CN106694899A - Preparing method for silver nano wire pipe with controllable size - Google Patents
Preparing method for silver nano wire pipe with controllable size Download PDFInfo
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- CN106694899A CN106694899A CN201611021491.3A CN201611021491A CN106694899A CN 106694899 A CN106694899 A CN 106694899A CN 201611021491 A CN201611021491 A CN 201611021491A CN 106694899 A CN106694899 A CN 106694899A
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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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Abstract
The invention relates to a preparing method for a silver nano wire pipe with the controllable size. According to the preparing method, only silver is adopted as a seed crystal, a micromolecule heterocyclic compound is adopted as an inducing agent, the reactant matching is controlled, and the silver nano wire pipe with the controllable length-diameter ratio is obtained through the reaction at the low temperature. According to the method, operation is simple and convenient, the product purity is high, the success rate is high, and repeatability is high. A material obtained through preparing has the beneficial effects that the length-diameter ratio is high, and the size is controllable and can be applied to the fields of chemical and electrochemical catalysis, chemical sensors, biomolecule sensors, optical information storage, printing electronics, electromagnetic shielding, solar batteries, touch control screens and the like. In addition, in the preparing method, the formula is simple, a contaminative organic solvent and a contaminative surface active agent are not used, and environment friendliness is achieved.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, it is related to a kind of preparation method of the controllable silver nanoparticle spool of size.
Background technology
Silver nano material, especially silver nanoparticle spool, optics, electromagnetism, mechanics, catalytic performance with uniqueness, in addition
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, pliability 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 transparency electrode based on silver nanoparticle spool is also received in recent years
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 can be the pattern of strict control silver nano material, but its size and pattern are controlled by its institute
Template, has higher requirements to template used, and it has the disadvantage that template removal processes are complicated, it is difficult to efficient, easy, substantial amounts of conjunction
Into nano silver wire.It is wet chemistry synthetic method currently used for the main method for preparing silver nano material.Although wet chemistry synthesizes
Method can effectively prepare nano silver wire, but be directed to the complicated not environment friendly type of subsequent treatment during chemical synthesis greatly
The use of organic solvent, and preparation process uses more organic and inorganic assistant, easily causes environmental problem；While existing method
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.
The content of the invention
A kind of drawbacks described above it is an object of the invention to overcome prior art, there is provided system of the controllable silver nanoparticle spool of size
Preparation Method, the preparation method, with small molecule heterocyclic compound as derivant, controls reactant ratio, in low only with silver as crystal seed
The lower reaction of temperature obtains the controllable silver nanoparticle spool of draw ratio, and method is easy to operate, and product purity is high, and success rate is high, reproducible,
The material for preparing has high length-diameter ratio, the advantages of size is controllable, can be used 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 above-mentioned purpose of the invention was mainly achieved by following technical solution：
A kind of preparation method of the controllable silver nanoparticle spool of size, comprises 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 the small molecule heterocyclic compound aqueous solution, after being uniformly mixed,
It is positioned in cryogenic freezing environment and is reacted, stands recover temperature of reaction system to room temperature afterwards；
(4), by product be centrifuged and wash, organic solvent washing repeatedly, obtained using organic solvent dispersion
To silver nanoparticle spool concentrate, afterwards silver nanoparticle spool concentrate be vacuum dried and obtain silver nanoparticle spool powder.
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 one or
Two heteroatomic five-membered rings or hexa-atomic ring heterocyclic compound；The concentration of aqueous solution of the small molecule heterocyclic compound be 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 for 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 using heating water bath preparation small molecule heterocyclic compound, 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 the small molecule heterocyclic compound aqueous solution, stir mixing time be 3~5min, agitating mode be 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 mol ratio of silver salt is 10:1~10:10.
In the preparation method of the controllable silver nanoparticle spool of above-mentioned size, enter in cryogenic freezing environment in the step (3)
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)
It is 6000~10000r/min, the time is 5~20min.
In the preparation method of the controllable silver nanoparticle spool of above-mentioned size, product is washed in the step (4),
Each 3~5 times of organic solvent washing, the impurity in removal product, the washing organic solvent and dispersion organic solvent
It is ethanol.
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, with small molecule heterocyclic compound as derivant, controls reactant only with silver as crystal seed
Proportioning, the controllable silver nanoparticle spool of draw ratio is obtained in reaction under low temperature, and method is easy to operate, and product purity is high, and success rate is high,
Reproducible, the material for preparing has high length-diameter ratio, the advantages of size is controllable,
(2) used composition of raw materials, is adopted in preparation method of the present invention simple, price is cheap, common to be easy to get, product purity
Height, success rate is high, reproducible, and does not use the organic solvent (using ethanol in the present invention) of contaminative (environmentally harmful)
And surfactant, environmental protection.
