CN110355359A - A kind of ultra-fine silver nanowires and preparation method thereof - Google Patents
A kind of ultra-fine silver nanowires and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of ultra-fine silver nanowiress and preparation method thereof.Based on the method for typical polyalcohol synthesis of silver nano-wire, introduce a kind of organic reducing agent with stronger reducing power, the a- hydroxybenzyl radical reduction silver ion generated by it, accelerate the rate of reduction of reaction, and it can be such that the reduction process of silver ion carries out at a lower reaction temperature, to inhibit the cross growth of silver nanowires.Auxiliary agent sodium bromide is added during simultaneous reactions, effective control line Diameter growth enables silver nanowires to grow thinner.This method does not need condition of high voltage, easy to operate, and prepared silver nanowires is averaged line footpath 13nm or so, and draw ratio is greater than 1000.
Description
Technical field
The invention belongs to nano materials to synthesize field, be related to the synthesis more particularly to a kind of ultra-fine silver of a kind of silver nanowires
Nano wire and preparation method thereof.
Background technique
Silver nanowires transparent conductive film compared with traditional ito thin film because having had both low cost manufacturing, square resistance and can
The features such as light-exposed transmitance has excellent performance, is easily achieved flexibility, touch-control is sensitive, so by domestic and international academia and industrial circle
Extensive concern.Silver nanowires transparent conductive film be by it is a kind of can the colloid of liquid phase coating be coated on flexible parent metal and prepare
It forms, and this colloid is then to be deployed into solution by silver nanowires solid to obtain, therefore preparing silver nanowires material is to prepare
The committed step of film, the in recent years preparation of silver nanowires are always the hot spot of industry research.The length of silver nanowires, diameter are
An important factor for influencing the performances such as square resistance, transmission, the mist degree of silver nanowires film.The diameter of silver nanowires and its film
Mist degree is directly proportional, and draw ratio is with overlapped that the quantity of line is relevant, the number of the tie point of the bigger film middle line of draw ratio and line
Amount is fewer, reduces contact resistance.Silver wire length is longer, and line footpath is thinner, and draw ratio is bigger, the photoelectric properties of transparent conductive film
Better.However the minimum general about 20nm of the silver nanowires diameter prepared using polyalcohol synthetic method most of at present, under this diameter
The silver wire a little higher than ITO of Film Haze value, therefore haze value is lower, the better silver nanowires film of photoelectric properties in order to prepare,
Need to synthesize the smaller silver nanowires of diameter.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of ultra-fine silver nanowires and preparation method thereof, preparation
Silver nanowires diameter it is smaller.
The present invention is to be achieved through the following technical solutions:
A kind of preparation method of ultra-fine silver nanowires, comprising the following steps:
Step 1, PVP, potassium bromide and silver nitrate are dissolved in ethylene glycol, are uniformly mixed, obtain mixed solution A;
Step 2, organic reducing agent A is added into mixed solution A, is uniformly mixed, obtains mixed solution B, be passed through nitrogen
Under conditions of mixed solution B is warming up to reaction temperature, then stop being passed through nitrogen, react under confined conditions, after the reaction was completed
By reaction solution quenching, ultra-fine silver nanowires magma is obtained;Wherein, organic reducing agent A is that can generate Alpha-hydroxy benzyl radicals
Compound.
Preferably, step 1 specifically: prepare the ethylene glycol solution of PVP, the ethylene glycol solution and silver nitrate of potassium bromide respectively
Ethylene glycol solution;The ethylene glycol solution of PVP is mixed with the ethylene glycol solution of silver nitrate, stirs, is then added dropwise to potassium bromide
Ethylene glycol solution, stirring, obtain mixed solution A.
Further, the ethylene glycol solution of PVP is prepared specifically: PVP is added in glycol, heating stirring dissolution;It prepares
The ethylene glycol solution of potassium bromide specifically: potassium bromide is added in ethylene glycol, heating stirring dissolution;Prepare the ethylene glycol of silver nitrate
Solution specifically: silver nitrate is added in ethylene glycol, is placed in ultrasound condition, is made it completely dissolved under ice bath.
