CN108856726A - A kind of preparation method of super nano silver wires with high length-diameter ratio - Google Patents
A kind of preparation method of super nano silver wires with high length-diameter ratio Download PDFInfo
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- CN108856726A CN108856726A CN201710230534.7A CN201710230534A CN108856726A CN 108856726 A CN108856726 A CN 108856726A CN 201710230534 A CN201710230534 A CN 201710230534A CN 108856726 A CN108856726 A CN 108856726A
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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
Abstract
Disclose a kind of nano-silver thread preparation method of draw ratio 500~1000, (1) by polyvinylpyrrolidone, 160~180 DEG C of 8~10min of reaction of ethylene glycol solution of copper chloride and silver nitrate prepare crystal seed, silver nitrate solution is disposably injected as silver-colored source is grown in crystal seed system again, makes its oriented growth nano-silver thread.(2) above-mentioned a certain amount of nano-silver thread slurry is taken, the disposable polyvinylpyrrolidone and the ethylene glycol solution of silver nitrate of injecting makes its continued growth in silver wire.(3) super nano silver wires with high length-diameter ratio of the draw ratio 500~1000 can be produced by step (2) being repeated several times.The nano-silver thread that this method is produced not only size uniformity, it is easy to operate, it is at low cost, and significantly improve the draw ratio of nano-silver thread.
Description
Technical field
The present invention relates to the preparation technical field of nano-silver thread more particularly to a kind of preparations of super nano silver wires with high length-diameter ratio
Method.
Background technique
A kind of line of the nano wire as nanoscale is horizontally to be restricted to 100 nanometers or less (not limit longitudinally
System) one-dimentional structure.Nano-silver thread also has in addition to having the excellent electric conductivity of silver due to the dimensional effect of Nano grade
Excellent translucency and buckle resistance is accordingly regarded as being the most possible material for substituting conventional oxidation indium tin (ITO) transparent electrode
Material.Relatively traditional transparent conductive material, nano-silver thread has the advantages such as the low, relative moderate of dosage, therefore can be widely applied
In various transparent conductive materials, such as flexible solar battery, capacitance plate conductive material, thus to realize flexible, bent LED
Display, touch screen etc. provide possibility.
Consider from the translucency of flexible clear materials and electric conductivity, added nano-silver thread need suitable diameter and
Higher draw ratio is easy to be prepared on a large scale, and free from admixture.High length-diameter ratio is conducive to nano-silver thread and is being overlapped to form conductive path
When can generate less contact point, the contact resistance of contact point generation can be reduced in this way to improving electric conductivity, high major diameter
The nano-silver thread of ratio can improve the electric conductivity and light transmission of transparent conductive material simultaneously.
The nano-silver thread preparation method having disclosed has template, electrochemical process, alcohol reduction method, wet chemistry method, solvent heat
Method etc., silver nanowires material can be prepared in above method, but Yield comparison is low；Or need to introduce other particles, such as
Nano platinum particle is added during the reaction as crystal seed, causes product impure, yield is lower.
Chinese patent (CN201110162476.1) discloses one kind and is quickly prepared on a large scale nano silver wires with high length-diameter ratio
Method, this method using microwave carry out auxiliary silver wire growth, troublesome in poeration, the diameter 300nm of preparing nano silver wire, influence its
Application in transparent conductive film；
Chinese patent (CN201210201644.8) discloses a kind of preparation method of nano-silver thread, and this method introduces acid
Solution helps producing for silver wire, and nano-silver thread major diameter obtained is relatively low.
Bibliography 1 prepares silver nano-grain/PVA fiber with method of electrostatic spinning, and this method preparation process is simple, easily grasps
Make, and significantly increases the draw ratio (93.5 μm of average length) of silver wire.
The ultra-long silver nanowire that length is about 100 μm is made using solvent-thermal method for bibliography 2, and simple process is easy to grasp
Make.But the ultra-long silver nanowire surface of this method preparation usually coats layer of surface activating agent, hinders the transmission of electronics,
Cause its conductivity lower, cannot be directly used to prepare fexible conductor.
