CN108907224A - A kind of method and its application of silver nanowires amplification preparation - Google Patents
A kind of method and its application of silver nanowires amplification preparation Download PDFInfo
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- CN108907224A CN108907224A CN201810692144.6A CN201810692144A CN108907224A CN 108907224 A CN108907224 A CN 108907224A CN 201810692144 A CN201810692144 A CN 201810692144A CN 108907224 A CN108907224 A CN 108907224A
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- silver nanowires
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- silver
- ethylene glycol
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Abstract
The present invention provides a kind of method and its application of silver nanowires amplification preparation, include the following steps：(1) polyvinylpyrrolidone is dissolved in ethylene glycol, heats 1-2h under stirring, obtain the first solution；(2) ferric chloride solution is added dropwise in first solution dropwise, is heated to 100-120 DEG C, obtain the second solution；The mass ratio of the iron chloride and polyvinylpyrrolidone is 1:(0.5~5)；(3) ethylene glycol solution of silver nitrate is added drop-wise in second solution, 2-5min is stirred under 200-400rpm revolving speed, after being sufficiently mixed uniformly, closes stirring, sustained response 15h-17h, after refrigerated separation, washing obtains silver nanowires, the silver nanowires that the method for the present invention is prepared not only morphology controllable, stable structure, it is reproducible, while there is good SERS activity.
Description
Technical field
The invention belongs to field of nanometer material technology more particularly to a kind of method and its application of silver nanowires amplification preparation.
Background technique
Surface enhanced Raman scattering (Surface enhanced Raman Scattering, SERS) technology is widely applied
It is that research is single in the orientation and conformation of the detection of super low concentration molecule, macromolecular or small molecule, the chemical phase of composite material etc.
Molecule, surface, interface and phase structure important tool.Forefathers' studies have shown that metallic surface form is to generate SERS effect
One of important factor in order, therefore metal nanoparticle is concentrated mainly on to the research for the metallic matrix that can be used for SERS effect
Size and shape synthesis and control etc..It is silver nanostructured due to good physicochemical properties and optical
Matter is that SERS studies the various common matrixes of Physico-Chemical Problems.In numerous silver-colored micro-nano structures, silver nanowires structure causes
The extensive concern of people, however there are still poor repeatability, preparation process are complicated, experiment condition not easy-regulating, it is difficult on a large scale
The problems such as synthesis.
Summary of the invention
For the drawbacks described above in background technique, the main purpose of the present invention is to provide a kind of amplifications of silver nanowires to prepare
Method and its application, the silver nanowires (referred to as AgNWs) that this method is prepared not only morphology controllable, stable structure, weight
Renaturation is good, while having good SERS activity.
In order to achieve the above object, the present invention adopts the following technical scheme that：A kind of method of silver nanowires amplification preparation, packet
Include following steps：
(1) polyvinylpyrrolidone (PVP) is dissolved in ethylene glycol, heats 1-2h under stirring, it is molten obtains first
Liquid；The molecular weight of the polyvinylpyrrolidone is selected from 24000,58000 and 1300000；
(2) ferric chloride solution is added dropwise in first solution dropwise, is heated to 100-120 DEG C, obtain the second solution；
The mass ratio of the iron chloride and polyvinylpyrrolidone is 1:(0.5~5)；
(3) ethylene glycol solution of silver nitrate is added drop-wise to dropwise in second solution, is stirred under 200-400rpm revolving speed
2-5min is mixed, after being sufficiently mixed uniformly, closing is stirred, sustained response 15h-17h, and after refrigerated separation, washing obtains silver nanoparticle
Line.
As a further preference, in the step 1), the revolving speed of the stirring is 200-400rpm.
As a further preference, in the step 2), the concentration of the iron chloride is 550-650 μm of ol/L.
As a further preference, described to be heated to 115 DEG C in the step 2).
As a further preference, in the step 2), the mass ratio of the iron chloride and polyvinylpyrrolidone is 1:
1。
As a further preference, in the step 3), the revolving speed of the stirring is 300rpm.
As a further preference, in the step (3), the washing is washed using deionized water.
Another object of the present invention is to provide the application for the silver nanowires that the above method is prepared, the silver nanowiress
As SERS matrix.
The beneficial effects of the invention are as follows：Whole process step involved by the method for silver nanowires amplification preparation of the present invention
Simply, process conditions are easy to control, and not using especially large-scale or expensive instrument, experiment condition is easy to accomplish, convenient for amplification system
It is standby, thus present invention process is simple, reproducible, mild condition, safety, equipment investment is few, production cost is low, to environment without dirt
The advantages that dye, solar battery, conductive component, the electrode material of supercapacitor, photoelectrocatalysis, in terms of have
There is good application prospect.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of silver nanowires prepared by the embodiment of the present invention 1.