Further, the concentration of PVP is 0.005-0.01g/mL in the ethylene glycol solution of PVP, and the ethylene glycol of potassium bromide is molten
The concentration of potassium bromide is 0.01-0.030g/mL in liquid, and the concentration of silver nitrate is 0.01- in the ethylene glycol solution of silver nitrate
0.05g/mL;The volume ratio of the ethylene glycol solution of the ethylene glycol solution of silver nitrate, the ethylene glycol solution of PVP and potassium bromide is 1:
(2-6): (0.03-0.3).
Preferably, organic reducing agent A be styrax, 4,4 '-dimethoxy styraxes, 4,4 '-dimethyl styraxes, 4,
4 '-diamino styraxes and 4, at least one of 4 '-dichloro styraxes.
Preferably, in step 2, reaction temperature is 140-170 DEG C, reaction time 60-120min.
Preferably, in step 2, mixed solution B, which is warming up to reaction temperature, under conditions of being passed through nitrogen is specifically: being passed through
After nitrogen 5-20min, mixed solution B is warming up to 140-170 DEG C, heating-up time 10-30min.
Preferably, the mass ratio of PVP, potassium bromide, silver nitrate and organic reducing agent A are 1:(0.05-1): (0.5-5): (5-
15)。
The ultra-fine silver nanowires that the preparation method is prepared.
The ultra-fine silver nanowires, a diameter of 12-14nm.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention in reactant by being added a kind of organic reducing agent that can generate Alpha-hydroxy benzyl radicals, this freedom
Since with uncoupled electron, chemical reactivity is higher on base, Ag is quickly restored by electronics free thereon+, improve
The rate of reduction of reaction inhibits silver wire cross growth;Br simultaneously-Absorption on Ag core surface helps to make by electrostatic equilibrium
With control silver wire line footpath, so that the silver nanowires diameter distribution of preparation is narrower, average line footpath is thinner, reaches 13nm or so, and long
Diameter ratio is greater than 1000.Silver nanowires diameter is thinner, the quantity of the tie point of film middle line and line is advantageously reduced, so as to significant
Improve the photoelectric properties of silver nanowires conductive film.Furthermore preparation method of the present invention is simple, easy to operate, does not need high-pressure section
Part does not need critical conditions.
Further, reaction temperature of the present invention is low, saves energy.
Silver nanowires diameter distribution prepared by the present invention is narrower, and average line footpath is thinner, reaches 13nm or so, and draw ratio is big
In 1000.Silver nanowires diameter is thinner, advantageously reduces the quantity of the tie point of film middle line and line, so as to significantly improve silver
The photoelectric properties of nano wire conductive film.
Detailed description of the invention
Fig. 1 is silver nanowires SEM figure prepared by embodiment 1;
Fig. 2 is silver nanowires SEM figure prepared by embodiment 2;
Fig. 3 is silver nanowires SEM figure prepared by embodiment 3;
Fig. 4 is silver nanowires SEM figure prepared by comparative example 1;
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
A method of ultra-fine silver nanowires being prepared using organic reducing agent, comprising steps of
(1) it prepares the ethylene glycol solution of PVP: weighing PVP and be dissolved in glycol, be placed in stirring and dissolving in heating plate, heating temperature
Degree is 130 DEG C, obtains PVP solution.Wherein the molecular weight of used PVP is between 55000~1300000, the solution of preparation
Concentration is 0.005-0.01g/mL.
(2) prepare the ethylene glycol solution of sodium bromide: the potassium bromide for weighing certain mass is dissolved in ethylene glycol, is placed in heating plate
On dissolved in 130 DEG C, concentration 0.01-0.030g/mL obtains potassium bromide solution.
(3) AgNO is prepared3Ethylene glycol solution: weigh a certain amount of pretreated silver nitrate and be dissolved in ethylene glycol, be placed in
In ultrasound, dissolves in 5-10min, make it completely dissolved, concentration 0.01-0.05g/mL obtains silver nitrate solution under ice bath.
