20 mL n-butyl alcohol, 20 L sulfydryl second in the nano silver wire suspension described in embodiment 11.1
Acid, stirs；
11.3 add 0.1 mL butyl titanate in the mixed liquor described in embodiment 11.2, are uniformly mixed；
Mixed liquor described in embodiment 11.3 is transferred in 50 mL reactors by 11.4,150 DEG C, reacts 10 h.
11.5 by embodiment 11.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure (as shown in Figure 4), titanium dioxide thickness of the shell is 25 nm, a diameter of 40 nm of nano silver wire.
Embodiment 12
0.1mmol nano silver wire is dispersed in 0.1 mL deionized water by 12.1, impregnates 12 h, obtains suspension；
12.2 add 20 mL n-butyl alcohol, 20 L sulfydryl second in the nano silver wire suspension described in embodiment 12.1
Acid, stirs；
12.3 add 0.05 mL butyl titanate in the mixed liquor described in embodiment 12.2, are uniformly mixed；
Mixed liquor described in embodiment 12.3 is transferred in 50 mL reactors by 12.4,150 DEG C, reacts 10 h.
12.5 by embodiment 12.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure (as shown in Figure 5), titanium dioxide thickness of the shell is 5 nm, a diameter of 40 nm of nano silver wire.
Embodiment 13
0.1 mmol nano silver wire is directly dispersing in 5 mL ethanol by 13.1, impregnates 5 days, obtains suspension；
13.2 add 15 mL methanol in the nano silver wire suspension described in embodiment 13.1,20 L TGAs,
Stir；
13.3 add 0.5 mL butyl titanate in the mixed liquor described in embodiment 13.2, are uniformly mixed；
Mixed liquor described in embodiment 13.3 is transferred in 50 mL reactors by 13.4,150 DEG C, reacts 10 h.
13.5 by embodiment 13.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure, titanium dioxide thickness of the shell is 80 nm, a diameter of 30 nm of nano silver wire.
Embodiment 14
0.1 mmol nano silver wire is directly dispersing in 5 mL propanol by 14.1, impregnates 3 days, obtains suspension；
14.2 add 15 mL ethanol in the nano silver wire suspension described in embodiment 14.1,20 L TGAs,
Stir；
14.3 add 0.5 mL butyl titanate in the mixed liquor described in embodiment 14.2, are uniformly mixed；
Mixed liquor described in embodiment 14.3 is transferred in 50 mL reactors by 14.4,150 DEG C, reacts 10 h.
14.5 by embodiment 14.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure, titanium dioxide thickness of the shell is 75 nm, a diameter of 20 nm of nano silver wire.
Embodiment 15
0.1 mmol nano silver wire is directly dispersing in 5 mL ethanol by 15.1, impregnates 1 day, obtains suspension；
15.2 add 15 mL ethanol in the nano silver wire suspension described in embodiment 15.1,20 L TGAs,
Stir；
15.3 add 0.25 mL butyl titanate in the mixed liquor described in embodiment 15.2, are uniformly mixed；
Mixed liquor described in embodiment 15.3 is transferred in 50 mL reactors by 15.4,150 DEG C, reacts 10 h.
15.5 by embodiment 15.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure (as shown in Figure 6), titanium dioxide thickness of the shell is 80 nm, a diameter of 40 nm of nano silver wire.
Embodiment 16
0.1 mmol nano silver wire is directly dispersing in 5 mL ethanol by 16.1, impregnates 1 day, obtains suspension；
16.2 add 15 mL ethanol in the nano silver wire suspension described in embodiment 16.1,20 L TGAs,
Stir；
16.3 add 0.1 mL butyl titanate in the mixed liquor described in embodiment 16.2, are uniformly mixed；
Mixed liquor described in embodiment 16.3 is transferred in 50 mL reactors by 16.4,150 DEG C, reacts 10 h.
16.5 by embodiment 16.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure (as shown in Figure 7), titanium dioxide thickness of the shell is 30 nm, a diameter of 40 nm of nano silver wire.
