CN106694899B - A kind of preparation method of the controllable silver nanoparticle spool of size - Google Patents
A kind of preparation method of the controllable silver nanoparticle spool of size Download PDFInfo
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- CN106694899B CN106694899B CN201611021491.3A CN201611021491A CN106694899B CN 106694899 B CN106694899 B CN 106694899B CN 201611021491 A CN201611021491 A CN 201611021491A CN 106694899 B CN106694899 B CN 106694899B
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Abstract
The present invention relates to a kind of preparation methods of the controllable silver nanoparticle spool of size, belong to technical field of nanometer material preparation, the preparation method is only using silver as crystal seed, using small molecule heterocyclic compound as derivant, silver soluble saline solution is added in small molecule heterocyclic compound aqueous solution, control reactant ratio, the controllable silver nanoparticle spool of draw ratio is obtained by the reaction under low temperature, method is easy to operate, product purity is high, success rate is high, it is reproducible, the material being prepared has high length-diameter ratio, the advantages that size is controllable, available for chemistry and electrochemical catalysis, chemical sensor, bimolecular sensors, optical information stores, printed electronic, electromagnetic shielding, solar cell, the fields such as Touch Screen, in addition inventive formulation is simple, without using the organic solvent and surfactant of pollution, it is environmentally protective.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, are related to a kind of preparation method of the controllable silver nanoparticle spool of size.
Background technology
Silver nano material, especially silver nanoparticle spool have unique optics, electromagnetism, mechanics, catalytic performance, in addition
The tunnel-effect and electron transmission ability that tubular material is had by its special construction so that it has of crucial importance in various fields
Effect and application.The electric conductivity of particularly silver nanoparticle spool is high, flexibility is good, into film uniformity is good, processing and fabricating is simple, energy
In enough transparent conductive films effectively applied in touch-control product, and the transparent electrode in recent years based on silver nanoparticle spool also by
To extensive concern.
At present, the method for synthesis of silver nano-wire mainly has template and wet chemistry synthetic method.Template have hard template and
Two kinds of approach of soft template.Its advantage is can strictly to control the pattern of silver nano material, but its size and pattern are controlled by its institute
Template has higher requirements to template used, the drawback is that template removal processes are complicated, it is difficult to efficiently, simplicity, largely close
Into nano silver wire.Main method currently used for preparing silver nano material is wet chemistry synthetic method.Although wet chemistry synthesizes
Method can effectively prepare nano silver wire, but be directed to the not environment friendly type of subsequent processing complexity during chemical synthesis greatly
The use of organic solvent, and preparation process easily causes environmental problem using more organic and inorganic assistant；Existing method simultaneously
In lack the effective measures regulated and controled on a large scale to nano silver wire draw ratio.And the preparation of silver nanotube then relies primarily on template,
It is less efficient.
Invention content
It is an object of the invention to overcome the drawbacks described above of the prior art, a kind of system of the controllable silver nanoparticle spool of size is provided
Preparation Method, the preparation method is only using silver as crystal seed, using small molecule heterocyclic compound as derivant, reactant ratio is controlled, in low
The controllable silver nanoparticle spool of draw ratio is obtained by the reaction under temperature, method is easy to operate, and product purity is high, and success rate is high, reproducible,
The material being prepared has many advantages, such as high length-diameter ratio, and size is controllable, available for chemistry and electrochemical catalysis, chemical sensor,
The fields such as bimolecular sensors, optical information storage, printed electronic, electromagnetic shielding, solar cell, Touch Screen.
What the above-mentioned purpose of the present invention was mainly achieved by following technical solution：
A kind of preparation method of the controllable silver nanoparticle spool of size, includes the following steps：
(1), by soluble silver salt obtained aqueous solution；
(2), by small molecule heterocyclic compound obtained aqueous solution；
(3), silver soluble saline solution is added in small molecule heterocyclic compound aqueous solution, after being uniformly mixed,
It is positioned in cryogenic freezing environment and is reacted, stand restore temperature of reaction system to room temperature later；
(4), reaction product is centrifuged and washed, organic solvent washing it is multiple, obtained using organic solvent dispersion
To silver nanoparticle spool concentrate, silver nanoparticle spool concentrate is dried in vacuo to obtain silver nanoparticle spool powder later.
