CN105750559A - Method of preparing silver nanowire and transparent conductive film of silver nanowire - Google Patents
Method of preparing silver nanowire and transparent conductive film of silver nanowire Download PDFInfo
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- CN105750559A CN105750559A CN201610022132.3A CN201610022132A CN105750559A CN 105750559 A CN105750559 A CN 105750559A CN 201610022132 A CN201610022132 A CN 201610022132A CN 105750559 A CN105750559 A CN 105750559A
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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
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
Abstract
The invention discloses a method of preparing a silver nanowire and a transparent conductive film of the silver nanowire, and belongs to the technical field of nano material synthesis and thin film preparation.The transparent conductive film has high light transmission and low surface resistance.The method for preparing the silver nanowire is simple, the prepared silver nanowire is good in diameter uniformity, the conductive film is good in light transmission and low in surface resistance, and the silver nanowire can be applied to preparation of the transparent conductive film, so that the prepared conductive film is good in light transmission and low in surface resistance.Under the condition of similar light transmitting performance, the prepared transparent conductive film is low in square resistance, and meanwhile good adhesion performance is achieved.
Description
Technical field
The invention belongs to nano material synthesis and technical field of film preparation, particularly to the preparation method of a kind of nano silver wire and nesa coating thereof, described nesa coating has high light transmittance and low sheet resistance.
Background technology
Except tin indium oxide (ITO), prepare the material of nesa coating (TCFs) also just like Graphene, CNT, metal nanometer line etc..Nano silver wire nesa coating therein, because nano silver wire is prepared relatively easy, its can on hard substrate film forming, again can on organic flexible substrate film forming, and the TCFs prepared has the light transmission of excellence and less sheet resistance, and it will have a wide range of applications in fields such as photoelectricity, bio-sensing, catalysis, diode and touch screens.
Research for nano silver wire has expanded numerous research work, and its synthetic method has electrochemical process, chemical reduction method, photoreduction met hod, microwave heating method etc..Nano silver wire is also prepared nesa coating and has been studied by current a lot of scholars.(JongDeckPark, SoomanLim, the HaekyongKim.ThinSolidFilms such as Jian-YangLin, 2015,586:70-75.) using the nano silver wire film forming prepared of polyol process, it has the light transmittance of 92.15% under visible ray mean wavelength, and square resistance is 20 Ω/.Nano silver wire is prepared film forming through printing ink printing art by JongDeckpark etc. (J.Jiu, T.Araki, J.Wang, M.Nogi, T.Sugahara.ournalofMaterialsChemistryA, 2014,2:6326-6330.), and its resistance is 32 Ω mm-1Time have 95% light transmittance.J.JIU uses length to be about the nano silver wire of 60nm more than 60um, diameter, prepares the thin film that light transmittance is 91% that square resistance is 25 Ω/, 550nm wavelength place.(the AnujR.Madaria such as AnujR.Madaria, AkshayKumar, FumiakiN.Ishikawa, ChongwuZhou.NanoRes, 2010,3:564-573.) to use nano silver wire to prepare square resistance on flexible substrate PET be 10 Ω/, light transmittance be the nesa coating of 85%.But, when close light transmission, prepare square resistance less and there is the nesa coating of good adhesion property simultaneously there be difficulties involved when.
Summary of the invention
The primary and foremost purpose of the present invention is in that the preparation method providing a kind of nano silver wire.The nano silver wire prepared by the method can apply in the preparation of nesa coating, makes the conducting film light transmission prepared good, and sheet resistance is little.
Another object of the present invention is to provide the nano silver wire obtained by described preparation method.The diameter homogeneity of described nano silver wire is good, and conducting film light transmission is good, and sheet resistance is little.
It is still another object of the present invention to provide the method utilizing described nano silver wire to prepare nesa coating.
