CN107720711A - The more thorn-like magnetic telluride nickel nano wires of functional gold and preparation, application - Google Patents
The more thorn-like magnetic telluride nickel nano wires of functional gold and preparation, application Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of more thorn-like magnetic telluride nickel nano wires, comprise the following steps：Tellurous acid or tellurite are added in nickel salt aqueous solution, stirring obtains turbid solution；Hydrazine hydrate solution is added dropwise into turbid solution, it is that brown obtains mixed solution to stir to solution；Mixed solution is subjected to hydro-thermal reaction, hydrothermal temperature is 120~160 DEG C, and the hydro-thermal reaction time is 4~10h, washing, is dried to obtain more thorn-like magnetic telluride nickel nano wires.The invention also discloses above-mentioned more thorn-like magnetic telluride nickel nano wires.The invention also discloses a kind of more thorn-like magnetic telluride nickel nano wires of functional gold.The invention also discloses more thorn-like magnetic telluride nickel nanowire preparation methods of above-mentioned functional gold.The invention also discloses the application of more thorn-like magnetic telluride nickel nano wires of above-mentioned functional gold.
Description
Technical field
The present invention relates to monodimension nanometer material technical field, more particularly to a kind of more thorn-like magnetic telluride nickel nano wires and its
Preparation method, more thorn-like magnetic telluride nickel nano wires of a kind of functional gold and preparation method thereof, application.
Background technology
The nanostructureds such as noble metal gold nano grain, gold nanorods, nanowires of gold, due in the only of light, electricity, power etc.
Property values, it is set to be had broad application prospects as sensitive body material in fields such as biochemical sensor, opto-electronic devices.But price of gold
Lattice are expensive, and in order to cost-effective, later stage research arrives gold nano grain decoration on the surface of other nanometer body materials, it is expected to reach same
The sensitive Detection results of sample.
Research of the early stage primarily with respect to the gold nano body material such as gold nano grain, gold nanorods.For example, W.R.Yang etc. is comprehensive
State preparation and the optical property progress of research [Materials2014,7,5169-5201] reported on gold nano material body；
The mode that Y.S.Yang etc. is irradiated using linear polarization laser be prepared for gold nano grain, nanorod and nanowire [Sci Rep.,
2017,7,44680].In addition, sacrifice template also be used to preparing one-dimensional nanowires of gold, nanotube etc., Ballabh, R. etc. with
Sodium sulphate nano wire as sacrifice template, using chemical deposition synthesized gold nanotubes [Indian J.Exp.Biol.,
2015,53,828-33]。
Report of the gold nano grain decoration to other nanometer body material surfaces is more, wherein for use as electrochemical sensor
Sensitive layer application is wider.For example, H.W, Wang etc. are used as molecular imprinting electricity using the multi-walled carbon nanotube for being modified with gold nano grain
The sensitive material [Biosens Bioelectron., 2017,87,417-421] of chemical sensor；X.Liu etc. is by titanium dioxide
Nanotube/polyaniline/gold nano grain is assembled on electrode, and constructing electrochemical enzymatic biology using the synergy between three passes
Sensor [Anal.Chim.Acta., 2016,911,59-68].
However, when liquid phase prepares gold nano grain, because particle size is small, surface energy is big, and gold nano grain holds
Agglomeration easily occurs, prior art often use anti-coagulants, then repeatedly cleans the product process of preparation repeatedly, reaches point
Dissipate the purpose of gold nano grain, nanometer rods etc..For example, Tan, S.F. etc. using disodium ethylene diamine tetraacetate complexing gold particle with
Silver nanocubes reaction be reduced into gold nano grain uniform deposition cube face [ACS Nano., 2016,10,
7689-95].But the introducing of anti-coagulants can cause preparation process complexity, introduce new impurity, influence subsequent detection effect etc..
Research at present is considered as and the golden nano material that can be formed Ka and cut down Buddhist nun's displacement reaction, in metal with silver, platinum most
It is common.For example, Sun, Y etc. have monitored reaction of the nano silver wire in chlorauric acid solution in real time, cutting down Buddhist nun's displacement by Ka observes
Change procedure [Nano Lett., 2011,11,4386-92] of its pattern from nano silver wire to gold nanotubes；Slater,T.J.