In the preparation method of the controllable silver nanoparticle spool of above-mentioned size, the soluble silver salt is silver fluoride AgF, silver nitrate
AgNO3Or silver perchlorate AgClO4；The concentration of aqueous solution of soluble silver salt is 1~20mmol/L.
In the preparation method of the controllable silver nanoparticle spool of above-mentioned size, the small molecule heterocyclic compound be containing there are one or
Two heteroatomic five-membered rings or hexa-atomic ring heterocyclic compound；The concentration of aqueous solution of the small molecule heterocyclic compound for 1~
20mmol/L。
In the preparation method of the controllable silver nanoparticle spool of above-mentioned size, the small molecule heterocyclic compound is melamine,
Pyridine, imidazoles or niacinamide.
In the preparation method of the controllable silver nanoparticle spool of above-mentioned size, the pyridine is aminopyridine or cyanopyridine；Institute
Imidazoles is stated as nitroimidazole.
In the preparation method of the controllable silver nanoparticle spool of above-mentioned size, small molecule is prepared at normal temperatures in the step (2)
The aqueous solution of heterocyclic compound or the aqueous solution that small molecule heterocyclic compound is prepared using heating water bath, wherein heating water bath temperature
Spend the digestion temperature for small molecule heterocyclic compound.
In the preparation method of the controllable silver nanoparticle spool of above-mentioned size, by silver soluble saline solution in the step (3)
Be added in small molecule heterocyclic compound aqueous solution, the time being stirred is 3~5min, agitating mode for magnetic agitation or
Mechanical agitation.
In the preparation method of the controllable silver nanoparticle spool of above-mentioned size, reactant small molecular heterocyclic compound and solubility
The molar ratio of silver salt is 10:1~10:10.
In the preparation method of the controllable silver nanoparticle spool of above-mentioned size, in the step (3) in cryogenic freezing environment into
The reaction temperature of row reaction is -40 DEG C~0 DEG C, and the reaction time is 6~18h.
In the preparation method of the controllable silver nanoparticle spool of above-mentioned size, the centrifugal rotational speed of centrifugation in the step (4)
For 6000~10000r/min, the time is 5~20min.
In the preparation method of the controllable silver nanoparticle spool of above-mentioned size, reaction product is washed in the step (4),
Each 3~5 times of organic solvent washing removes the impurity in reaction product, washing organic solvent and dispersion organic solvent
For ethyl alcohol.
In the preparation method of the controllable silver nanoparticle spool of above-mentioned size, vacuum drying temperature is 40 in the step (4)
~80 DEG C, drying time is 4~10h.
The present invention has the advantages that compared with prior art：
(1), preparation method of the present invention is only using silver as crystal seed, using small molecule heterocyclic compound as derivant, controls reactant
Proportioning, is obtained by the reaction the controllable silver nanoparticle spool of draw ratio under low temperature, and method is easy to operate, and product purity is high, and success rate is high,
Reproducible, the material being prepared has many advantages, such as high length-diameter ratio, and size is controllable,
(2), adopt that used composition of raw materials is simple, and price is cheap in preparation method of the present invention, common to be easy to get, product purity
Height, success rate is high, reproducible, and without using the organic solvent (ethyl alcohol is used in the present invention) of pollution (environmentally harmful)
And surfactant, it is environmentally protective.
(3) silver nanoparticle spool prepared by the method for the present invention has many advantages, such as high length-diameter ratio, and size is controllable, available for chemical and
Electrochemical catalysis, chemical sensor, bimolecular sensors, optical information storage, printed electronic, electromagnetic shielding, solar-electricity
The fields such as pond, Touch Screen, have a wide range of application, highly practical.
(4), the present invention by a large number of experiments to nano silver wire control it is standby during raw material component, with when reacting item
Part optimizes, and has advanced optimized preparation process so that and the silver nanoparticle spool of preparation has more excellent performance, and
Product purity is high, and success rate is high, reproducible.
(5) preparation method operating procedure of the present invention is easy, easy to operate, can realize large-scale production.
