CN106345997A - Superfine silver nanowires uniform in morphology and preparation method thereof - Google Patents
Superfine silver nanowires uniform in morphology and preparation method thereof Download PDFInfo
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Abstract
Provided are superfine silver nanowires uniform in morphology and a preparation method thereof. A modified polyhydric alcohol method is adopted to prepare silver nanowires with a diameter of 20-40 nm and a length of 20-50 [mu]m. The method comprises the steps of heating a PVP solution to 120-170 DEG C, adding a certain amount of haloid salt and AgNO3, reacting for 0.5 h, adding dropwise an AgNO3 solution with a certain concentration, wherein the dropwise adding time is 0.25-4 h; reacting for 0.5-4 h after the dropwise adding, performing centrifugal separation after the reaction is over, and then dispersing the product in a dispersing agent at a certain concentration. According to the method, different haloid salts and PVP are mixed and used as a control agent and modifier, the temperature rise process and the feeding process are controlled, so that the nucleation size and growth speed of the silver nanowires are effectively controlled, and the superfine silver nanowires which have a diameter lower than 40 nm and are uniform in length and diameter are prepared.
Description
Technical field
The present invention relates to nano material synthesis technical field, the homogeneous ultra-fine nano silver wire of more particularly, to a kind of pattern and its
Preparation method.
Background technology
Nano silver material is got more and more people's extensive concerning for a long time with its unique optics, electricity, thermal property, people
Its preparation method and using value are carried out with substantial amounts of research and has explored, and achieved excellent achievement.In recent years, with section
The development of technology and the raising of people's living standard, transparent conductive film is in solaode, touch panel, LCDs
Demand Deng neck increasingly increases severely.Ito as traditional transparent electrode material, for a long time in occupation of most parts in this market
Volume.But, because it has the shortcomings that matter is crisp, process costs are high, resource is few, people are devoted to developing the transparent of a new generation always
Electrode material, such as Graphene, CNT, metal grill, nano silver wire etc..Wherein nano silver wire is due to its excellent electric conductivity
Become, with optical property, the new material most possibly substituting tin indium oxide at present, and nano silver wire thin film also has flexibility, is
Following flexible display device and the exploitation of wearable electronic product, have laid a good foundation.
Nano silver wire typically refers to diameter and arrives hundreds of nanometer at tens nanometers, and length is several microns to tens microns one-dimensional
Silver nano material.Since the advent of the world, people have carried out substantial amounts of research to its preparation method.Wherein, Physical includes magnetic control and splashes
Penetrate, the method such as ultrasonic grinding, mechanical activation comminution.Chemical method includes hydrothermal synthesis method, photochemical reduction, electrochemical process, template
Method, ultrasound wave reducing process and polyol process etc..Physical technique is complex, and energy consumption is larger, and technical requirements are high, and obtain
Product morphology homogeneity poor, serious being restricted of nano silver wire specification of preparation.Physical relatively, the technique of chemical method
Relatively simple, preparation cost is relatively low, and the nano silver wire specification prepared is more diversified, is hopeful most to be applied to silver nanoparticle
Thread industrial metaplasia is produced.Wherein polyol process is high with its preparation efficiency, product morphology is homogeneous, process is simple the advantages of become nearly more than ten
Study hotspot over year.
After preparing nano silver wire using polyol process first from Xia Younan, people have carried out substantial amounts of research to the method
And improvement, prepared a series of nano silver wire of different-diameters and length, and be applied in transparency electrode carried out each
Plant performance test.It has been found that the diameter of nano silver wire and length are to the electric conductivity of nano silver wire transparent conductive film, light transmission
And mist degree has extreme influence, prepare the nano silver wire that diameter is relatively thin, length is longer, pattern is homogeneous extremely urgent.At present,
The diameter of the nano silver wire prepared that substantial amounts of document and patent are reported is in more than 40nm, and nano silver wire length is homogeneous
Property is not ideal, but this some factor has all directly influenced the mist degree of transparent conductive film, greatly hinders nano silver wire
The development and application of transparency electrode.
Content of the invention
It is an object of the invention to provide a kind of nano silver wire, this preparation method is by being used in mixed way different types of halogen
With pvp as controlling agent and dressing agent, by controlling temperature-rise period and charging process thus the nucleation of effective control nano silver wire
Size and the speed of growth, prepare diameter and are less than 40nm, length and the homogeneous ultra-fine nano silver wire of diameter.
The technical solution used in the present invention:
A kind of homogeneous ultra-fine nano silver wire of pattern, its a diameter of 20-40nm, length is 20-50 μm.