The silver nanowires that bibliography 3 is prepared by multiple round-robin method makes nano silver on the basis of polyol reduction method
Line is fixed
To multistep cycling deposition is carried out, average length is obtained as 95 μm of nano silver wires with high length-diameter ratio, but the method
Strict control material addition manner and process reaction speed are needed, the production technology time is very long.
In summary, the prior art is difficult in the nano-silver thread for being prepared superelevation draw ratio using easy operating condition,
So need to be improved.Pertinent literature is as follows：
Bibliography 1：Barakat Nasser AM, Woo Kee-Do, Kanjwal Muzafar A, et
Al.Surface plasmon resonances, optical properties, and electrical conductivity
thermal hystersis of silver nanofibers produced by the electrospinning
Technique [J] .Langmuir, 2008,24 (20)：11982-11987.
Bibliography 2：Yao Hong-Bin, Huang Gang, Cui Chun-Hua, et al.Macroscale
elastomeric conductors generated from hydrothermally synthesized metal-
Polymer hybrid nanocable sponges [J] .Advanced Materials, 2011,23 (32)：3643-3647.
Bibliography 3：Seobh Lee Seung, HwanLKo Seung.Very long Ag nanowire
Synthesis and its application in a highly transparent, conductive and flexible
Metal electrode touch panel [J] .Nanoscale, 2012,4 (20)：6408-6414.
Summary of the invention
It is surprisingly found by the inventors that the combination of the addition manner and growth conditions of material prepares nanometer to polyol reduction method
The draw ratio of silver wire has different technical effects.The invention discloses a kind of preparation method of super nano silver wires with high length-diameter ratio,
It can get 50~200 μm, diameter 80nm~100nm of length, the nano-silver thread that draw ratio is 500~1000, and products pure, ruler
It is very little it is uniform, be easy to realize industrial production.
The technical solution adopted by the present invention includes the following steps：
(1) by polyvinylpyrrolidone, the ethylene glycol solution of copper chloride and silver nitrate, which is added in reaction kettle, to be stirred, and is controlled
Temperature processed is 160~180 DEG C, and 8~20min of heat preservation is obtained containing nano-silver thread crystal seed suspending liquid A；
The concentration of the polyvinylpyrrolidonesolution solution is 0.2~0.5mol/L, the concentration of copper chloride solution is 0.02~
0.05mol/L, the concentration of silver nitrate solution are 0.05~0.09mol/L；
Preferably, the number-average molecular weight of the polyvinylpyrrolidone is 10000~50000；
Preferably, polyvinylpyrrolidone and silver nitrate molar ratio are 5~7, and the molar ratio of silver nitrate and copper chloride is 2；
(2) the silver nitrate ethylene glycol solution of 0.075~0.095mol/L of concentration is disposably injected in A, and keeps identical
Temperature 20min obtains the grey suspension B containing nano-silver thread, to complete a secondary growth；
Preferably, silver nitrate solution and the mass ratio of crystal seed suspending liquid A are 1: 2~1: 4 in step (2)；
(3) a quarter is taken out from nano-silver thread grey suspension B, the ethylene glycol with polyvinylpyrrolidone and silver nitrate
Solution mixes in a kettle, keeps the temperature 1 hour at a temperature of 160~180 DEG C, completes diauxic growth, obtains diauxic growth suspension
Liquid；
The concentration of polyvinylpyrrolidone used is 0.4~0.5mol/L；The concentration of silver nitrate used be 0.075~
0.095mol/L；
The mole of silver nitrate solution is 20%~46% of silver-colored mole in suspension B；Polyvinylpyrrolidone used
It is 5~7 with silver nitrate molar ratio；
(4) 5/6~5/7 part is taken out from diauxic growth suspension, the ethylene glycol with polyvinylpyrrolidone and silver nitrate
Solution mixes in a kettle, carries out third secondary growth, the nitre of polyvinylpyrrolidone used according to the identical condition of step (3)
The concentration and its proportion of sour silver solution are identical as step (3), and the mole of silver nitrate is also identical as step (3)；
(5) the 4th time and the 5th secondary growth are successively carried out according to step (4) same procedure；Can successively be made diameter 80nm~
The super nano silver wires with high length-diameter ratio product of 100nm, draw ratio 500~1000；
(6) suspension is synthesized using acetone and deionized water cleaning silver wire, and silver wire product is saved in ethanol.