Description of the drawings
Fig. 1 is the XRD spectrum of nano silver wire in the embodiment of the present invention 1；
Fig. 2 is the SEM scanning electron microscope (SEM) photographs of nano silver wire in the embodiment of the present invention 1, and wherein Fig. 2 a are different amplifications from Fig. 2 b
The SEM scanning electron microscope (SEM) photographs of multiple；
Fig. 3 is the SEM scanning electron microscope (SEM) photographs of silver nanotube in the embodiment of the present invention 2；
Fig. 4 is the SEM scanning electron microscope (SEM) photographs of silver nanotube in the embodiment of the present invention 3.
Specific embodiment
The present invention is described in further detail in the following with reference to the drawings and specific embodiments：
The preparation method of the controllable silver nanoparticle spool of size of the present invention, specifically comprises the following steps：
(1), by soluble silver salt obtained aqueous solution；Soluble silver salt be silver fluoride (AgF), silver nitrate (AgNO3) or it is high
Silver chlorate (AgClO4), the concentration of aqueous solution of soluble silver salt is 1~20mmol/L.
(2), small molecule heterocyclic compound is passed through into heating water bath obtained aqueous solution；Small molecule heterocyclic compound is contains one
A or two heteroatomic five-membered rings or hexa-atomic ring heterocyclic compound, such as melamine, pyridine, imidazoles or niacinamide, wherein
Pyridine is aminopyridine, cyanopyridine etc., and imidazoles is nitroimidazole.Water-bath solution temperature is the digestion of each heterocyclic compound
Temperature (solution temperature i.e. in water), if melamine is 60 DEG C.The concentration of aqueous solution of small molecule heterocyclic compound for 1~
20mmol/L。
(3), the soluble silver salt solution of certain volume is added to the prepared small molecule heterocycle of water-bath of certain volume
It in compound solution, after being uniformly mixed, is transferred in plastic containers, is positioned in cryogenic freezing environment and carries out one section of reaction
After time, take out to stand and restore system temperature to room temperature.It is 3~5min that the time, which is wherein mixed, and agitating mode is according to solution
The size of total volume may be selected magnetic agitation or mechanical agitation, reactant small molecular heterocyclic compound and soluble silver salt
Molar ratio is 10:1~10:10.The reaction temperature of cryogenic freezing is -40~0 DEG C, and the reaction time is 6~18h, ensures reactant
System stands clear-cutting forestland to room temperature generally in icing condition is freezed after low-temp reaction.
(4), reaction product is centrifuged and washed, ethyl alcohol is washed each three times to five times, disperse to obtain using ethyl alcohol
Silver nanoparticle spool concentrate is then dried in vacuo to obtain silver nanoparticle spool powder by silver nanoparticle spool concentrate.
Above-mentioned product separation condition is to be centrifuged at a high speed, and centrifugal rotational speed is 6000~10000r, and the time is 5~20min；
Product is washed in centrifugal process, ethyl alcohol is washed each three to five times, the impurity in removal product；Silver nanoparticle after ethyl alcohol dispersion
Spool concentrate is dried in vacuo to obtain silver nanoparticle spool powder；Vacuum drying temperature is 40~80 DEG C, drying time for 4~
10h。
Embodiment 1
Silver nitrate 0.4246g is taken to prepare its aqueous solution 250mL first；Take melamine 0.124g, at 60 DEG C water-bath add
Heat prepares its aqueous solution 100mL；Then the silver nitrate solution of 50mL is added to the prepared melamine solution of 100mL water-baths
In so that the molar ratio of reactant melamine and silver nitrate is 10:5, magnetic agitation 5min after mixing, are transferred to modeling
It in material container, is positioned over after carrying out reaction 10h in -20 DEG C of cryogenic freezing environment, takes out and stand clear-cutting forestland system temperature to room
Temperature；Then reaction product is centrifuged and washed, ethyl alcohol washs each five times, centrifugal condition 8000r, 20min, use
Ethyl alcohol disperses to obtain silver nanoparticle spool contracting liquid, is finally dried in vacuo silver nanoparticle spool concentrate to obtain silver nanoparticle spool powder
Body, vacuum drying temperature are 60 DEG C, drying time 10h.