(4) the PVP solution that step (1) is configured is mixed with the silver nitrate solution that step (3) is configured, revolving speed 500r/
5-20min is stirred under min, is then added dropwise to potassium bromide solution, is stirred 20-50min under revolving speed 1000r/min, obtains mixing molten
Liquid A.Wherein the volume ratio of silver nitrate solution, PVP solution and potassium bromide solution is 1:(2-6): (0.03-0.3);Potassium bromide drop
Acceleration is 0.05-0.3mL/s;Mixed solution temperature is kept for 20-40 DEG C.
(5) organic reducing agent A is added in mixed solution A, wherein the mass ratio of A and potassium bromide, silver nitrate, PVP are (5-
15): (0.05-1): (0.5-5): 1.Stop after 1500r/min stirring 2-10min, obtains mixed solution B, be passed through nitrogen 5-
After 20min, mixed solution B progress oil bath heating is warming up to 140-170 DEG C, heating-up time 10-30min, nitrogen flow 100-
300mL/min.Wherein organic reducing agent A is a kind of compound that can generate a- hydroxybenzyl free radical, including styrax, 4,
4 '-dimethoxy styraxes, 4,4 '-dimethyl styraxes, 4,4 '-diamino styraxes and 4, in 4 '-dichloro styraxes at least
It is a kind of.
(6) after being warming up to set temperature, stop ventilation, closed reactor stands reaction 60-120min, reaction solution is quenched
It is cold, obtain ultra-fine silver nanowires magma.
Embodiment 1
(1) it configures the ethylene glycol solution of PVP: weighing PVP and be dissolved in glycol, be placed in stirring and dissolving in heating plate, heating temperature
Degree is 130 DEG C, and the solution concentration of preparation is 0.007g/mL.Wherein the molecular weight of used PVP 55000~1300000 it
Between.
(2) prepare the ethylene glycol solution of potassium bromide: the potassium bromide for weighing certain mass is dissolved in ethylene glycol, is placed in heating plate
On in 130 DEG C dissolve, concentration 0.02g/mL.
(3) AgNO is prepared3Ethylene glycol solution: weigh a certain amount of pretreated silver nitrate and be dissolved in ethylene glycol, be placed in
In ultrasound, dissolves in 5min, make it completely dissolved, concentration 0.02g/mL under ice bath.
(4) the PVP solution that step (1) is configured is mixed with the silver nitrate solution that step (3) is configured, revolving speed 500r/
5min is stirred under min, is then added dropwise to potassium bromide, is stirred 30min under revolving speed 1000r/min.Wherein silver nitrate solution and PVP are molten
The volume of liquid is respectively 45mL and 145mL, and potassium bromide volume is 4.5mL, rate of addition 0.15mL/s, mixed solution temperature guarantor
Hold 25 DEG C.
(5) after stirring, organic reducing agent A 0.05mol is added, stops after 1500r/min stirring 2min, is passed through nitrogen
After gas 10min, mixed solution progress oil bath heating is warming up to 155 DEG C, heating-up time about 18min, nitrogen flow 200mL/
min.Wherein organic reducing agent A is styrax.
(6) after being warming up to set temperature, stop ventilation, closed reactor stands reaction 60min and obtains reaction solution quenching
To ultra-fine silver nanowires magma.
The obtained silver nanowires average diameter of the present embodiment is 12.45nm, average length 14.05um, and draw ratio is
1129, silver nanowires morphology characterization figure SEM is shown in Fig. 1.
Embodiment 2
(1) it configures the ethylene glycol solution of PVP: weighing PVP and be dissolved in glycol, be placed in stirring and dissolving in heating plate, heating temperature
Degree is 130 DEG C.Wherein for the molecular weight of used PVP between 55000~1300000, the solution concentration of preparation is 0.005g/
mL。
(2) prepare the ethylene glycol solution of potassium bromide: the potassium bromide for weighing certain mass is dissolved in ethylene glycol, is placed in heating plate
On in 130 DEG C dissolve, concentration 0.01g/mL.
(3) AgNO is prepared3Ethylene glycol solution: weigh a certain amount of pretreated silver nitrate and be dissolved in ethylene glycol, be placed in
In ultrasound, dissolves in 8min, make it completely dissolved, concentration 0.01g/mL under ice bath.