Deng the Ka using silver particles and gold chloride cut down Buddhist nun displacement directly synthesis hollow silver/gold nano grain [Nano Lett., 2014,14,
1921-6]；Goodman, A.M. etc. cut down Buddhist nun using Ka and replace gold/silver nanoparticle core shell structure of the synthesis using silver as kernel, near
Infrared resonance detection [ACS Nano., 2014,8,3222-31]；Hsu, C. etc. cut down Buddhist nun's displacement using Ka and have synthesized gold/platinoid core
Shell particle [Phys.Chem.Chem.Phys., 2012,14,4696-701].
And it is nonmetallic with it is golden between Ka cut down Buddhist nun replace react, wherein most commonly seen with silicon, carbon.Such as the profit such as Lee, S.H.
Buddhist nun's displacement reaction is cut down with the Ka between silicon and gold to load gold grain to silicon face to improve the temperature coefficient of the resistivity of silicon
[ACS Nano.,2017,11,1572-1580]；Kye, J. etc. cut down Buddhist nun using the Ka between silicon and gold and replace reaction by gold nano
Structure is formed and silicon face [ACS Nano., 2013,7,6017-23]；Sayed, S.Y. etc. have studied cuts down Buddhist nun's displacement instead by Ka
Should, the nano heterojunction that is formed between silicon and gold [ACS Nano., 2009,3,2809-17]；Yu, C. etc. put into CNT
In chlorauric acid solution, using Ka cut down Buddhist nun replace reaction reduction gold nano grain to carbon nano tube surface [ACS Nano., 2011,5,
1297-303]。
Chalcogenide CdSe, CdTe, ZnS, ZnTe etc. have unique optical and electrical properties, particularly functionalization gold nano
After particle, have wide practical use in catalyst, antiseptic, biomedicine, solar cell etc..Such as Costi,
A.E. Reporting of Overview metal/semiconductor functionalization and hybridization nano material is waited, wherein having highlighted the chalcogenide of golden functionalization
Compound Au@CdSe, Au@ZnS, Au@CdS etc. controllable preparation [Angew Chem.Int.Edit., 2010,49,4878-
4897]；Costi, A.E. etc., by optimizing solution concentration, utilize chemical metal deposition method under conditions of visible ray is according to auxiliary
Deposit gold nano grain on CdSe nanometer rods top, synthesized Au-CdSe nanometer rods [Nano Lett., 2008,8,637-
641]；Zheng, Q. etc. utilize electroless deposition method reduction platinum, gold nano grain [Thin Solid on CdZnTe surfaces
Films, 2012,525,56-63].
Preparing for present telluride nickel nano material is actually rare, and existing report is often nanometer rods
[Nano.Struct.Mater., 1999,8,1057-1071], nano-hollow ball [patent CN103058289], nano wire
[Inorg.Chem.,2003,42,2174-2175].But it there is no at present on more thorn-like magnetic telluride nickel (NiTe) nano wires
With the relevant report of the more thorn-like magnetic telluride nickel of functional gold (Au NiTe) nano wire.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of more thorn-like magnetic of functional gold
Property telluride nickel nano wire and preparation, application, technique are simple, low production cost, without using any dispersant and surfactant,
Preparation process is easily controlled, and sample post processing is simple, is extremely suitable for industrialized production, and more thorn-like magnetic telluride nickel nanometers
The gold nano grain of line surface modification is evenly distributed.
A kind of preparation method of more thorn-like magnetic telluride nickel nano wires proposed by the present invention, comprises the following steps：
S1, tellurous acid or tellurite added in nickel salt aqueous solution, stirring obtains turbid solution；
S2, hydrazine hydrate solution is added dropwise into turbid solution, it is that brown obtains mixed solution to stir to solution；
S3, mixed solution carrying out to hydro-thermal reaction, hydrothermal temperature is 120~160 DEG C, the hydro-thermal reaction time is 4~
10h, washing, is dried to obtain more thorn-like magnetic telluride nickel nano wires.