XRD spectrum for nano silver wire in the embodiment of the present invention 1 as shown in Figure 1；Fig. 2 is that silver is received in the embodiment of the present invention 1
The SEM scanning electron microscope (SEM) photographs of rice noodles, wherein Fig. 2 a and the SEM scanning electron microscope (SEM) photographs that Fig. 2 b are different magnification ratios；It can be with by XRD spectrum
Find out, prepared silver nanoparticle spool characteristic peak is fairly obvious, and miscellaneous peak is seldom, and product purity is higher.Prepared silver nanoparticle spool
Yield is average more than 60%.It can be seen that prepared nano silver wire pipe size is controllable by SEM pictures, draw ratio is controllable, size
Uniformity is preferable.
Embodiment 2
Silver fluoride 0.0634g is taken to prepare its aqueous solution 500mL first；3- aminopyridine 0.0941g are taken, are prepared under room temperature
Its aqueous solution 100mL；Then the silver fluoride aqueous solution of 100mL is added in the prepared 3- aminopyridine solutions of 100mL, made
The molar ratio for obtaining reactant 3- aminopyridines and silver fluoride is 10:1, magnetic agitation 3min after mixing, are transferred to plastics appearance
It in device, is positioned over after carrying out reaction 18h in -20 DEG C of cryogenic freezing environment, takes out and stand clear-cutting forestland system temperature to room temperature；It connects
Reaction product is centrifuged and washed, ethyl alcohol washing it is each five times, centrifugal condition 10000r, 5min use ethyl alcohol
Dispersion obtains silver nanoparticle spool contracting liquid, is finally dried in vacuo silver nanoparticle spool concentrate to obtain silver nanoparticle spool powder,
Vacuum drying temperature is 80 DEG C, drying time 6h, is illustrated in figure 3 the SEM scanning electricity of silver nanotube in the embodiment of the present invention 2
Mirror figure.
Embodiment 3
Silver perchlorate 0.1036g is taken to prepare its aqueous solution 500mL first；Niacinamide 0.0122g is taken, it is prepared under room temperature
Aqueous solution 100mL；Then the silver perchlorate aqueous solution of 100mL is added in the prepared nicotinamide solns of 100mL so that anti-
It is 10 to answer the molar ratio of object niacinamide and silver perchlorate:10, magnetic agitation 5min after mixing, are transferred in plastic containers,
It is positioned over after carrying out reaction 6h in -20 DEG C of cryogenic freezing environment, takes out and stand clear-cutting forestland system temperature to room temperature；It then will be anti-
Product is answered to be centrifuged and wash, ethyl alcohol washing it is each five times, centrifugal condition 6000r, 20min are disperseed using ethyl alcohol
To silver nanoparticle spool contracting liquid, finally silver nanoparticle spool concentrate is dried in vacuo to obtain silver nanoparticle spool powder, vacuum is done
Dry temperature is 80 DEG C, drying time 4h.It is illustrated in figure 4 the SEM scanning electron microscope (SEM) photographs of silver nanotube in the embodiment of the present invention 3.
The above, best specific embodiment only of the invention, but protection scope of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, the change or replacement that can be readily occurred in,
It should be covered by the protection scope of the present invention.
The content not being described in detail in description of the invention belongs to the known technology of professional and technical personnel in the field.
Claims (12)
1. a kind of preparation method of the controllable silver nanoparticle spool of size, it is characterised in that：Include the following steps：
(1), by soluble silver salt obtained aqueous solution；
(2), by small molecule heterocyclic compound obtained aqueous solution；
(3), silver soluble saline solution is added in small molecule heterocyclic compound aqueous solution, after being uniformly mixed, placed
It is reacted in cryogenic freezing environment, stands restore temperature of reaction system to room temperature later；
(4), reaction product is centrifuged and washed, organic solvent washing it is multiple, obtain silver using organic solvent dispersion
Silver nanoparticle spool concentrate, is dried in vacuo to obtain silver nanoparticle spool powder later by nanometer spool concentrate.