(4) the PVP solution that step (1) is configured is mixed with the silver nitrate solution that step (3) is configured, is added dropwise to immediately
Then potassium bromide improves under revolving speed to 1000r/min and stirs 20min.Wherein the volume of silver nitrate solution and PVP solution is respectively
75mL and 150mL, potassium bromide volume are 2mL, rate of addition 0.05mL/s;Mixed solution temperature is kept for 20 DEG C.
(5) after stirring, organic reducing agent A 0.03mol is added, after being passed through nitrogen 5min, mixed solution is subjected to oil
Bath is heated to 140 DEG C, heating-up time 10min, nitrogen flow 100mL/min.Wherein organic reducing agent A is 4,4 '-diformazans
Base styrax.
(6) after being warming up to set temperature, stop ventilation, closed reactor stands reaction 90min and obtains reaction solution quenching
To ultra-fine silver nanowires magma.
The obtained silver nanowires average diameter of the present embodiment is 12.54nm, average length 13.72um, and draw ratio is
1094, silver nanowires morphology characterization figure SEM is shown in Fig. 2.
Embodiment 3
(1) it configures the ethylene glycol solution of PVP: weighing PVP and be dissolved in glycol, be placed in stirring and dissolving in heating plate, heating temperature
Degree is 130 DEG C.Wherein for the molecular weight of used PVP between 55000~1300000, the solution concentration of preparation is 0.01g/
mL。
(2) prepare the ethylene glycol solution of potassium bromide: the potassium bromide for weighing certain mass is dissolved in ethylene glycol, is placed in heating plate
On in 130 DEG C dissolve, concentration 0.030g/mL.
(3) AgNO is prepared3Ethylene glycol solution: weigh a certain amount of pretreated silver nitrate and be dissolved in ethylene glycol, be placed in
In ultrasound, dissolves in 10min, make it completely dissolved, concentration 0.05g/mL under ice bath.
(4) the PVP solution that step (1) is configured is mixed with the silver nitrate solution that step (3) is configured, revolving speed 500r/
10min is stirred under min, is then added dropwise to potassium bromide, is stirred 50min under revolving speed 1000r/min.Wherein silver nitrate solution and PVP
The volume of solution is 30mL and 180mL,;Potassium bromide volume is 9mL, rate of addition 0.3mL/s;Mixed solution temperature
Kept for 40 DEG C.
(5) after stirring, organic reducing agent A 0.08mol is added, stops after 1500r/min stirring 10min, is passed through nitrogen
After gas 20min, mixed solution progress oil bath heating is warming up to 170 DEG C, heating-up time 30min, nitrogen flow 300mL/min.
Wherein organic reducing agent A is 4,4 '-dimethoxy styraxes.
(6) after being warming up to set temperature, stop ventilation, closed reactor stands reaction 120min and obtains reaction solution quenching
To ultra-fine silver nanowires magma.
The obtained silver nanowires average diameter of the present embodiment is 13.99nm, average length 16.00um, and draw ratio is
1144, silver nanowires morphology characterization figure SEM is shown in Fig. 3.
Comparative example 1 (is added without organic reducing agent A)
(1) it configures the ethylene glycol solution of PVP: weighing PVP and be dissolved in glycol, be placed in stirring and dissolving in heating plate, heating temperature
Degree is 130 DEG C, and the solution concentration of preparation is 0.007g/mL.Wherein the molecular weight of used PVP 55000~1300000 it
Between.
(2) prepare the ethylene glycol solution of potassium bromide: the potassium bromide for weighing certain mass is dissolved in ethylene glycol, is placed in heating plate
On in 130 DEG C dissolve, concentration 0.02g/mL.
(3) AgNO is prepared3Ethylene glycol solution: weigh a certain amount of pretreated silver nitrate and be dissolved in ethylene glycol, be placed in
In ultrasound, dissolves in 5min, make it completely dissolved, concentration 0.02g/mL under ice bath.
(4) the PVP solution that step (1) is configured is mixed with the silver nitrate solution that step (3) is configured, revolving speed 500r/
5min is stirred under min, is then added dropwise to potassium bromide, is stirred 30min under revolving speed 1000r/min.Wherein silver nitrate solution and PVP are molten
The volume of liquid is respectively 45mL and 145mL, and potassium bromide volume is 4.5mL, rate of addition 0.15mL/s, mixed solution temperature guarantor
Hold 25 DEG C.