The purpose of the present invention is achieved through the following technical solutions: the preparation method of a kind of nano silver wire, comprises the steps:
(1) will be 0.037g/mL containing polyvinylpyrrolidone (PVP) concentration and salinity be 0.001g/mL cumulative volume will be the polyhydric alcohol solutions of 30ml, be added drop-wise to volume to be 20ml concentration be the silver nitrate (AgNO of 0.250mol/l3) polyhydric alcohol solutions in, through magnetic stirring apparatus mix and blend 10min, obtain mixed solution；
(2) mixed solution of step (1) is poured in reactor, react 7h in 160 DEG C, obtain the dehydrated alcohol dispersion liquid of nano silver wire；
In step (1):
nullThe molecular weight of described polyvinylpyrrolidone is 0.35 ten thousand-176 ten thousand，Being preferably molecular weight is the PVPK12 of 0.35 ten thousand、Molecular weight is the PVPK17 of 1.01 ten thousand、Molecular weight is the PVPK25 of 3.2 ten thousand、Molecular weight is the PVPK30 of 4.0 ten thousand、Molecular weight is the PVPK45 of 150,000、Molecular weight is the PVPK60 of 210,000、Molecular weight is the PVPK70 of 400,000、Molecular weight is the PVPK80 of 580,000、Molecular weight is the PVPK85 of 600,000、Molecular weight is the PVPK90 of 630,000、Molecular weight is the PVPK100 of 780,000、Molecular weight is the PVPK110 of 1,100,000、Molecular weight is the mixture of a kind of or at least two in the PVPK120 and PVPK150 that molecular weight is 1,760,000 of 1,390,000.
Described polyvinylpyrrolidone is more preferably the PVPK30 that molecular weight is 4.0 ten thousand.
Described salt is potassium chloride (KCl), magnesium chloride (MgCl2), copper chloride (CuCl2), sodium chloride (NaCl), calcium chloride (CaCl2), silver chloride (AgCl), ferrous chloride (FeCl2), platinous chloride (PtCl2), copper bromide (CuBr2), potassium bromide (KBr), magnesium bromide (MgBr2), calcium bromide (CaBr2), sodium bromide (NaBr), one in Silver monobromide (AgBr) or at least two mixture, it is preferred to sodium chloride.
Described polyhydric alcohol is the one in ethylene glycol, propylene glycol, glycerol or at least two mixture, it is preferred to ethylene glycol.
Described polyvinylpyrrolidone (PVP) and the polyhydric alcohol solutions of salt obtain for polyvinylpyrrolidone and salt being dissolved in polyhydric alcohol solutions；
The polyhydric alcohol solutions of described silver nitrate obtains for being dissolved in polyhydric alcohol solutions by silver nitrate；This operation needs to carry out in the environment of lucifuge.
Operation in step (2) carries out preferably in electric heating constant-temperature blowing drying box.
A kind of nano silver wire, is obtained by above-mentioned preparation method.
A kind of method utilizing described nano silver wire to prepare nesa coating, comprises the steps:
The dehydrated alcohol dispersant liquid drop of above-mentioned nano silver wire is added on glass substrate through 10s rotating speed be 500-2000r/min spin coating；Then spin coating is had 10s on the hot plate that the glass substrate of nano silver wire is placed in 100 DEG C；Then the 1-Methyl-2-Pyrrolidone solution of polymethyl methacrylate (PMMA) is dripped in spin coating have on the glass substrate of nano silver wire through 10s rotating speed be 3000-5000r/min spin coating, then anneal 0-2min on the hot plate of 200-400 DEG C, obtains nano silver wire nesa coating；The mass ratio of described polymethyl methacrylate (PMMA) and 1-Methyl-2-Pyrrolidone is 1:40.
Described AgNO3, PVP, polyhydric alcohol, salt, dehydrated alcohol, PMMA and 1-Methyl-2-Pyrrolidone be analytical pure.