Fig. 2 is the electron microscope for the silver nanowires being prepared after raw material dosage all in embodiment 1 is amplified 2 times.
Fig. 3 is 10-12The R6G of M is adsorbed on the SERS spectra on the silver nanowires matrix of the embodiment of the present invention 1.
Specific embodiment
The present invention solves in existing silver nanowires preparation method by providing a kind of method of silver nanowires amplification preparation
Existing poor repeatability, preparation process are complicated, experiment condition not easy-regulating, it is difficult to the problems such as synthesizing on a large scale.
To solve the above-mentioned problems, the main thought of the embodiment of the present invention is：
A kind of method of silver nanowires amplification preparation, includes the following steps：
(1) polyvinylpyrrolidone (PVP) is dissolved in ethylene glycol, heats 1-2h under stirring, it is molten obtains first
Liquid；The molecular weight of the polyvinylpyrrolidone is selected from 24000,58000 and 1300000；
(2) ferric chloride solution is added dropwise in first solution dropwise, is heated to 100-120 DEG C, obtain the second solution；
The mass ratio of the iron chloride and polyvinylpyrrolidone is 1:(0.5~5)；
(3) ethylene glycol solution of silver nitrate is added drop-wise in second solution, stirs 2- under 200-400rpm revolving speed
5min after being sufficiently mixed uniformly, is closed and is stirred, sustained response 15h-17h, and after refrigerated separation, washing obtains silver nanowires.
When above-mentioned evenly dispersed, ultrasonic power or auxiliary mixing plant, such as magnetic stirring apparatus can be used.
Above-mentioned each raw material or agent formulations can be bought by commercially available channel or be prepared by existing method.
Commercially available analytical reagents can be used in reagent PVP, silver nitrate, ethyl alcohol etc. used in embodiment.
Above-mentioned steps 1) in, PVP is sufficiently dissolved, it is otherwise uniform to be conducive to uniform cladding of the PVP in silver nanowires
Property will receive influence, can be realized by way of heating, ultrasound, stirring quickening dissolution.The polyvinylpyrrolidone
Molecular weight is selected from 24000,58000 and 1300000, this molecular weight ranges can be conducive to form line style pattern.
Above-mentioned steps 2) in, reaction temperature is low, is selected as 100~120 DEG C.
Above-mentioned steps 3) in, dropwise addition mode is to be added dropwise dropwise, is conducive to the evenly dispersed of solution, avoids silver-colored crystal seed nucleation poly-
Phenomena such as collecting, silver nanowires accumulation occur causes pattern inhomogenous, guarantees the normal growth of silver-colored crystal seed.
It is washed in above-mentioned steps (3) using deionized water, is not needed purchase etoh solvent, acetone etc., may be implemented
Experimental cost is reduced while environmentally friendly.
In order to which above and other purpose, feature and the advantage of the present invention can be clearer and more comprehensible, several implementations are cited below particularly
Example, to illustrate the method and its application of silver nanowires amplification preparation of the present invention.
Embodiment 1
The method of silver nanowires of embodiment of the present invention amplification preparation, includes the following steps：
1) a certain amount of PVP is dissolved in ethylene glycol, and heats 1h under 300rpm revolving speed magnetic agitation；The polyethylene
The molecular weight of pyrrolidones is 1300000；
2) ferric chloride solution for being 600 μm of ol/L by the concentration of 3.4g, is added dropwise dropwise in above-mentioned steps 1) treated PVP
Ethylene glycol solution in, under the conditions of 115 DEG C, react 1h；
3) ethylene glycol solution of silver nitrate is added drop-wise to step 2) treated in solution, with 300rpm revolving speed magnetic agitation
Uniformly, 4min is stirred, after being sufficiently mixed uniformly, closing is stirred, sustained response 15h, after refrigerated separation, is carried out using deionized water
Washing, obtains silver nanowires.
The AgNWs silver nanowires that above each step obtains is subjected to electron microscope scanning, has obtained Flied emission scanning electricity
Mirror micrograph, as shown in Fig. 1.It can be seen in the drawings that not only pattern is good by the obtained AgNWs of the present invention, size uniformity.?
The silver nanowires of morphology controllable can be still prepared in the raw material dosage of embodiment 1 after amplifying 2-4 times, if Fig. 2 is that embodiment 1 is put
Big 2 times of dosages, the electron microscope for the silver nanowires being prepared, it can be seen that line style is obvious, size uniformity.
Using above-mentioned AgNWs as SERS matrix, select rhodamine 6G and 3MPA as probe molecule to silver nanowires matrix
SERS activity characterized, as shown in figure 3, can detecte the R6G (10 of super low concentration-12Mol/L) spectral signal, this table
It is illustrated and shows good sensitivity using silver nanowires as SERS matrix.Activity is good as the result is shown, and stability is good.