(5) after stirring, after being passed through nitrogen 10min, mixed solution progress oil bath heating is warming up to 150 DEG C, heating
Time about 18min, nitrogen flow 200mL/min.
(6) after being warming up to set temperature, stop ventilation, closed reactor stands reaction 60min and obtains reaction solution quenching
To silver nanowires magma.
This comparative example is not add silver nanowires magma prepared under organic reducing agent, be can be seen by Electronic Speculum phenogram
Obtained under lower temperature is all substantially particle and tubbiness stick, does not obtain ultra-fine silver nanowires, magma morphology characterization figure SEM is shown in
Fig. 4.
Embodiment 4
(1) it configures the ethylene glycol solution of PVP: weighing PVP and be dissolved in glycol, be placed in stirring and dissolving in heating plate, heating temperature
Degree is 130 DEG C.Wherein for the molecular weight of used PVP between 55000~1300000, the solution concentration of preparation is 0.008g/
mL。
(2) prepare the ethylene glycol solution of potassium bromide: the potassium bromide for weighing certain mass is dissolved in ethylene glycol, is placed in heating plate
On in 130 DEG C dissolve, concentration 0.020g/mL.
(3) AgNO is prepared3Ethylene glycol solution: weigh a certain amount of pretreated silver nitrate and be dissolved in ethylene glycol, be placed in
In ultrasound, dissolves in 8min, make it completely dissolved, concentration 0.035g/mL under ice bath.
(4) the PVP solution that step (1) is configured is mixed with the silver nitrate solution that step (3) is configured, revolving speed 500r/
5min is stirred under min, is then added dropwise to potassium bromide, is stirred 25min under revolving speed 1000r/min.Wherein silver nitrate solution and PVP are molten
The volume of liquid is respectively 35mL and 165mL;Potassium bromide volume is 4mL, rate of addition 0.16mL/s;Mixed solution temperature is kept
35℃。
(5) after stirring, organic reducing agent A 0.05mol is added, stops after 1500r/min stirring 1min, is passed through nitrogen
After gas 7min, mixed solution progress oil bath heating is warming up to 150 DEG C, heating-up time 20min, nitrogen flow 150mL/min.Its
Middle organic reducing agent A is 4,4 '-diamino styraxes.
(6) after being warming up to set temperature, stop ventilation, closed reactor stands reaction 80min and obtains reaction solution quenching
To ultra-fine silver nanowires magma.
Embodiment 5
(1) it configures the ethylene glycol solution of PVP: weighing PVP and be dissolved in glycol, be placed in stirring and dissolving in heating plate, heating temperature
Degree is 130 DEG C.Wherein for the molecular weight of used PVP between 55000~1300000, the solution concentration of preparation is 0.008g/
mL。
(2) prepare the ethylene glycol solution of potassium bromide: the potassium bromide for weighing certain mass is dissolved in ethylene glycol, is placed in heating plate
On in 130 DEG C dissolve, concentration 0.020g/mL.
(3) AgNO is prepared3Ethylene glycol solution: weigh a certain amount of pretreated silver nitrate and be dissolved in ethylene glycol, be placed in
In ultrasound, dissolves in 8min, make it completely dissolved, concentration 0.035g/mL under ice bath.
(4) the PVP solution that step (1) is configured is mixed with the silver nitrate solution that step (3) is configured, revolving speed 500r/
5min is stirred under min, is then added dropwise to potassium bromide, is stirred 25min under revolving speed 1000r/min.Wherein silver nitrate solution and PVP are molten
The volume of liquid is respectively 35mL and 165mL;Potassium bromide volume is 4mL, rate of addition 0.16mL/s;Mixed solution temperature is kept
35℃。
(5) after stirring, organic reducing agent A 0.05mol is added, stops after 1500r/min stirring 1min, is passed through nitrogen
After gas 7min, mixed solution progress oil bath heating is warming up to 150 DEG C, heating-up time 20min, nitrogen flow 150mL/min.Its
Middle organic reducing agent A is 4,4 '-dichloro styraxes.
