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 PDF

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CN110355359A
CN110355359A CN201910735167.5A CN201910735167A CN110355359A CN 110355359 A CN110355359 A CN 110355359A CN 201910735167 A CN201910735167 A CN 201910735167A CN 110355359 A CN110355359 A CN 110355359A
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ethylene glycol
solution
ultra
pvp
silver nanowires
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陈微微
魏葳
李宇
黄林泉
闫国栋
田占元
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Shaanxi Coal and Chemical Technology Institute Co Ltd
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Shaanxi Coal and Chemical Technology Institute Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • B22F1/0547Nanofibres or nanotubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07Metallic powder characterised by particles having a nanoscale microstructure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

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

A kind of ultra-fine silver nanowires and preparation method thereof
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.
CN201910735167.5A 2019-08-09 2019-08-09 A kind of ultra-fine silver nanowires and preparation method thereof Pending CN110355359A (en)

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CN112809014A (en) * 2020-12-29 2021-05-18 深圳市华科创智技术有限公司 Preparation method of nano silver wire
CN113732300A (en) * 2021-08-31 2021-12-03 中硕实业(上海)有限公司 Silver nanowire containing polyphenol compound and preparation method and application thereof
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CN105874889A (en) * 2013-11-22 2016-08-17 C3奈米有限公司 Transparent conductive coatings based on metal nanowires and polymer binders, solution processing thereof, and patterning approaches
CN104313687A (en) * 2014-07-16 2015-01-28 浙江坦福纳米科技有限公司 Preparation technology of silver nanowires with small diameter and high length-diameter ratio
CN109475943A (en) * 2016-06-02 2019-03-15 加利福尼亚大学董事会 Superfine metal nano wire is synthesized with organic free radical
CN109465440A (en) * 2018-11-08 2019-03-15 陕西煤业化工技术研究院有限责任公司 A method of it is separated for silver nanowires length
CN109261983A (en) * 2018-11-22 2019-01-25 韩金玲 A kind of preparation method of ultra-fine high length-diameter ratio silver nanowires
CN109434132A (en) * 2018-12-07 2019-03-08 陕西煤业化工技术研究院有限责任公司 A method of purifying ultra-fine silver nanowires
CN109622984A (en) * 2018-12-07 2019-04-16 陕西煤业化工技术研究院有限责任公司 A kind of preparation method of ultrapure ultra-fine silver nanowires

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CN112705725A (en) * 2020-12-17 2021-04-27 紫金矿业集团股份有限公司 Method for synthesizing superfine silver nanowires by utilizing low-temperature nucleation
CN112809014A (en) * 2020-12-29 2021-05-18 深圳市华科创智技术有限公司 Preparation method of nano silver wire
CN113732300A (en) * 2021-08-31 2021-12-03 中硕实业(上海)有限公司 Silver nanowire containing polyphenol compound and preparation method and application thereof
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
CN113732300B (en) * 2021-08-31 2023-10-17 中硕实业(上海)有限公司 Silver nanowire containing polyphenol compound and preparation method and application thereof
CN113732299B (en) * 2021-08-31 2024-03-26 中硕实业(上海)有限公司 Silver nanowire and preparation method and application thereof

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