The present invention has such advantages as relative to prior art and effect:
The preparation method of the nano silver wire of the present invention is simple, and the diameter homogeneity of the nano silver wire prepared is good, makes the conducting film light transmission prepared good, and sheet resistance is little.When close light transmission, nesa coating square resistance prepared by the present invention is less, has good adhesion property simultaneously.
Accompanying drawing explanation
Fig. 1 is the SEM figure of nano silver wire, wherein: a, 10.0 microns；B, 1.00 microns；
Fig. 2 is XRD (a) and UV-VIS (b) the test result figure of nano silver wire；
Fig. 3 is the light transmission test result figure and sample number figure that different square resistance is corresponding, wherein: (a), (b) are the light transmission test result figure that different square resistance is corresponding, (c) is sample number figure that square resistance is 12 Ω/.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
The preparation method of a kind of nano silver wire nesa coating is as follows:
(1) polyhydric alcohol solutions of polyvinylpyrrolidone 1.11g and NaCl0.03g is added in the polyhydric alcohol solutions of silver nitrate 0.85g, mix and blend 10min, obtain mixed liquor；Polyhydric alcohol is ethylene glycol, and volume is 0.05L；
(2) mixed solution of step (1) is poured in reactor, react 7h in 160 DEG C, stand through 3-4 washing of deionized water, obtain nano silver wire；The nano silver wire prepared has good draw ratio.The diameter of the nano silver wire prepared is at about 100nm, and length is at 30-50um.
(3) the dehydrated alcohol dispersant liquid drop that concentration is 0.1mol/l nano silver wire is added on glass substrate and through 10s rotating speed be 500r/min spin coating；Then spin coating is had 10s on the hot plate that the glass substrate of nano silver wire is placed in 100 DEG C, makes dehydrated alcohol volatilize；Then the 1-Methyl-2-Pyrrolidone solution of polymethyl methacrylate is dripped in spin coating have on the glass substrate of nano silver wire through 10s rotating speed be 4000r/min spin coating, then anneal 1min on the hot plate of 300 DEG C, obtain nano silver wire nesa coating, it is 97.15% at wavelength 500nm place light transmittance, and square resistance is 70.0 Ω/；The mass ratio of described polymethyl methacrylate and 1-Methyl-2-Pyrrolidone is 1:40.
Described AgNO3, PVP, polyhydric alcohol, salt, dehydrated alcohol, PMMA and 1-Methyl-2-Pyrrolidone be analytical pure.
Wherein, the SEM of the nano silver wire in embodiment 1 schemes as shown in Figure 1；The diameter of the nano silver wire in figure is at about 100nm, and length is between 30-50um, simultaneously it can also be seen that there is a small amount of nano-particle from figure, describes the practicality standing washing methods.
XRD and the UV-VIS test result of the nano silver wire in embodiment 1 is as shown in Figure 2；Fig. 2 (a) exists in the XRD figure of nano silver wire four obvious diffraction maximums, respectively at 38.1 °, 44.3 °, 64.4 ° and 77.4 °, this is essentially identical with the XRD standard card (JCPDS04-0783) of Ag, illustrate that polycrystalline nano silver wire is face-centered cubic crystal formation, calculate cell parameter according to XRD figure modal dataThis and standard valueClosely；And data can calculate (111) face peak value be 6139 is 6.84 with the ratio of the relative diffraction peak intensity that (200) face peak value is 898 from figure, relative diffraction peak intensity 2.50 more than theoretical (111) face with (200) face, simultaneously it can also be seen that the diffraction peak intensity in (111) face is equally much larger than (220) face and (311) face, this illustrates that the speed of growth in (111) face of crystal, more than the speed of growth in other faces, carries out one-dimensional growth and obtains nano silver wire in course of reaction.In UV-VIS absorption spectrum the absworption peak at 350nm and 390nm place correspond respectively to nano silver wire longitudinal plasmon absorption and what horizontal plasma resonance absorption caused, absworption peak later for 410nm corresponding to ping-pong ball shape, cube etc. granule.From Fig. 2 (b) it can be seen that the obvious absworption peak of existence the UV-VIS abosrption spectrogram of nano silver wire, at 350nm and 390nm place, it was demonstrated that the existence of nano silver wire；After 410nm, absworption peak is inconspicuous, it was demonstrated that Argent grain exists less, and this is identical with SEM test.