(3) nano silver wire pipe prepared by the inventive method has high length-diameter ratio, the advantages of size is controllable, can be used for chemistry 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, practical.
(4), the component of raw material of the present invention by lot of experiments to nano silver wire control during standby, with when reacting bar
Part optimizes design, further optimizes preparation process so that the nano silver wire pipe 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.
Brief 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 with specific embodiment below in conjunction with the accompanying drawings：
The preparation method of the controllable silver nanoparticle spool of size of the present invention, specifically includes following steps：
(1), by soluble silver salt obtained aqueous solution；Soluble silver salt is 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 to contain one
Individual 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), such as melamine are 60 DEG C.The concentration of aqueous solution of small molecule heterocyclic compound be 1~
20mmol/L。
(3) the small molecule heterocycle for, preparing the water-bath that the soluble silver salt solution of certain volume is added to certain volume
In compound solution, after being uniformly mixed, it is transferred in plastic containers, being positioned in cryogenic freezing environment carries out one section of reaction
After time, take out to stand and recover system temperature to room temperature.The time is wherein mixed for 3~5min, agitating mode is according to solution
The size of cumulative volume optional magnetic agitation or mechanical agitation, reactant small molecular heterocyclic compound and soluble silver salt
Mol ratio is 10:1~10:10.The reaction temperature of cryogenic freezing is -40~0 DEG C, and the reaction time is 6~18h, it is ensured that reactant
Generally in freezing icing condition, low-temp reaction stands clear-cutting forestland to room temperature after terminating for system.
(4), by product be centrifuged and wash, ethanol is washed each three times to five times, using ethanol disperse obtain
Silver nanoparticle spool concentrate, silver nanoparticle spool concentrate then be vacuum dried obtain silver nanoparticle spool powder.
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, ethanol is washed each three to five times, the impurity in removal product；Silver nanoparticle after ethanol dispersion
Spool concentrate be vacuum dried and obtains silver nanoparticle spool powder；Vacuum drying temperature be 40~80 DEG C, drying time be 4~
10h。
Embodiment 1
Silver nitrate 0.4246g is taken first prepares its aqueous solution 250mL；Melamine 0.124g is taken, is added in water-bath at 60 DEG C
Heat prepares its aqueous solution 100mL；Then the silver nitrate solution of 50mL is added to the melamine solution that 100mL water-baths are prepared
In so that the mol ratio of reactant melamine and silver nitrate is 10:5, magnetic agitation 5min, after being well mixed, are transferred to modeling
In material container, it is positioned in -20 DEG C of cryogenic freezing environment after carrying out reaction 10h, takes out and stand clear-cutting forestland system temperature to room
Temperature；Then by product be centrifuged and wash, ethanol washing it is each five times, centrifugal condition is 8000r, 20min, is used
Ethanol dispersion obtains silver nanoparticle spool contracting liquid, finally by silver nanoparticle spool concentrate be vacuum dried and obtains silver nanoparticle spool powder
Body, vacuum drying temperature is 60 DEG C, and drying time is 10h.
It is as shown in Figure 1 the XRD spectrum of nano silver wire in the embodiment of the present invention 1；Fig. 2 be the embodiment of the present invention 1 in silver receive
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；Can be with by XRD spectrum
Find out, prepared silver nanoparticle spool characteristic peak is fairly obvious, seldom, product purity is higher for miscellaneous peak.Prepared silver nanoparticle spool
Yield is average more than 60%.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 first prepares its aqueous solution 500mL；3- aminopyridine 0.0941g are taken, in preparation under normal temperature
Its aqueous solution 100mL；Then the silver fluoride aqueous solution of 100mL is added in the 3- aminopyridine solutions that 100mL is prepared, is made
The mol ratio for obtaining reactant 3- aminopyridines and silver fluoride is 10:1, magnetic agitation 3min, after being well mixed, are transferred to plastics appearance
In device, it is positioned in -20 DEG C of cryogenic freezing environment after carrying out reaction 18h, takes out and stand clear-cutting forestland system temperature to room temperature；Connect
By product be centrifuged and wash, ethanol washing it is each five times, centrifugal condition is 10000r, 5min, uses ethanol
Dispersion obtains silver nanoparticle spool contracting liquid, finally by silver nanoparticle spool concentrate be vacuum dried and obtains silver nanoparticle spool powder,
Vacuum drying temperature is 80 DEG C, and drying time is 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 first prepares its aqueous solution 500mL；Niacinamide 0.0122g is taken, in preparing it under normal temperature
Aqueous solution 100mL；Then the silver perchlorate aqueous solution of 100mL is added in the nicotinamide soln that 100mL is prepared so that anti-
The mol ratio for answering thing niacinamide and silver perchlorate is 10:10, magnetic agitation 5min, after being well mixed, are transferred in plastic containers,
It is positioned in -20 DEG C of cryogenic freezing environment after carrying out reaction 6h, takes out and stand clear-cutting forestland system temperature to room temperature；Then will be anti-
Product is answered to be centrifuged and wash, ethanol washs each five times, centrifugal condition is 6000r, 20min, is disperseed using ethanol
To silver nanoparticle spool contracting liquid, finally silver nanoparticle spool concentrate be vacuum dried and obtain silver nanoparticle spool powder, vacuum is done
Dry temperature is 80 DEG C, and drying time is 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, optimal specific embodiment only of the invention, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in,
Should all be included within the 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. the preparation method of the controllable silver nanoparticle spool of a kind of size, it is characterised in that：Comprise 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 the small molecule heterocyclic compound aqueous solution, after being uniformly mixed, is placed
Reacted in cryogenic freezing environment, stand recover temperature of reaction system to room temperature afterwards；
(4), by product be centrifuged and wash, organic solvent washing repeatedly, obtain silver using organic solvent dispersion
Nanometer spool concentrate, silver nanoparticle spool concentrate be vacuum dried obtain silver nanoparticle spool powder afterwards.