In embodiment, in S3 hydrothermal temperature can be 120 DEG C, 125 DEG C, 130 DEG C, 135 DEG C, 140 DEG C,
142 DEG C, 145 DEG C, 148 DEG C, 150 DEG C, 152 DEG C, 155 DEG C, 158 DEG C, 160 DEG C, in S3 the hydro-thermal reaction time can be 4h, 5h,
6h、7h、8h、8.2h、8.5h、8.8h、9h、9.5h、10h。
In the present invention, the effect of hydrazine hydrate is to be used to reduce crosslinking agent and regulation solution ph.
After adding hydrazine hydrate in S2 of the present invention, solution colour becomes green from colourless, eventually becomes brown.
Preferably, in S1, the mol ratio of tellurious acid ion and nickel ion is 0.5~1：1.
Preferably, in S1, nickel salt is nickel sulfate, nickel chloride or nickel acetylacetonate.
Preferably, in S1, mixing time is 20~60min.
Preferably, in S2, the mass fraction of hydrazine hydrate solution is 25~30wt%.
Preferably, in S2, the pH value of mixed solution is 8~10.
Above-mentioned more thorn-like magnetic telluride nickel nano wires that the present invention also proposes, using above-mentioned more thorn-like magnetic telluride nickel nanometers
The preparation method of line is made.
A kind of more thorn-like magnetic telluride nickel nanowire preparation methods for functional gold that the present invention also proposes, bag
Include following steps：Above-mentioned more thorn-like magnetic telluride nickel nano wires are added in aqueous solution of chloraurate, normal temperature shaking table is reacted to solution
Clarification, obtains more thorn-like magnetic telluride nickel nano wires of functional gold.
Preferably, the mass volume ratio (mg/mL) of above-mentioned more thorn-like magnetic telluride nickel nano wires and aqueous solution of chloraurate is 2
~6：1, the mass fraction of aqueous solution of chloraurate is 0.01~0.05wt%.
Preferably, the shaking table reaction time is 6~24h.
The more thorn-like magnetic telluride nickel nano wires for the above-mentioned functional gold that the present invention also proposes, using above-mentioned work(
More thorn-like magnetic telluride nickel nanowire preparation methods that gold nano grain can be changed are made.
The more thorn-like magnetic telluride nickel nano wires for the above-mentioned functional gold that the present invention also proposes are used in preparation
Micro-nano electronic device, biochemical sensor, solar cell nano material in application.
The preparation technology of the present invention is simple, low production cost, without using any dispersant and surfactant, prepares
Journey is easily controlled, and sample post processing is simple, is extremely suitable for industrialized production；The present invention is in more thorn-like magnetic telluride nickel nano wires
The gold nano grain of surface modification is evenly distributed.
More thorn-like magnetic telluride nickel nano wires of gained functional gold of the invention will be micro-nano electronic device, life
Change sensor, solar cell etc. and novel nano-material is provided.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of the more thorn-like magnetic telluride nickel nano wires of the gained of the embodiment of the present invention 1.
Fig. 2 is the panorama of more thorn-like magnetic telluride nickel nano wires of the gained functional gold of the embodiment of the present invention 1
Scanning electron microscope diagram.
Fig. 3 is the transmission of more thorn-like magnetic telluride nickel nano wires of the gained functional gold of the embodiment of the present invention 1
Electron microscope.
Fig. 4 is the electronics of more thorn-like magnetic telluride nickel nano wires of the gained functional gold of the embodiment of the present invention 1
Diffraction spectroscopy figure.
Embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of more thorn-like magnetic telluride nickel nanowire preparation methods of functional gold, comprise the following steps：
S1, by 1.19g Nickel dichloride hexahydrates add 30ml deionized waters in, magnetic agitation is completely dissolved it, adds
0.56g sodium tellurites, white precipitate is produced immediately, magnetic agitation 40min, obtains turbid solution；
S2, into turbid solution, dropwise addition mass fraction is the hydrazine hydrate solution that 10ml mass fractions are 25wt%, and magnetic force stirs
Mix and be changed into brown to solution and obtain mixed solution；
S3, mixed solution is transferred in autoclave, and puts it into heated at constant temperature case and carry out, hydro-thermal reaction,
Hydrothermal temperature is 140 DEG C, the hydro-thermal reaction time 8h, washing, is dried to obtain more thorn-like magnetic telluride nickel nano wires；
S4, will 1g gold chlorides put into 100ml deionized waters in dissolving obtain mass fraction be 1wt% chlorauric acid solution,
Then it is diluted to the chlorauric acid solution that mass fraction is 0.02wt% with deionized water；It is to 10ml mass fractions
The more thorn-like magnetic telluride nickel nano wires of 30mg are added in 0.02wt% chlorauric acid solution, normal temperature shaking table reaction 12h is clear to solution
Clearly, more thorn-like magnetic telluride nickel nano wires of functional gold are obtained.
As shown in figure 1, Fig. 1 is the transmission electron microscope picture of more thorn-like magnetic telluride nickel nano wires obtained by the present embodiment.Can from Fig. 1
To find out：A diameter of 42-88nm of more thorn-like magnetic telluride nickel nano wires, the length that it is pierced is up to 160nm.
As shown in Fig. 2 Fig. 2 is more thorn-like magnetic telluride nickel nano wires of functional gold obtained by the present embodiment
Panoramic scanning electron microscope picture.As can be known from Fig. 2：Products therefrom shape homogeneity is preferable, is distributed on the nano wire of more thorn-likes
Nano particle.
As shown in figure 3, Fig. 3 is more thorn-like magnetic telluride nickel nano wires of functional gold obtained by the present embodiment
Transmission electron microscope picture.It can clearly be seen that nanowire surface uniform fold nano particle from Fig. 3, the size of these particles is equal
Even property is preferable.
As shown in figure 4, Fig. 4 is the electronic diffraction energy spectrum diagram of black rectangles thin slice.Fig. 4 can be confirmed that it is Au@NiTe,
That is more thorn-like magnetic telluride nickel nano wires of functional gold.
Embodiment 2
A kind of more thorn-like magnetic telluride nickel nanowire preparation methods of functional gold, comprise the following steps：
S1, by 1.32g six hydration nickel sulfates add 30ml deionized waters in, magnetic agitation is completely dissolved it, adds
1.11g sodium tellurites, produce white precipitate immediately, and magnetic agitation obtains turbid solution；
S2, into turbid solution, dropwise addition mass fraction is the hydrazine hydrate solution that 10ml mass fractions are 25wt%, and magnetic force stirs
Mix and be changed into brown to solution and obtain mixed solution；
S3, mixed solution is transferred in autoclave, and puts it into heated at constant temperature case and carry out, hydro-thermal reaction,
Hydrothermal temperature is 120 DEG C, the hydro-thermal reaction time 6h, and gained sediment is used into water and ethanol eccentric cleaning respectively, is dried
Obtain more thorn-like magnetic telluride nickel nano wires；
S4, will 1g gold chlorides put into 100ml deionized waters in dissolving obtain mass fraction be 1wt% chlorauric acid solution,
Then it is diluted to the chlorauric acid solution that mass fraction is 0.01wt% with deionized water；It is to 10ml mass fractions
The more thorn-like magnetic telluride nickel nano wires of 40mg are added in 0.01wt% chlorauric acid solution, normal temperature shaking table reaction 24h is clear to solution
Clearly, more thorn-like magnetic telluride nickel nano wires of functional gold are obtained.