Embodiment 2
Substantially keep identical with embodiment 1, be distinctive in that the spin coating rotating speed of the dehydrated alcohol dispersion liquid of nano silver wire is 1000r/min.
Embodiment 3
Substantially keep identical with embodiment 1, be distinctive in that the spin coating rotating speed of the dehydrated alcohol dispersion liquid of nano silver wire is 2000r/min.
Embodiment 4
Substantially keep identical with embodiment 1, be distinctive in that the spin coating rotating speed of polymethyl methacrylate solution is 3000r/min.
Embodiment 5
Substantially keep identical with embodiment 1, be distinctive in that the spin coating rotating speed of polymethyl methacrylate solution is 5000r/min.
Embodiment 6
Substantially keep identical with embodiment 1, be distinctive in that the glass substrate of the good polymethyl methacrylate solution of spin coating is in 200 DEG C of 1min that anneal.
Embodiment 7
Substantially keep identical with embodiment 1, be distinctive in that the glass substrate of the good polymethyl methacrylate solution of spin coating is in 400 DEG C of 1min that anneal.
Embodiment 8
Substantially keep identical with embodiment 1, be distinctive in that the glass substrate of the good polymethyl methacrylate solution of spin coating is in 400 DEG C of 0min that anneal.
Embodiment 9
Substantially keep identical with embodiment 1, be distinctive in that the glass substrate of the good polymethyl methacrylate solution of spin coating is in 400 DEG C of 2min that anneal.
Embodiment 10
Substantially keep identical with embodiment 1, be distinctive in that the spin coating number of plies of the dehydrated alcohol dispersion liquid of nano silver wire is two-layer.
Embodiment 11
Substantially keep identical with embodiment 1, be distinctive in that the spin coating number of plies of the dehydrated alcohol dispersion liquid of nano silver wire is three layers.
Embodiment 12
Substantially keep identical with embodiment 1, be distinctive in that the spin coating number of plies of the dehydrated alcohol dispersion liquid of nano silver wire is four layers.
Fig. 3 is the light transmission test result figure and sample number figure that different square resistance is corresponding, wherein: (a), (b) are the light transmission test result figure that different square resistance is corresponding, square resistance is the sample correspondence embodiment 1 of 70 Ω/, square resistance is the sample correspondence embodiment 10 of 35 Ω/, square resistance is the sample correspondence embodiment 11 of 12 Ω/, square resistance is the sample correspondence embodiment 12 of 9 Ω/, and (c) is sample number figure that square resistance is 12 Ω/.
Above-described embodiment is the present invention preferably embodiment; but embodiments of the present invention are also not restricted to the described embodiments; the change made under other any spirit without departing from the present invention and principle, modification, replacement, combination, simplification; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. the preparation method of a nano silver wire, it is characterised in that comprise the steps:
(1) will be 0.037g/mL containing polyvinylpyrrolidoneconcentration concentration and salinity be 0.001g/mL cumulative volume is the polyhydric alcohol solutions of 30ml, it is added drop-wise to volume to be 20ml concentration is in the silver nitrate polyhydric alcohol solutions of 0.250mol/l, through magnetic stirring apparatus mix and blend 10min, obtain mixed solution；
(2) mixed solution of step (1) is poured in reactor, react 7h in 160 DEG C, obtain the dehydrated alcohol dispersion liquid of nano silver wire.