Compared with prior art, the present invention has the following advantages that：
The present invention combines polyol reduction method and crystal seed method, using the nano-silver thread of back reaction preparation as latter
The seed of reaction is walked, is repeatedly added and grows silver-colored source, make short nano-silver thread successively oriented growth, to realize superelevation draw ratio
Nano-silver thread is produced.The simple process is feasible, easy to operate, significantly improves the draw ratio of nano-silver thread, by growing number
Control, the nano-silver thread of draw ratio 500~1000 can be prepared.
Detailed description of the invention
The SEM photograph of the obstructed growth phase product of Fig. 1 embodiment 1.
The SEM photograph of 2 product of Fig. 2 embodiment.
The SEM photograph of 3 product of Fig. 3 embodiment.
The SEM photograph of 4 product of Fig. 4 embodiment.
The SEM photograph of 1 product of Fig. 5 comparative example.
The SEM photograph of 2 product of Fig. 6 comparative example.
Specific embodiment
Embodiment 1
1) using ethylene glycol as solvent, the AgNO for being 0.08mol/L by 100ml concentration3Solution, 100ml concentration are
The CuCl of 0.04mol/L2Solution, PVP solution (molecular weight of PVP is 40000) mixing that 100ml concentration is 0.45mol/L add
Enter in reaction kettle, the mixing speed of 400rpm and 170 DEG C at a temperature of react 10min.
2) AgNO for being 0.09mol/L by 50ml molar concentration3Solution disposably injects in above-mentioned system, at identical temperature
Insulated and stirred 20min obtains the crystal seed suspension of a secondary growth.The pattern of nano-silver thread is shown in Fig. 1 in gained crystal seed suspension
(a)。
3) 100ml is taken out from the crystal seed suspension of an above-mentioned secondary growth, it is molten for the PVP of 0.45mol/L with 10ml concentration
The AgNO that liquid and 10ml concentration are 0.09mol/L3Another reaction kettle is added in solution after mixing, and keeps the temperature at the same temperature
Stirring 1 hour, obtains diauxic growth suspension.Nano-silver thread product is shown in Fig. 1 (b).
4) 100ml is taken out from above-mentioned growth suspension, the PVP solution and 10ml concentration for being 0.45mol/L with 10ml concentration
For the AgNO of 0.09mol/L3Another reaction kettle is added in solution after mixing again, and under the conditions of above-mentioned same reaction temperature
It is stirred to react 1 hour, obtains three secondary growth suspension.Nano-silver thread product is shown in Fig. 1 (c).
5) the step of repeating step 4), successively obtains four times and five secondary growth suspension, after the 4th time and the 5th secondary growth
Product SEM figure see attached drawing 1 (d) and (e) respectively, wherein the 5th 200 μm of obtained nano-silver thread average length, draw ratio
Greater than 1000.
Embodiment 2
1) using ethylene glycol as solvent, the AgNO for being 0.06mol/L by 50ml concentration3Solution, 50ml concentration are 0.03mol/L
CuCl2Solution, PVP solution (molecular weight of PVP is 10000) mixing that 50ml concentration is 0.4mol/L are added in reaction kettle,
The mixing speed of 400rpm and 170 DEG C at a temperature of react 10min.
2) AgNO for being 0.08mol/L by 50ml concentration3Solution disposably injects in reaction kettle, continues insulated and stirred reaction
20min obtains the crystal seed suspension of a secondary growth.
3) 50ml is taken out from the crystal seed suspension of an above-mentioned secondary growth, the PVP solution for being 0.4mol/L with 10ml concentration
The AgNO for being 0.08mol/L with 10ml concentration3Reaction kettle is added in solution after mixing again, and in same reaction temperature condition
Under be stirred to react 1 hour, obtain diauxic growth suspension.