A kind of preparation method of the homogeneous ultra-fine nano silver wire of pattern, using improved polyol process, the steps include: by
Pvp solution is heated to 120-170 DEG C, adds a certain amount of halogen and agno3, react 0.5h, the more certain density agno of Deca3
Solution, time for adding is 0.25-4h, reacts 0.5-4h after completion of dropping again, and reaction terminates rear centrifugation, then by product with
Finite concentration is dispersed in dispersant.
Described halogen is nacl, nicl2, nabr and kbr therein one or more combination, during multiple combination be Mixed bittern
Salt, is made up of a kind of chloride and a kind of bromide.
Described agno3First time addition with add halogen ion mol ratio be 1:1-5:1.
Described agno3In whole reaction system, concentration is 0.03-0.07m, wherein nacl and agno3Mol ratio be 1:
10-1:100, nicl2With agno3Mol ratio be 1:50-1:500, nabr and agno3Mol ratio be 1:20-1:200, kbr
With agno3Mol ratio be 1:20-1:200.
Described pvp and agno3Mol ratio be 1:1-9:1, wherein pvp molecular weight is 5.5 ten thousand, 360,000,1,300,000 therein
One or more combination.
The mixed proportion of described multiple combination its different molecular weight of pvp is 1,300,000: 5.5 ten thousand=2:1 or 360,000: 130
Ten thousand=1:1.
Described reaction temperature is 120 DEG C -170 DEG C, corresponding agno3Time for adding 4h-0.25h.Temperature is lower, Deca speed
Degree is slower, and the response time is longer.
The process of described centrifugation is divided into twice, and after stock solution is diluted 5 times, first time centrifugal rotational speed is 2000-
3000rpm, second rotating speed is 1000-2000rpm, each centrifugation ten minutes.
Described dispersant is water, ethanol, isopropanol, and dispersion concentration in dispersant for the product is 0.1%-1%.
Beneficial effects of the present invention: the nano silver wire of the present invention and its synthetic method, compared with prior art, its beneficial effect
Fruit shows:
1st, the present invention is therein a kind of or many by being used in mixed way sodium chloride and Nickel dichloride. and sodium bromide and nickelous bromide
Plant combination, by introducing bromide ion, on the one hand form silver chloride and Silver monobromide reduces the rate of reduction of silver ion well, have
Nucleation process beneficial to nano silver wire;Another reverse side bromide ion selective absorption, on the different crystal faces of silver atoms, effectively presses down
Make the cross growth of nano silver wire, thus reducing the diameter of silver wire.Can effectively be adjusted by the species and concentration changing halogen
The diameter of nano silver wire, prepares the nano silver wire that average diameter is 25nm, 30nm, 35nm.
2nd, the present invention pvp of different molecular one of is used or several as dressing agent, greatly improve silver nanoparticle
The homogeneity of the pattern of line, especially its diameter.The addition concentration that this method one side passes through to change pvp changes reaction system
Viscosity;On the other hand, change the stand density in nanometer silver surface for the pvp by regulating and controlling the molecular weight of pvp.Pvp molecular weight is got over
Greatly, the viscosity of the higher reaction system of concentration is bigger, sterically hindered bigger suffered by silver nanowire growth.Viscosity too high or
The too low growth being all unfavorable for nano silver wire, leads to by-product to increase, diameter pole heterogeneity.By being used in mixed way different molecular weight
Pvp can effectively adjust reaction system viscosity, small molecule pvp can be made to be inserted in the middle of macromole pvp again, lifting modify effect
Really, thus improving the pattern of nano silver wire.
3rd, in preparation technology, the present invention, according to the thermodynamics and kineticses rule of reaction, reaction is divided into three phases.The
One stage was at a certain temperature, generated silver chloride and Silver monobromide as heterogeneous nucleus;Second stage is silver ion in silver halide
Colloid surface starts to be reduced to silver atoms, is grown into as twin crystal seed;Phase III crystal seed is grown into as nano silver wire.Its
In, second step is rate-determining step.In the case that reaction temperature is corresponding with the addition speed of silver ion, could effectively prepare
The homogeneous nano silver wire of pattern.