Embodiment 3
A kind of more thorn-like magnetic telluride nickel nanowire preparation methods of functional gold, comprise the following steps：
S1, by 1.02g nickel acetylacetonates add 30ml deionized waters in, magnetic agitation is completely dissolved it, adds
0.88g sodium tellurites, white precipitate is produced immediately, magnetic agitation 60min, obtains turbid solution；
S2, into turbid solution, dropwise addition mass fraction is the hydrazine hydrate solution that 15ml mass fractions are 25wt%, and magnetic force stirs
Mix and be changed into brown to solution and obtain mixed solution；
S3, mixed solution is transferred in autoclave, and puts it into heated at constant temperature case and carry out, hydro-thermal reaction,
Hydrothermal temperature is 130 DEG C, the hydro-thermal reaction time 10h, and gained sediment is used into water and ethanol eccentric cleaning respectively, is dried
Obtain more thorn-like magnetic telluride nickel nano wires；
S4, will 1g gold chlorides put into 100ml deionized waters in dissolving obtain mass fraction be 1wt% chlorauric acid solution,
Then it is diluted to the chlorauric acid solution that mass fraction is 0.02wt% with deionized water；It is to 10ml mass fractions
The more thorn-like magnetic telluride nickel nano wires of 20mg are added in 0.02wt% chlorauric acid solution, normal temperature shaking table reaction 16h is clear to solution
Clearly, more thorn-like magnetic telluride nickel nano wires of functional gold are obtained.
Embodiment 4
A kind of more thorn-like magnetic telluride nickel nanowire preparation methods of functional gold, comprise the following steps：
S1, by 1.32g six hydration nickel sulfates add 30ml deionized waters in, magnetic agitation is completely dissolved it, adds
0.89g tellurous acid, produces white precipitate immediately, and magnetic agitation obtains turbid solution；
S2, mass fraction is added dropwise into turbid solution is hydrazine hydrate solution that 5ml mass fractions are 25wt%, magnetic agitation
It is changed into brown to solution and obtains mixed solution；
S3, mixed solution is transferred in autoclave, and puts it into heated at constant temperature case and carry out, hydro-thermal reaction,
Hydrothermal temperature is 150 DEG C, the hydro-thermal reaction time 10h, and gained sediment is used into water and ethanol eccentric cleaning respectively, is dried
Obtain more thorn-like magnetic telluride nickel nano wires；
S4, will 1g gold chlorides put into 100ml deionized waters in dissolving obtain mass fraction be 1wt% chlorauric acid solution,
Then it is diluted to the chlorauric acid solution that mass fraction is 0.01wt% with deionized water；It is to 10ml mass fractions
The more thorn-like magnetic telluride nickel nano wires of 60mg are added in 0.01wt% chlorauric acid solution, normal temperature shaking table reaction 24h is clear to solution
Clearly, more thorn-like magnetic telluride nickel nano wires of functional gold are obtained.
Embodiment 5
A kind of preparation method of more thorn-like magnetic telluride nickel nano wires, comprises the following steps：
S1, tellurous acid added in nickel chloride aqueous solution, the mol ratio of tellurous acid and nickel ion is 0.5：1, stirring
60min, obtain turbid solution；
S2, the hydrazine hydrate solution that mass fraction is 25wt% is added dropwise into turbid solution, stirs to solution and obtained for brown
PH value is 10 mixed solution；
S3, mixed solution being carried out to hydro-thermal reaction, hydrothermal temperature is 120 DEG C, the hydro-thermal reaction time 10h, washing,
It is dried to obtain more thorn-like magnetic telluride nickel nano wires.
A kind of more thorn-like magnetic telluride nickel nanowire preparation methods of functional gold, comprise the following steps：Will
Above-mentioned more thorn-like magnetic telluride nickel nano wires are added in the aqueous solution of chloraurate that mass fraction is 0.05wt%, more thorn-like magnetic telluriums
The mass volume ratio (mg/mL) for changing nickel nano wire and aqueous solution of chloraurate is 2：1, normal temperature shaking table reaction 6h, clarify, obtain to solution
To more thorn-like magnetic telluride nickel nano wires of functional gold.