4) 50ml is taken out from above-mentioned growth suspension, the PVP solution for being 0.4mol/L with 10ml concentration and 10ml concentration are
The AgNO of 0.08mol/L3Solution is uniformly mixed reaction kettle is added again, and is stirred to react 1 hour under the conditions of same reaction temperature,
Obtain three secondary growth suspension.
5) the step of repeating step 4), successively obtains four times and five secondary growth suspension, the SEM figure of final product is shown in attached drawing
2, nano-silver thread average length is about 70 μm, and draw ratio is more than 800.
Embodiment 3
1) using ethylene glycol as solvent, the AgNO for being 0.08mol/L by 100ml concentration3Solution, 100ml concentration are
The CuCl of 0.04mol/L2Solution, PVP solution (molecular weight of PVP is 40000) mixing that 100ml concentration is 0.48mol/L add
Enter in reaction kettle, the mixing speed of 400rpm and 160 DEG C at a temperature of react 15min.
2) AgNO for being 0.08mol/L by 100ml concentration3Solution disposably injects in reaction kettle, and it is anti-to continue insulated and stirred
It answers 1 hour, obtains the crystal seed suspension of a secondary growth.
3) 100ml is taken out from the crystal seed suspension of an above-mentioned secondary growth, it is molten for the PVP of 0.48mol/L with 10ml concentration
The AgNO that liquid and 10ml concentration are 0.08mol/L3Reaction kettle is added in solution after mixing again, and in same reaction temperature item
It is stirred to react under part 1 hour, obtains diauxic growth suspension.
4) 100ml is taken out from above-mentioned growth suspension, the PVP solution and 10ml concentration for being 0.48mol/L with 10ml concentration
For the AgNO of 0.08mol/L3Solution is uniformly mixed reaction kettle is added again, and it is small under the conditions of same reaction temperature to be stirred to react 1
When, obtain three secondary growth suspension.
5) the step of repeating step 4), successively obtains four times and five secondary growth suspension, the SEM figure of final product is shown in attached drawing
3, nano-silver thread average length is about 80 μm, and draw ratio is more than 800.
Embodiment 4
1) using ethylene glycol as solvent, the AgNO for being 0.08mol/L by 100ml concentration3Solution, 100ml concentration are
The CuCl of 0.04mol/L2Solution, PVP solution (molecular weight of PVP is 40000) mixing that 100ml concentration is 0.45mol/L add
Enter in reaction kettle, the mixing speed of 400rpm and 170 DEG C at a temperature of react 10min.
2) AgNO for being 0.09mol/L by 100ml concentration3Solution disposably injects in reaction kettle, and it is anti-to continue insulated and stirred
It answers 1 hour, obtains the crystal seed suspension of a secondary growth.
3) 50ml is taken out from the crystal seed suspension of an above-mentioned secondary growth, the PVP solution for being 0.45mol/L with 10ml concentration
The AgNO for being 0.09mol/L with 10ml concentration3Reaction kettle is added in solution after mixing again, and in same reaction temperature condition
Under be stirred to react 1 hour, obtain diauxic growth suspension.
4) 50ml is taken out from above-mentioned growth suspension, the PVP solution for being 0.45mol/L with 10ml concentration and 10ml concentration are
The AgNO of 0.09mol/L3Solution is uniformly mixed reaction kettle is added again, and is stirred to react 1 hour under the conditions of same reaction temperature,
Obtain three secondary growth suspension.
5) the step of repeating step 4), successively obtains four times and five secondary growth suspension, the SEM figure of final product is shown in attached drawing
3, nano-silver thread average length is more than 100 μm
Comparative example 1
Keeping other reaction conditions and embodiment 1 under the same conditions, this comparative example is by the PVP solution (molecular weight of PVP
40000) and AgNO for3The concentration of solution adjusts the product SEM figure that respectively 0.5mol/L and 0.05mol/L are obtained and sees attached drawing 5,
Nano-silver thread draw ratio is lower than 100, and pattern is irregular.