Embodiment 17
0.1 mmol nano silver wire is directly dispersing in 5 mL methanol by 17.1, impregnates 7 days, obtains suspension；
17.2 add 15 mL propanol in the nano silver wire suspension described in embodiment 17.1,20 L TGAs,
Stir；
17.3 add 0.25 mL butyl titanate in the mixed liquor described in embodiment 17.2, are uniformly mixed；
Mixed liquor described in embodiment 17.3 is transferred in 50 mL reactors by 17.4,150 DEG C, reacts 10 h.
17.5 by embodiment 17.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure, titanium dioxide thickness of the shell is 45 nm, a diameter of 10 nm of nano silver wire.
Embodiment 18
0.1 mmol nano silver wire is directly dispersing in 5 mL ethanol by 18.1, impregnates 1 day, obtains suspension；
18.2 add 15 mL n-butyl alcohol, 20 L sulfydryl second in the nano silver wire suspension described in embodiment 18.1
Acid, stirs；
18.3 add 0.5 mL butyl titanate in the mixed liquor described in embodiment 18.2, are uniformly mixed；
Mixed liquor described in embodiment 18.3 is transferred in 50 mL reactors by 18.4,150 DEG C, reacts 10 h.
18.5 by embodiment 18.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure (as shown in Figure 8), titanium dioxide thickness of the shell is 90 nm, a diameter of 40 nm of nano silver wire.
Embodiment 19
0.1 mmol nano silver wire is directly dispersing in 5 mL ethanol by 19.1, impregnates 12 h, obtains suspension；
19.2 add 15 mL n-butyl alcohol, 20 L sulfydryl second in the nano silver wire suspension described in embodiment 19.1
Acid, stirs；
19.3 add 0.1 mL butyl titanate in the mixed liquor described in embodiment 19.2, are uniformly mixed；
Mixed liquor described in embodiment 19.3 is transferred in 50 mL reactors by 19.4,150 DEG C, reacts 10 h.
19.5 by embodiment 19.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure (as shown in Figure 9), titanium dioxide thickness of the shell is 30 nm, a diameter of 40 nm of nano silver wire.
Embodiment 20
0.1 mmol nano silver wire is directly dispersing in 5 mL ethanol by 20.1, impregnates 4 h, obtains suspension；
20.2 add 15 mL isopropanols, 50 L sulfydryl second in the nano silver wire suspension described in embodiment 20.1
Acid, stirs；
20.3 add 0.025 mL butyl titanate in the mixed liquor described in embodiment 20.2, are uniformly mixed；
Mixed liquor described in embodiment 20.3 is transferred in 50 mL reactors by 20.4,150 DEG C, reacts 10 h.
20.5 by embodiment 20.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure, titanium dioxide thickness of the shell is 5 nm, a diameter of 50 nm of nano silver wire.
Embodiment 21
0.1 mmol nano silver wire is directly dispersing in 5 mL ethanol by 21.1, impregnates 12 h, obtains suspension；
21.2 add 15 mL n-amyl alcohols, 20 L sulfydryl second in the nano silver wire suspension described in embodiment 21.1
Acid, stirs；
21.3 add 0.5 mL butyl titanate in the mixed liquor described in embodiment 21.2, are uniformly mixed；
Mixed liquor described in embodiment 21.3 is transferred in 50 mL reactors by 21.4,150 DEG C, reacts 10 h.
21.5 by embodiment 21.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure, titanium dioxide thickness of the shell is 85 nm, a diameter of 40 nm of nano silver wire.
Embodiment 22
0.1 mmol nano silver wire is directly dispersing in 5 mL butanol by 22.1, impregnates 12 h, obtains suspension；
22.2 add 15 mL ethanol in the nano silver wire suspension described in embodiment 22.1,100 L TGAs,
Stir；
22.3 add 0.5 mL butyl titanate in the mixed liquor described in embodiment 22.2, are uniformly mixed；
Mixed liquor described in embodiment 22.3 is transferred in 50 mL reactors by 22.4,120 DEG C, reacts 4 h.
22.5 by embodiment 22.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure, titanium dioxide thickness of the shell is 65 nm, a diameter of 30 nm of nano silver wire.