(6) after being warming up to set temperature, stop ventilation, closed reactor stands reaction 80min and obtains reaction solution quenching
To ultra-fine silver nanowires magma.
Claims (10)
1. a kind of preparation method of ultra-fine silver nanowires, which comprises the following steps:
Step 1, PVP, potassium bromide and silver nitrate are dissolved in ethylene glycol, are uniformly mixed, obtain mixed solution A;
Step 2, organic reducing agent A is added into mixed solution A, is uniformly mixed, mixed solution B is obtained, in the item for being passed through nitrogen
Mixed solution B is warming up to reaction temperature under part, then stops being passed through nitrogen, react under confined conditions, it after the reaction was completed will be anti-
Liquid quenching is answered, ultra-fine silver nanowires magma is obtained;Wherein, organic reducing agent A is the chemical combination that can generate Alpha-hydroxy benzyl radicals
Object.
2. the preparation method of ultra-fine silver nanowires according to claim 1, which is characterized in that step 1 specifically: match respectively
The ethylene glycol solution of the ethylene glycol solution of PVP processed, the ethylene glycol solution of potassium bromide and silver nitrate;By the ethylene glycol solution of PVP with
The ethylene glycol solution of silver nitrate mixes, then stirring is added dropwise to the ethylene glycol solution of potassium bromide, stirs, obtains mixed solution A.
3. the preparation method of ultra-fine silver nanowires according to claim 2, which is characterized in that the ethylene glycol for preparing PVP is molten
Liquid specifically: PVP is added in glycol, heating stirring dissolution;Prepare the ethylene glycol solution of potassium bromide specifically: by potassium bromide plus
Enter in ethylene glycol, heating stirring dissolution;Prepare the ethylene glycol solution of silver nitrate specifically: silver nitrate is added in ethylene glycol, sets
In ultrasound condition, made it completely dissolved under ice bath.
4. the preparation method of ultra-fine silver nanowires according to claim 2, which is characterized in that in the ethylene glycol solution of PVP
The concentration of PVP is 0.005-0.01g/mL, and the concentration of potassium bromide is 0.01-0.030g/mL, nitre in the ethylene glycol solution of potassium bromide
The concentration of silver nitrate is 0.01-0.05g/mL in the ethylene glycol solution of sour silver;The ethylene glycol of the ethylene glycol solution of silver nitrate, PVP
The volume ratio of solution and the ethylene glycol solution of potassium bromide is 1:(2-6): (0.03-0.3).
5. the preparation method of ultra-fine silver nanowires according to claim 1, which is characterized in that organic reducing agent A is to rest in peace
Perfume, 4,4 '-dimethoxy styraxes, 4,4 '-dimethyl styraxes, 4,4 '-diamino styraxes and 4, in 4 '-dichloro styraxes
It is at least one.
6. the preparation method of ultra-fine silver nanowires according to claim 1, which is characterized in that in step 2, reaction temperature is
140-170 DEG C, reaction time 60-120min.
7. the preparation method of ultra-fine silver nanowires according to claim 1, which is characterized in that in step 2, be passed through nitrogen
Under conditions of mixed solution B be warming up to reaction temperature be specifically: after being passed through nitrogen 5-20min, mixed solution B is warming up to
140-170 DEG C, heating-up time 10-30min.
8. the preparation method of ultra-fine silver nanowires according to claim 1, which is characterized in that PVP, potassium bromide, silver nitrate
Mass ratio with organic reducing agent A is 1:(0.05-1): (0.5-5): (5-15).
9. the ultra-fine silver nanowires that the described in any item preparation methods of claim 1-8 are prepared.
10. ultra-fine silver nanowires according to claim 9, which is characterized in that a diameter of 12-14nm.
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CN113732299A (en) * | 2021-08-31 | 2021-12-03 | 中硕实业(上海)有限公司 | Silver nanowire and preparation method and application thereof |
CN116213707A (en) * | 2023-04-17 | 2023-06-06 | 吉林大学 | Preparation method of ultrahigh-yield silver nanowires |
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