Comparative example 2
Other reaction conditions and embodiment 1 are being kept under the same conditions, except that first time growth time extends
To 60min, obtained product SEM figure is shown in attached drawing 6, and nano-silver thread still keeps lower draw ratio and random by multistep growth
Pattern.
Claims (4)
1. a kind of preparation method of super nano silver wires with high length-diameter ratio, which is characterized in that include the following steps：
(1) by polyvinylpyrrolidone, the ethylene glycol solution of copper chloride and silver nitrate, which is added in reaction kettle, to be stirred, control temperature
Degree is 160~180 DEG C, and 8~20min of heat preservation is obtained containing nano-silver thread crystal seed suspending liquid A；
Polyvinylpyrrolidone and silver nitrate molar ratio are 5~7, and the molar ratio of silver nitrate and copper chloride is 2；
(2) the silver nitrate ethylene glycol solution of 0.075~0.095mol/L of concentration is disposably injected in A, and kept mutually synthermal
20min obtains the grey suspension B containing nano-silver thread, to complete a secondary growth；
(3) a quarter is taken out from nano-silver thread grey suspension B, the ethylene glycol solution with polyvinylpyrrolidone and silver nitrate
It mixes in a kettle, keeps the temperature 1 hour at a temperature of 160~180 DEG C, complete diauxic growth, obtain diauxic growth suspension；
The concentration of polyvinylpyrrolidone used is 0.4~0.5mol/L；The concentration of silver nitrate used be 0.075~
0.095mol/L；
The mole of silver nitrate solution is 20%~46% of silver-colored mole in suspension B；Polyvinylpyrrolidone and nitre used
Sour silver molar ratio is 5~7；
(4) 5/6~5/7 part is taken out from diauxic growth suspension, the ethylene glycol solution with polyvinylpyrrolidone and silver nitrate
It mixes in a kettle, carries out third secondary growth, the silver nitrate of polyvinylpyrrolidone used according to the identical condition of step (3)
The concentration and its proportion of solution are identical as step (3), and the mole of silver nitrate is also identical as step (3)；
(5) the 4th time and the 5th secondary growth are successively carried out according to step (4) same procedure；Can successively be made 80~100nm of diameter,
The super nano silver wires with high length-diameter ratio product of draw ratio 500~1000；
(6) suspension is synthesized using acetone and deionized water cleaning silver wire, and silver wire product is saved in ethanol.
2. the preparation method of super nano silver wires with high length-diameter ratio according to claim 1, which is characterized in that polyvinylpyrrolidine
The number-average molecular weight of ketone is 10000~50000.
3. the preparation method of any one super nano silver wires with high length-diameter ratio according to claim 1~2, which is characterized in that step
(2) silver nitrate solution and the mass ratio of crystal seed suspending liquid A are 1: 2~1: 4 in.
4. the nano-silver thread of any one the method preparation according to claim 1~3.
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Cited By (6)
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| CN111426742A (en) * | 2020-04-21 | 2020-07-17 | 四川大学 | Application of silver nanowire material as MA L DI-TOF MS matrix in metabolite detection |
| CN112207271A (en) * | 2019-09-29 | 2021-01-12 | 海泰纳鑫科技(成都)有限公司 | Superfine silver nanowire and preparation method thereof |
| CN112643044A (en) * | 2020-12-18 | 2021-04-13 | 哈尔滨工业大学（深圳） | Preparation method of silver nanowire with high length-diameter ratio |
| CN112893862A (en) * | 2021-01-19 | 2021-06-04 | 南京苏展智能科技有限公司 | Silver nanowire, preparation method thereof and conductive film prepared from silver nanowire |
| CN113059181A (en) * | 2021-03-25 | 2021-07-02 | 广东工业大学 | Nano silver wire and preparation method and application thereof |
| WO2023078320A1 (en) * | 2021-11-08 | 2023-05-11 | 西北有色金属研究院 | Ultralong silver nanowire material and preparation method therefor |
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| WO2023078320A1 (en) * | 2021-11-08 | 2023-05-11 | 西北有色金属研究院 | Ultralong silver nanowire material and preparation method therefor |
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