2. a kind of preparation method of the controllable silver nanoparticle spool of size according to claim 1, it is characterised in that：It is described solvable
Property silver salt be silver fluoride AgF, silver nitrate AgNO3Or silver perchlorate AgClO4；The concentration of aqueous solution of soluble silver salt for 1~
20mmol/L。
3. a kind of preparation method of the controllable silver nanoparticle spool of size according to claim 1, it is characterised in that：Described small point
Sub- heterocyclic compound is contains one or two heteroatomic five-membered ring or hexa-atomic ring heterocyclic compound；The small molecule jeterocyclic chemistry
The concentration of aqueous solution for closing object is 1~20mmol/L.
4. a kind of preparation method of the controllable silver nanoparticle spool of size according to claim 3, it is characterised in that：Described small point
Sub- heterocyclic compound is melamine, pyridine, imidazoles or niacinamide.
5. a kind of preparation method of the controllable silver nanoparticle spool of size according to claim 4, it is characterised in that：The pyridine
For aminopyridine or cyanopyridine；The imidazoles is nitroimidazole.
6. a kind of preparation method of the controllable silver nanoparticle spool of size according to one of Claims 1 to 5, it is characterised in that：
The aqueous solution of small molecule heterocyclic compound or miscellaneous using heating water bath preparation small molecule is prepared in the step (2) at normal temperatures
The aqueous solution of cycle compound, wherein water bath heating temperature are the digestion temperature of small molecule heterocyclic compound.
7. a kind of preparation method of the controllable silver nanoparticle spool of size according to one of Claims 1 to 5, it is characterised in that：
Silver soluble saline solution is added in small molecule heterocyclic compound aqueous solution in the step (3), the time being stirred
For 3~5min, agitating mode is magnetic agitation or mechanical agitation.
8. a kind of preparation method of the controllable silver nanoparticle spool of size according to one of Claims 1 to 5, it is characterised in that：
The molar ratio of reactant small molecular heterocyclic compound and soluble silver salt is 10:1~10:10.
9. a kind of preparation method of the controllable silver nanoparticle spool of size according to one of Claims 1 to 5, it is characterised in that：
The reaction temperature reacted in cryogenic freezing environment in the step (3) is -40 DEG C~0 DEG C, and the reaction time is 6~18h.
10. a kind of preparation method of the controllable silver nanoparticle spool of size according to one of Claims 1 to 5, it is characterised in that：
The centrifugal rotational speed centrifuged in the step (4) is 6000~10000r/min, and the time is 5~20min.
11. a kind of preparation method of the controllable silver nanoparticle spool of size according to one of Claims 1 to 5, it is characterised in that：
Reaction product is washed in the step (4), each 3~5 times of organic solvent washing, remove the impurity in reaction product, institute
It is ethyl alcohol that washing organic solvent and dispersion, which are stated, with organic solvent.
12. a kind of preparation method of the controllable silver nanoparticle spool of size according to one of Claims 1 to 5, it is characterised in that：
Vacuum drying temperature is 40~80 DEG C in the step (4), and drying time is 4~10h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424163A (en) * | 2002-12-31 | 2003-06-18 | 中国科学院上海光学精密机械研究所 | Synthesis for mono-crystal silver nano wire |
| CN102699341A (en) * | 2012-04-26 | 2012-10-03 | 蔡雄辉 | Wet-chemical preparation method for silver micro/nanowires |
| CN103042225A (en) * | 2012-11-05 | 2013-04-17 | 中科院广州化学有限公司 | Linear nano silver and preparation method and application thereof |
| CN104014805A (en) * | 2014-05-20 | 2014-09-03 | 苏州明动新材料科技有限公司 | Preparing method for silver nanometer wire |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20120126181A1 (en) * | 2010-11-22 | 2012-05-24 | Whitcomb David R | Nanowire preparation methods, compositions, and articles |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424163A (en) * | 2002-12-31 | 2003-06-18 | 中国科学院上海光学精密机械研究所 | Synthesis for mono-crystal silver nano wire |
| CN102699341A (en) * | 2012-04-26 | 2012-10-03 | 蔡雄辉 | Wet-chemical preparation method for silver micro/nanowires |
| CN103042225A (en) * | 2012-11-05 | 2013-04-17 | 中科院广州化学有限公司 | Linear nano silver and preparation method and application thereof |
| CN104014805A (en) * | 2014-05-20 | 2014-09-03 | 苏州明动新材料科技有限公司 | Preparing method for silver nanometer wire |
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