Embodiment 23
0.1 mmol nano silver wire is directly dispersing in 5 mL ethanol by 23.1, impregnates 1 day, obtains suspension；
23.2 add 15 mL ethanol in the nano silver wire suspension described in embodiment 23.1,35 L TGAs,
Stir；
23.3 add 0.5 mL butyl titanate in the mixed liquor described in embodiment 23.2, are uniformly mixed；
Mixed liquor described in embodiment 23.3 is transferred in 50 mL reactors by 23.4,120 DEG C, reacts 10 h.
23.5 by embodiment 23.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure, titanium dioxide thickness of the shell is 90 nm, a diameter of 50 nm of nano silver wire.
Embodiment 24
0.1 mmol nano silver wire is directly dispersing in 5 mL ethanol by 24.1, impregnates 1 day, obtains suspension；
24.2 add 15 mL ethanol in the nano silver wire suspension described in embodiment 24.1,75 L TGAs,
Stir；
24.3 add 0.5 mL butyl titanate in the mixed liquor described in embodiment 24.2, are uniformly mixed；
Mixed liquor described in embodiment 24.3 is transferred in 50 mL reactors by 24.4,120 DEG C, reacts 20 h.
24.5 by embodiment 24.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure, titanium dioxide thickness of the shell is 90 nm, a diameter of 40 nm of nano silver wire.
Embodiment 25
0.1 mmol nano silver wire is directly dispersing in 5 mL ethanol by 25.1, impregnates 1 day, obtains suspension；
25.2 add 15 mL ethanol in the nano silver wire suspension described in embodiment 25.1,50 L TGAs,
Stir；
25.3 add 0.5 mL butyl titanate in the mixed liquor described in embodiment 25.2, are uniformly mixed；
Mixed liquor described in embodiment 25.3 is transferred in 50 mL reactors by 25.4,200 DEG C, reacts 4 h.
25.5 by embodiment 25.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure, titanium dioxide thickness of the shell is 75 nm, a diameter of 30 nm of nano silver wire.
Embodiment 26
0.1 mmol nano silver wire is directly dispersing in 5 mL ethanol by 26.1, impregnates 12 h, obtains suspension；
26.2 add 15 mL ethanol in the nano silver wire suspension described in embodiment 26.1,10 L TGAs,
Stir；
26.3 add 0.5 mL butyl titanate in the mixed liquor described in embodiment 26.2, are uniformly mixed；
Mixed liquor described in embodiment 26.3 is transferred in 50 mL reactors by 26.4,200 DEG C, reacts 20 h.
26.5 by embodiment 26.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure, titanium dioxide thickness of the shell is 95 nm, a diameter of 60 nm of nano silver wire.
Embodiment 27
0.1 mmol nano silver wire is directly dispersing in 5 mL ethanol by 27.1, impregnates 12 h, obtains suspension；
27.2 add 15 mL n-butyl alcohol in the nano silver wire suspension described in embodiment 27.1, stir；
27.3 add 0.1 mL butyl titanate in the mixed liquor described in embodiment 27.2, are uniformly mixed；
Mixed liquor described in embodiment 27.3 is transferred in 50 mL reactors by 27.4,160 DEG C, reacts 10 h.
27.5 by embodiment 27.4 gained sample, is centrifuged washing, prepares nano silver wire and TiO2Hud typed hetero-junctions
Structure (as shown in Figure 10), titanium dioxide thickness of the shell is 70 nm, a diameter of 40 nm of nano silver wire.
Embodiment 28
AgNWs@TiO with embodiment 5,6,7 and 162Pelletron type and hud typed heterojunction structure as a example by, verify this
The catalytic effect of bright sample, its step is as follows:
The 28.1 AgNWs@TiO taking 10 mg2Pelletron type (embodiment 5,6,7 sample) and AgNWs@TiO2Hud typed
Sample (embodiment 16 sample), is separately added in the methyl orange solution of 20 mL 10 mg/L；
Methyl orange solution is stirred 30 min at dark by 28.2, makes solution be in adsorption equilibrium state, then in ultraviolet
Irradiate under light (light source 12 W), take out 2 mL samples every 30 min and carry out absorbing test, measure methyl orange in now solution
Absorbance, calculates concentration according to langbobier law, calculates sampling concentration and initial orange concentration proportion；
28.3 with the time as abscissa, and sampling concentration is vertical coordinate with initial concentration ratio, draws curve, such as Figure 11 institute
Show；As can be seen from the figure: two kinds of heterojunction structures of the present invention are respectively provided with photocatalysis effect, the catalytic effect of embodiment 5 and 16 is
It is good that (embodiment 5, ultraviolet lighting 150 min degraded methyl orange degree is 50%；Embodiment 16, ultraviolet lighting 150 min degrades first
Base orange degree is 56%).