Embodiment 2
The method of silver nanowires of embodiment of the present invention amplification preparation, includes the following steps：
1) a certain amount of PVP is dissolved in ethylene glycol, and heats 2h under 200rpm revolving speed magnetic agitation；The polyethylene
The molecular weight of pyrrolidones is 58000；
2) ferric chloride solution for being 600 μm of ol/L by the concentration of 3.4g, is added dropwise dropwise in above-mentioned steps 1) treated PVP
Ethylene glycol solution in, under the conditions of 100 DEG C, react 2h；
3) ethylene glycol solution of silver nitrate is added drop-wise to step 2) treated in solution, with 200rpm revolving speed magnetic agitation
Uniformly, 5min is stirred, after being sufficiently mixed uniformly, closing is stirred, sustained response 17h, after refrigerated separation, using deionized water and second
Alcohol is washed, and silver nanowires is obtained.
Not only pattern is good by the AgNWs that the present invention obtains, size uniformity.
Above-mentioned AgNWs is subjected to SERS test, its SERS activity is good as the result is shown, and stability is good.
Embodiment 3
The method of silver nanowires of embodiment of the present invention amplification preparation, includes the following steps：
1) a certain amount of PVP is dissolved in ethylene glycol, and heats 1h under 400rpm revolving speed magnetic agitation；The polyethylene
The molecular weight of pyrrolidones is 24000；
2) ferric chloride solution for being 600 μm of ol/L by the concentration of 3.4g, is added dropwise dropwise in above-mentioned steps 1) treated PVP
Ethylene glycol solution in, under the conditions of 120 DEG C, react 1h；
3) ethylene glycol solution of silver nitrate is added drop-wise to step 2) treated in solution, with 400rpm revolving speed magnetic agitation
Uniformly, 3min is stirred, after being sufficiently mixed uniformly, closing is stirred, sustained response 16h, after refrigerated separation, is carried out using deionized water
Washing, obtains silver nanowires.
Not only pattern is good by the AgNWs that the present invention obtains, size uniformity.
Above-mentioned AgNWs is subjected to SERS test, its SERS activity is good as the result is shown, and stability is good.
Embodiment 4
The method of silver nanowires of embodiment of the present invention amplification preparation, includes the following steps：
1) a certain amount of PVP is dissolved in ethylene glycol, and heats 1h under 300rpm revolving speed magnetic agitation；The polyethylene
The molecular weight of pyrrolidones is 58000；
2) ferric chloride solution for being 600 μm of ol/L by the concentration of 3.4g, is added dropwise dropwise in above-mentioned steps 1) treated PVP
Ethylene glycol solution in, under the conditions of 110 DEG C, react 1.5h；
3) ethylene glycol solution of silver nitrate is added drop-wise to step 2) treated in solution, with 350rpm revolving speed magnetic agitation
Uniformly, 2min is stirred, after being sufficiently mixed uniformly, closing is stirred, sustained response 17h, after refrigerated separation, is carried out using deionized water
Washing, obtains silver nanowires.
Not only pattern is good by the AgNWs that the embodiment of the present invention obtains, size uniformity.
Above-mentioned AgNWs is subjected to SERS test, its SERS activity is good as the result is shown, and stability is good.
Embodiment 5
The method of silver nanowires of embodiment of the present invention amplification preparation, includes the following steps：
1) a certain amount of PVP is dissolved in ethylene glycol, and heats 1h under 300rpm revolving speed magnetic agitation；The polyethylene
The molecular weight of pyrrolidones is 1300000；
2) ferric chloride solution for being 550 μm of ol/L by the concentration of 3.8g, is added dropwise dropwise in above-mentioned steps 1) treated PVP
Ethylene glycol solution in, under the conditions of 115 DEG C, react 1h；
3) ethylene glycol solution of silver nitrate is added drop-wise to step 2) treated in solution, with 300rpm revolving speed magnetic agitation
Uniformly, 5min is stirred, after being sufficiently mixed uniformly, closing is stirred, sustained response 16h, after refrigerated separation, is carried out using deionized water
Washing, obtains silver nanowires.
Not only pattern is good by the AgNWs that the embodiment of the present invention obtains, size uniformity.
Above-mentioned AgNWs is subjected to SERS test, its SERS activity is good as the result is shown, and stability is good.
Embodiment 6
The method of silver nanowires of embodiment of the present invention amplification preparation, includes the following steps：
1) a certain amount of PVP is dissolved in ethylene glycol, and heats 2h under 300rpm revolving speed magnetic agitation；The polyethylene
The molecular weight of pyrrolidones is 24000；
2) ferric chloride solution for being 650 μm of ol/L by the concentration of 3.2g, is added dropwise dropwise in above-mentioned steps 1) treated PVP
Ethylene glycol solution in, under the conditions of 105 DEG C, react 1h；
3) ethylene glycol solution of silver nitrate is added drop-wise to step 2) treated in solution, with 300rpm revolving speed magnetic agitation
Uniformly, 3min is stirred, after being sufficiently mixed uniformly, closing is stirred, sustained response 16h, after refrigerated separation, is carried out using deionized water
Washing, obtains silver nanowires.