Embodiment 6
A kind of preparation method of more thorn-like magnetic telluride nickel nano wires, comprises the following steps：
S1, potassium tellurite added in the nickel acetylacetonate aqueous solution, the mol ratio of tellurious acid ion and nickel ion is 1：
1,20min is stirred, obtains turbid solution；
S2, the hydrazine hydrate solution that mass fraction is 30wt% is added dropwise into turbid solution, stirs to solution and obtained for brown
PH value is 8 mixed solution；
S3, mixed solution being carried out to hydro-thermal reaction, hydrothermal temperature is 160 DEG C, the hydro-thermal reaction time 4h, washing,
It is dried to obtain more thorn-like magnetic telluride nickel nano wires.
A kind of more thorn-like magnetic telluride nickel nanowire preparation methods of functional gold, comprise the following steps：Will
Above-mentioned more thorn-like magnetic telluride nickel nano wires are added in aqueous solution of chloraurate, more thorn-like magnetic telluride nickel nano wires and mass fraction
Mass volume ratio (mg/mL) for 0.01wt% aqueous solution of chloraurate is 6：1, normal temperature shaking table reaction 24h, clarified to solution,
Obtain more thorn-like magnetic telluride nickel nano wires of functional gold.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of more thorn-like magnetic telluride nickel nano wires, it is characterised in that comprise the following steps：
S1, tellurous acid or tellurite added in nickel salt aqueous solution, stirring obtains turbid solution；
S2, hydrazine hydrate solution is added dropwise into turbid solution, it is that brown obtains mixed solution to stir to solution；
S3, mixed solution being carried out to hydro-thermal reaction, hydrothermal temperature is 120~160 DEG C, and the hydro-thermal reaction time is 4~10h,
Washing, is dried to obtain more thorn-like magnetic telluride nickel nano wires.
2. the preparation method of more thorn-like magnetic telluride nickel nano wires according to claim 1, it is characterised in that in S1, tellurious
The mol ratio of acid ion and nickel ion is 0.5~1：1.
3. the preparation method of more thorn-like magnetic telluride nickel nano wires according to claim 1 or claim 2, it is characterised in that in S1, nickel
Salt is nickel sulfate, nickel chloride or nickel acetylacetonate.
4. according to the preparation method of any one of claim 1-3 more thorn-like magnetic telluride nickel nano wires, it is characterised in that S2
In, the mass fraction of hydrazine hydrate solution is 25~30wt%；Preferably, the pH value of mixed solution is 8~10.
5. a kind of more thorn-like magnetic telluride nickel nano wires, it is characterised in that using any one of claim 1-4 more thorn-like magnetic
The preparation method of property telluride nickel nano wire is made.
A kind of 6. more thorn-like magnetic telluride nickel nanowire preparation methods of functional gold, it is characterised in that including with
Lower step：More thorn-like magnetic telluride nickel nano wires it will add as claimed in claim 5 in aqueous solution of chloraurate, the reaction of normal temperature shaking table
Clarified to solution, obtain more thorn-like magnetic telluride nickel nano wires of functional gold.
7. more thorn-like magnetic telluride nickel nanowire preparation methods of functional gold according to claim 6, it is special
Sign is, the mass volume ratio (mg/mL) of more thorn-like magnetic telluride nickel nano wires and aqueous solution of chloraurate as claimed in claim 5
For 2~6：1, the mass fraction of aqueous solution of chloraurate is 0.01~0.05wt%.
8. according to more thorn-like magnetic telluride nickel nanowire preparation methods of the functional gold of claim 5 or 6, its
It is characterised by, the shaking table reaction time is 6~24h.
9. more thorn-like magnetic telluride nickel nano wires of a kind of functional gold, it is characterised in that using claim 5-8
More thorn-like magnetic telluride nickel nanowire preparation methods of any one functional gold are made.
10. a kind of more thorn-like magnetic telluride nickel nano wires of functional gold are being prepared for micro-nano electronic device, life
Change the application in the nano material of sensor, solar cell.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108922784A (en) * | 2018-08-31 | 2018-11-30 | 扬州大学 | The non-platinum of dye-sensitized solar cells is to electrode CoTe/Te nano wire and preparation method thereof |
| CN114062449A (en) * | 2021-10-29 | 2022-02-18 | 合肥师范学院 | Molecularly imprinted electrochemical sensor for detecting L-lysine and application thereof |
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