Claims (12)
1. a Silver/titanium dioxide composite heterostructure, is characterized in that: described silver is nano silver wire, is covered with on nano silver wire
Titanium dioxide shell, nano silver wire and titanium dioxide form hud typed composite heterogenous junction structure；
The preparation method of described Silver/titanium dioxide composite heterostructure comprises the following steps:
(1) being disperseed in a solvent by nano silver wire, time of infusion makes solvent carry out moistening on the surface of nano silver wire, obtains silver-colored
Nanowire suspended liquid；
(2) stir under addition alcohol and bridging agent, room temperature in nano silver wire suspension；
(3) in the suspension of step (2), add titanium source, stir under room temperature；
(4) temperature of the suspension of ascending step (3), make titanium dioxide deposition on nano silver wire surface, centrifugation after reaction,
Washing, obtains Silver/titanium dioxide composite heterostructure；Described bridging agent is TGA or mercaptopropionic acid；
Wherein, the solvent in step (1) is deionized water, and the alcohol in step (2) is that isopropanol or carbon chain lengths are more than or equal to four
Monohydric alcohol；Or, the solvent in step (1) is methanol, ethanol, propanol or butanol, and the alcohol in step (2) is arbitrary unitary
Alcohol；
The volume ratio of titanium source and bridging agent is (1 ~ 10): (0 ~ 2), and wherein bridging agent volume is not 0.
Silver/titanium dioxide composite heterostructure the most according to claim 1, is characterized in that: described nano silver wire is a diameter of
10-60 nm；Described titanium dioxide thickness of the shell is 5-100 nm.
Silver/titanium dioxide composite heterostructure the most according to claim 2, is characterized in that: described titanium dioxide thickness of the shell
For 30nm.
4. a Silver/titanium dioxide composite heterostructure, is characterized in that: include nano silver wire, on described nano silver wire string have to
A few titanium dioxide ball, all titanium dioxide balls are chained together by described nano silver wire, form pelletron type composite heterogenous junction
Structure.
Silver/titanium dioxide composite heterostructure the most according to claim 4, is characterized in that: tight between each titanium dioxide ball
Close be connected or there is certain interval.
Silver/titanium dioxide composite heterostructure the most according to claim 4, is characterized in that: described nano silver wire is polycrystalline
Nano silver wire, a diameter of 10-60 nm；The average diameter of described titanium dioxide ball is 200-600 nm.
Silver/titanium dioxide composite heterostructure the most according to claim 6, is characterized in that: putting down of described titanium dioxide ball
The most a diameter of 450nm.