Specific embodiment
Embodiment 1
Prepare the preparation method of the nano silver wire of a diameter of 25nm, the steps include: for pvp solution to be heated to 120 DEG C, add
A certain amount of halogen and agno3, wherein nacl and agno3Mol ratio be 1:20, nabr or kbr and agno3Mol ratio be 1:
50, react 0.5h, the more certain density agno of Deca3Solution, agno in maintenance system3Concentration is 0.03m, pvp and agno3's
Mol ratio is 1:2, and the dropwise reaction time is 4h, after reaction terminates, stock solution is diluted 5 times, carries out being centrifuged for the first time, rotating speed is
2000-3000rpm, after centrifugation 10min, pours out clear liquid, carries out second centrifugation, and rotating speed is 1000-2000rpm, is centrifuged 10min
Afterwards product is dispersed in water, dispersion concentration 1%, that is, prepares a diameter of 25nm nano silver wire.
Embodiment 2
Prepare the preparation method of the nano silver wire of a diameter of 30nm, the steps include: for pvp solution to be heated to 140 DEG C, add
A certain amount of halogen and agno3, wherein nicl2With agno3Mol ratio be 1:100, nabr or kbr and agno3Mol ratio be
1:200, reacts 0.5h, the more certain density agno of Deca3Solution, agno in maintenance system3Concentration is 0.05m, pvp and agno3
Mol ratio be 1:3, the dropwise reaction time is 2h, after reaction terminates, stock solution is diluted 5 times, carries out being centrifuged for the first time, rotating speed is
2000-3000rpm, after centrifugation 10min, pours out clear liquid, carries out second centrifugation, and rotating speed is 1000-2000rpm, is centrifuged 10min
Afterwards product is dispersed in water, dispersion concentration 1%, that is, prepares a diameter of 30nm nano silver wire.
Embodiment 3
Prepare the preparation method of the nano silver wire of a diameter of 35nm, the steps include: for pvp solution to be heated to 150 DEG C, add
A certain amount of halogen and agno3, wherein nacl and agno3Mol ratio be 1:25, nabr or kbr and agno3Mol ratio be 1:
100, react 0.5h, the more certain density agno of Deca3Solution, agno in maintenance system3Concentration is 0.06m, pvp and agno3's
Mol ratio is 1:3, and the dropwise reaction time is 1h, after reaction terminates, stock solution is diluted 5 times, carries out being centrifuged for the first time, rotating speed is
2000-3000rpm, after centrifugation 10min, pours out clear liquid, carries out second centrifugation, and rotating speed is 1000-2000rpm, is centrifuged 10min
Afterwards product is dispersed in water, dispersion concentration 0.5%, that is, prepares a diameter of 35nm nano silver wire.
Embodiment 4
Prepare the preparation method of the nano silver wire of a diameter of 40nm, the steps include: for pvp solution to be heated to 170 DEG C, add
A certain amount of halogen and agno3, wherein nacl and agno3Mol ratio be 1:25, nabr or kbr and agno3Mol ratio be 1:
100, react 0.5h, the more certain density agno of Deca3Solution, agno in maintenance system3Concentration is 0.07m, pvp and agno3's
Mol ratio is 1:6, and the dropwise reaction time is 0.25h, after reaction terminates, stock solution is diluted 5 times, carries out being centrifuged for the first time, rotating speed
For 2000-3000rpm, after being centrifuged 10min, pour out clear liquid, carry out second centrifugation, rotating speed is 1000-2000rpm, centrifugation
After 10min, product is dispersed in water, dispersion concentration 0.1%, that is, prepares a diameter of 40nm nano silver wire.
Above four embodiments of the present invention are described in detail, but described content has been only the preferable enforcement of the present invention
Example is it is impossible to be considered the practical range for limiting the present invention.All impartial changes made according to the present patent application scope and improvement
Deng all should still belong within the patent covering scope of the present invention.
Claims (10)
1. it is characterised in that a diameter of 20-40nm, length is 20-50 μm to a kind of homogeneous ultra-fine nano silver wire of pattern.
2. a kind of preparation method of the homogeneous ultra-fine nano silver wire of the pattern described in claim 1 is it is characterised in that with improved
Prepared by polyol process, the steps include: for pvp solution to be heated to 120-170 DEG C, adds a certain amount of halogen and agno3, reaction
0.5h, the more certain density agno of Deca3Solution, time for adding is 0.25-4h, reacts 0.5-4h after completion of dropping again, reaction
Then product is dispersed in dispersant by centrifugation after end with finite concentration.
3. the preparation method of the homogeneous ultra-fine nano silver wire of pattern according to claim 2 is it is characterised in that described halogen
For nacl, nicl2, nabr and kbr therein one or more combination, during multiple combination be mixing halogen, by a kind of chloride
With a kind of bromide composition.