2. the preparation method of the controllable silver nanoparticle spool of a kind 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 be 1~
20mmol/L。
3. the preparation method of the controllable silver nanoparticle spool of a kind of size according to claim 1, it is characterised in that：Described small point
Sub- heterocyclic compound is to contain one or two heteroatomic five-membered ring or hexa-atomic ring heterocyclic compound；The small molecule jeterocyclic chemistry
The concentration of aqueous solution of compound is 1~20mmol/L.
4. the preparation method of the controllable silver nanoparticle spool of a kind of size according to claim 3, it is characterised in that：Described small point
Sub- heterocyclic compound is melamine, pyridine, imidazoles or niacinamide.
5. the preparation method of the controllable silver nanoparticle spool of a kind of size according to claim 4, it is characterised in that：The pyridine
It is aminopyridine or cyanopyridine；The imidazoles is nitroimidazole.
6. according to a kind of preparation method of one of Claims 1 to 5 controllable silver nanoparticle spool of described size, 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. according to a kind of preparation method of one of Claims 1 to 5 controllable silver nanoparticle spool of described size, it is characterised in that：
Silver soluble saline solution is added in the small molecule heterocyclic compound aqueous solution in the step (3), stirs the time of mixing
It is 3~5min, agitating mode is magnetic agitation or mechanical agitation.
8. according to a kind of preparation method of one of Claims 1 to 5 controllable silver nanoparticle spool of described size, it is characterised in that：
The mol ratio of reactant small molecular heterocyclic compound and soluble silver salt is 10:1~10:10.
9. according to a kind of preparation method of one of Claims 1 to 5 controllable silver nanoparticle spool of described size, 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. according to a kind of preparation method of one of Claims 1 to 5 controllable silver nanoparticle spool of described size, it is characterised in that：
The centrifugal rotational speed of centrifugation is 6000~10000r/min in the step (4), and the time is 5~20min.
11. according to a kind of preparation method of one of Claims 1 to 5 controllable silver nanoparticle spool of described size, it is characterised in that：
Product is washed in the step (4), each 3~5 times of organic solvent washing, the impurity in removal product, institute
It is ethanol to state washing organic solvent and dispersion organic solvent.
12. according to a kind of preparation method of one of Claims 1 to 5 controllable silver nanoparticle spool of described size, 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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| CN201611021491.3A CN106694899B (en) | 2016-11-15 | 2016-11-15 | A kind of preparation method of the controllable silver nanoparticle spool of size |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113426425A (en) * | 2021-06-21 | 2021-09-24 | 西南科技大学 | Silver-based composite adsorbent for removing radioactive iodine and preparation method and application thereof |
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|---|---|---|---|---|
| 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 |
| US20120126181A1 (en) * | 2010-11-22 | 2012-05-24 | Whitcomb David R | Nanowire preparation methods, compositions, and articles |
| 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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2016
- 2016-11-15 CN CN201611021491.3A patent/CN106694899B/en not_active Expired - Fee Related
Patent Citations (5)
| 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 |
| US20120126181A1 (en) * | 2010-11-22 | 2012-05-24 | Whitcomb David R | Nanowire preparation methods, compositions, and articles |
| 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 |
|---|---|---|---|---|
| CN113426425A (en) * | 2021-06-21 | 2021-09-24 | 西南科技大学 | Silver-based composite adsorbent for removing radioactive iodine and preparation method and application thereof |
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