Not only pattern is good by the AgNWs that the embodiment of the present invention obtains, size uniformity.
Above-mentioned AgNWs is subjected to SERS test, its SERS activity is good as the result is shown, and stability is good.
Technical solution in above-mentioned the embodiment of the present application, at least has the following technical effect that or advantage：
AgNWs morphology controllable prepared by the present invention, reproducible, size uniformity；Present invention process is simple, it is reproducible,
Mild condition, the advantages that safety, equipment investment is few, production cost is low, no pollution to the environment, in solar battery, conductive element device
Part, the electrode material of supercapacitor, photoelectrocatalysis, sensor etc. have a good application prospect.
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects
It is described in detail, it should be understood that being not limited to this hair the foregoing is merely a specific embodiment of the invention
Bright, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the present invention
Protection scope within.
Claims (8)
1. a kind of method of silver nanowires amplification preparation, it is characterised in that：Include the following steps：
(1) polyvinylpyrrolidone is dissolved in ethylene glycol, heats 1-2h under stirring, obtain the first solution；It is described poly-
The molecular weight of vinylpyrrolidone is selected from 24000,58000 and 1300000；
(2) ferric chloride solution is added dropwise in first solution dropwise, is heated to 100-120 DEG C, obtain the second solution；It is described
The mass ratio of iron chloride and polyvinylpyrrolidone is 1:(0.5~5)；
(3) ethylene glycol solution of silver nitrate is added drop-wise to dropwise in second solution, stirs 2- under 200-400rpm revolving speed
5min after being sufficiently mixed uniformly, is closed and is stirred, sustained response 15h-17h, and after refrigerated separation, washing obtains silver nanowires.
2. the method for silver nanowires amplification preparation according to claim 1, it is characterised in that：It is described in the step 1)
The revolving speed of stirring is 200-400rpm.
3. the method for silver nanowires amplification preparation according to claim 1, it is characterised in that：It is described in the step 2)
The concentration of iron chloride is 550-650 μm of ol/L.
4. the method for silver nanowires amplification preparation according to claim 1, it is characterised in that：It is described in the step 2)
It is heated to 115 DEG C.
5. the method for silver nanowires amplification preparation according to claim 1, it is characterised in that：It is described in the step 2)
The mass ratio of iron chloride and polyvinylpyrrolidone is 1:1.
6. the method for silver nanowires amplification preparation according to claim 1, it is characterised in that：It is described in the step 3)
The revolving speed of stirring is 300rpm.
7. the method for silver nanowires amplification preparation according to claim 1, it is characterised in that：It is described in the step (3)
Washing is washed using deionized water.
8. the application for the silver nanowires that the method according to claim 1 to 7 is prepared, it is characterised in that：The silver
Nano wire is used as SERS matrix.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111014715A (en) * | 2019-11-28 | 2020-04-17 | 浙江省科创新材料研究院 | Preparation method of high-yield nano silver wire |
| CN113804669A (en) * | 2021-08-24 | 2021-12-17 | 南通大学 | Preparation method of multi-morphology nano silver substrate |
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| CN104511596A (en) * | 2013-09-30 | 2015-04-15 | 中科院广州化学有限公司 | Continuous preparation method and device for nano-silver wire |
| US20150107412A1 (en) * | 2013-10-21 | 2015-04-23 | Taiwan Textile Research Institute | Preparation method of silver nanowires |
| CN105537622A (en) * | 2016-01-07 | 2016-05-04 | 嘉兴禾浦光电科技有限公司 | Method for preparing silver nanowires |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2009203484A (en) * | 2008-02-26 | 2009-09-10 | Achilles Corp | Method for synthesizing wire-shaped metal particle |
| CN103084584A (en) * | 2013-01-29 | 2013-05-08 | 中国科学院理化技术研究所 | Method of preparing silver nanowire by utilization of hydrothermal method |
| CN104511596A (en) * | 2013-09-30 | 2015-04-15 | 中科院广州化学有限公司 | Continuous preparation method and device for nano-silver wire |
| US20150107412A1 (en) * | 2013-10-21 | 2015-04-23 | Taiwan Textile Research Institute | Preparation method of silver nanowires |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111014715A (en) * | 2019-11-28 | 2020-04-17 | 浙江省科创新材料研究院 | Preparation method of high-yield nano silver wire |
| CN113804669A (en) * | 2021-08-24 | 2021-12-17 | 南通大学 | Preparation method of multi-morphology nano silver substrate |
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Application publication date: 20181130 |