8. a preparation method for Silver/titanium dioxide composite heterostructure, is characterized in that: deposit titanium dioxide on nano silver wire surface
Titanium thus form hud typed or pelletron type composite heterogenous junction structure, comprise the following steps:
(1) being disperseed in a solvent by nano silver wire, time of infusion makes solvent carry out moistening on the surface of nano silver wire, obtains silver-colored
Nanowire suspended liquid；
(2) stir under addition alcohol and bridging agent, room temperature in nano silver wire suspension；
(3) in the suspension of step (2), add titanium source, stir under room temperature；
(4) temperature of the suspension of ascending step (3), make titanium dioxide deposition on nano silver wire surface, centrifugation after reaction,
Washing, obtains Silver/titanium dioxide composite heterostructure；Described bridging agent is TGA or mercaptopropionic acid；
In step (1), the solvent of dispersion nano silver wire is deionized water, methanol, ethanol, propanol or butanol；In step (2), institute
Stating alcohol is monohydric alcohol；
When the alcohol during the solvent in step (1) is deionized water, step (2) is methanol, ethanol or propanol, products obtained therefrom is silver
Nano wire and the pelletron type composite heterogenous junction structure of titanium dioxide；In the solvent in step (1) is deionized water, step (2)
When alcohol is isopropanol or the carbon chain lengths monohydric alcohol more than or equal to four, what products obtained therefrom was nano silver wire with titanium dioxide is hud typed
Composite heterogenous junction structure；Alcohol in the solvent in step (1) is methanol, ethanol, propanol or butanol, step (2) is arbitrary unitary
During alcohol, products obtained therefrom is the hud typed composite heterogenous junction structure of nano silver wire and titanium dioxide；
When preparing pelletron type composite heterogenous junction structure, the volume ratio of titanium source and bridging agent is (1 ~ 10): (0.4 ~ 2), prepares hud typed
During composite heterogenous junction structure, the volume ratio of titanium source and bridging agent is (1 ~ 10): (0 ~ 2), and wherein bridging agent volume is not 0.
Preparation method the most according to claim 8, is characterized in that: in step (3), and described titanium source is butyl titanate, titanium
Acid orthocarbonate.
Preparation method the most according to claim 8, is characterized in that: in step (3), and described titanium source is isopropyl titanate.
11. preparation methoies according to claim 8, is characterized in that: in step (1), and the time of dipping is 4h-7 days；Step
(4) in, suspension being risen to 120-200 DEG C and reacts, the response time is 4-20 h.
Preparation method 12. according to Claim 8, described in 9,10 or 11, is characterized in that: nano silver wire with the mol ratio in titanium source is
1:0.7~14；Described titanium source and bridging agent are liquid.
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| CN106141170B (en) * | 2015-02-02 | 2018-08-10 | 中国科学院苏州纳米技术与纳米仿生研究所 | Gold nanorods/titanium dioxide core-shell nanostructure and its one-step synthesis method method |
| CN105551811B (en) * | 2016-01-18 | 2018-05-15 | 吉林大学 | The porous SnO of graded structure2And TiO2The Ag@C nanos ball of cladding, preparation method and applications |
| CN105771977A (en) * | 2016-03-22 | 2016-07-20 | 济南大学 | Method for preparing graphene oxide coated carbon fiber-silver loaded TiO2 nano-wire array composite materials and application thereof |
| CN106057357A (en) * | 2016-06-15 | 2016-10-26 | 浙江大学 | Method for preparing silver nanowire-titanium dioxide composite transparent electrode and transparent electrode |
| TWI623945B (en) * | 2016-06-20 | 2018-05-11 | 國立清華大學 | Sensing device and methods of forming the same |
| TWI658155B (en) * | 2016-06-20 | 2019-05-01 | 國立清華大學 | Methods of forming nanowire composite structures |
| CN107376941B (en) * | 2017-06-22 | 2020-04-24 | 西安交通大学苏州研究院 | Preparation method of nanorod photocatalyst with core-shell structure |
| CN107469817B (en) * | 2017-08-04 | 2020-05-22 | 江苏安纳泰环保科技有限公司 | Silver nanorod-titanium dioxide composite material and preparation method and application thereof |
| CN108735409B (en) * | 2018-05-03 | 2020-10-09 | 上海理工大学 | Preparation method of core-shell structure nano composite material |
| JP2020040047A (en) * | 2018-09-13 | 2020-03-19 | 株式会社東芝 | Photocatalyst dispersion liquid, photocatalyst composite material and photocatalyst device |
| CN109742184B (en) * | 2018-12-11 | 2021-11-16 | 厦门大学 | Preparation method of semiconductor-wrapped metal nanowire |
| CN109503889B (en) * | 2018-12-17 | 2020-11-13 | 安徽大学 | Preparation method of silver nanowire hybrid filler and composite material using filler |
| CN110092933B (en) * | 2019-05-28 | 2021-06-29 | 中国人民解放军陆军工程大学 | Method for preparing field reversible nonlinear conductive composite material, prepared material and application |
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