4. the preparation method of the homogeneous ultra-fine nano silver wire of pattern according to claim 2 is it is characterised in that described agno3
First time addition with add halogen ion mol ratio be 1:1-5:1.
5. the preparation method of the homogeneous ultra-fine nano silver wire of pattern according to claim 3 is it is characterised in that described agno3
In whole reaction system, concentration is 0.03-0.07m, wherein nacl and agno3Mol ratio be 1:10-1:100, nicl2With
agno3Mol ratio be 1:50-1:500, nabr and agno3Mol ratio be 1:20-1:200, kbr and agno3Mol ratio be
1:20-1:200.
6. the preparation method of the homogeneous ultra-fine nano silver wire of pattern according to claim 2 is it is characterised in that described pvp
With agno3Mol ratio be 1:1-9:1, wherein pvp molecular weight be 5.5 ten thousand, 360,000,1,300,000 therein one or more combination.
7. the preparation method of the homogeneous ultra-fine nano silver wire of pattern according to claim 6 is it is characterised in that described is many
The mixed proportion planting combination its different molecular weight of pvp is 1,300,000: 5.5 ten thousand=2:1 or 360,000: 130 ten thousand=1:1.
8. the preparation method of the homogeneous ultra-fine nano silver wire of pattern according to claim 2 is it is characterised in that described reaction
Temperature is 120 DEG C -170 DEG C, corresponding agno3Time for adding 4h-0.25h, temperature is lower, and rate of addition is slower, the response time
Longer.
9. the preparation method of the homogeneous ultra-fine nano silver wire of pattern according to claim 2 is it is characterised in that described centrifugation
Detached process is divided into twice, and after stock solution is diluted 5 times, first time centrifugal rotational speed is 2000-3000rpm, and second centrifugation turns
Speed is 1000-2000rpm, each centrifugation ten minutes.
10. the preparation method of the homogeneous ultra-fine nano silver wire of pattern according to claim 2 is it is characterised in that described
Dispersant is water, ethanol, isopropanol, and dispersion concentration in dispersant for the product is 0.1%-1%.
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Cited By (8)
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CN108668517A (en) * | 2017-04-01 | 2018-10-16 | 中国科学院化学研究所 | Electromagnetic shielding film and preparation method thereof |
CN108927531A (en) * | 2018-08-22 | 2018-12-04 | 华南理工大学 | A kind of silver nanowires and its preparation method and application based on more nucleation controlling agents |
CN109261982A (en) * | 2018-11-07 | 2019-01-25 | 暨南大学 | A kind of method of simple and quick preparation silver nanowires |
CN109482900A (en) * | 2018-12-14 | 2019-03-19 | 浙江加州国际纳米技术研究院台州分院 | A kind of method high-volume synthesis and efficiently purify ultra-fine silver nanowires |
CN110010876A (en) * | 2019-04-15 | 2019-07-12 | 深圳市高能达电池有限公司 | A kind of controllable method for preparing of lithium sulphur one-shot battery nano anode material |
CN110976907A (en) * | 2019-12-23 | 2020-04-10 | 华南理工大学 | Preparation method of silver nanowire with high length-diameter ratio |
CN112155017A (en) * | 2020-08-31 | 2021-01-01 | 上海产业技术研究院 | Nano silver wire composite material and preparation method and application thereof |
CN112620644A (en) * | 2020-12-15 | 2021-04-09 | 紫金矿业集团股份有限公司 | Method for chemically synthesizing silver nanowires by using molten salt |
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CN108668517A (en) * | 2017-04-01 | 2018-10-16 | 中国科学院化学研究所 | Electromagnetic shielding film and preparation method thereof |
CN108927531A (en) * | 2018-08-22 | 2018-12-04 | 华南理工大学 | A kind of silver nanowires and its preparation method and application based on more nucleation controlling agents |
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CN110976907A (en) * | 2019-12-23 | 2020-04-10 | 华南理工大学 | Preparation method of silver nanowire with high length-diameter ratio |
CN112155017A (en) * | 2020-08-31 | 2021-01-01 | 上海产业技术研究院 | Nano silver wire composite material and preparation method and application thereof |
CN112620644A (en) * | 2020-12-15 | 2021-04-09 | 紫金矿业集团股份有限公司 | Method for chemically synthesizing silver nanowires by using molten salt |
CN112620644B (en) * | 2020-12-15 | 2022-03-01 | 紫金矿业集团股份有限公司 | Method for chemically synthesizing silver nanowires by using molten salt |
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Application publication date: 20170125 |