2. the preparation method of nano silver wire according to claim 1, it is characterised in that the molecular weight of the polyvinylpyrrolidone described in step (1) is 0.35 ten thousand-176 ten thousand.
null3. the preparation method of nano silver wire according to claim 1，It is characterized in that，Polyvinylpyrrolidone described in step (1) is molecular weight is the PVPK12 of 0.35 ten thousand、Molecular weight is the PVPK17 of 1.01 ten thousand、Molecular weight is the PVPK25 of 3.2 ten thousand、Molecular weight is the PVPK45 of 150,000、Molecular weight is the PVPK60 of 210,000、Molecular weight is the PVPK70 of 400,000、Molecular weight is the PVPK80 of 580,000、Molecular weight is the PVPK85 of 600,000、Molecular weight is the PVPK90 of 630,000、Molecular weight is the PVPK100 of 780,000、Molecular weight is the PVPK110 of 1,100,000、Molecular weight is the mixture of a kind of or at least two in the PVPK120 and PVPK150 that molecular weight is 1,760,000 of 1,390,000.
4. the preparation method of nano silver wire according to claim 1, it is characterised in that the polyvinylpyrrolidone described in step (1) is molecular weight is the PVPK30 of 4.0 ten thousand.
5. the preparation method of nano silver wire according to claim 1, it is characterized in that, the salt described in step (1) is the one in potassium chloride, magnesium chloride, copper chloride, calcium chloride, silver chloride, ferrous chloride, platinous chloride, copper bromide, potassium bromide, magnesium bromide, calcium bromide, sodium bromide, Silver monobromide or at least two mixture.
6. the preparation method of nano silver wire according to claim 1, it is characterised in that the salt described in step (1) is sodium chloride.
7. the preparation method of nano silver wire according to claim 1, it is characterised in that the polyhydric alcohol described in step (1) is one or both the mixture in propylene glycol, glycerol.
8. the preparation method of nano silver wire according to claim 1, it is characterised in that the polyhydric alcohol described in step (1) is ethylene glycol.
9. a nano silver wire, the preparation method described in any one of the claims 1-8 obtains.
10. the method utilizing nano silver wire described in claim 9 to prepare nesa coating, comprises the steps:
The dehydrated alcohol dispersion liquid of the nano silver wire described in claim 9 is dripped on glass substrate and through 10s rotating speed be 500-2000r/min spin coating；Then spin coating is had 10s on the hot plate that the glass substrate of nano silver wire is placed in 100 DEG C；Then the 1-Methyl-2-Pyrrolidone solution of polymethyl methacrylate is dripped and have on the glass substrate of nano silver wire through 10s rotating speed 3000-5000r/min spin coating in spin coating, then anneal 0-2min on the hot plate of 200-400 DEG C, obtains nano silver wire nesa coating；The mass ratio of described polymethyl methacrylate and 1-Methyl-2-Pyrrolidone is 1:40.
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Cited By (9)
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| CN106735294A (en) * | 2016-12-11 | 2017-05-31 | 浙江大学 | The preparation method of nano silver wire |
| CN107335811A (en) * | 2017-06-21 | 2017-11-10 | 天津宝兴威科技股份有限公司 | A kind of preparation method of high-purity nano silver wires with high length-diameter ratio |
| CN107486561A (en) * | 2017-07-27 | 2017-12-19 | 南京邮电大学 | A kind of method that extensive normal pressure prepares and separates nano silver wire |
| CN108262487A (en) * | 2018-01-20 | 2018-07-10 | 浙江大学 | The method that minor diameter nano silver wire is prepared using mixed alcohol |
| CN108436102A (en) * | 2018-05-28 | 2018-08-24 | 陕西科技大学 | A kind of preparation method of nano silver wires with high length-diameter ratio |
| CN109261982A (en) * | 2018-11-07 | 2019-01-25 | 暨南大学 | A kind of method of simple and quick preparation silver nanowires |
| CN109346242A (en) * | 2018-09-29 | 2019-02-15 | 华南理工大学 | A kind of transparent electrode and preparation method thereof based on silver nanowires |
| CN109926597A (en) * | 2019-02-20 | 2019-06-25 | 中国科学院金属研究所 | A kind of method that oil bath heating prepares tin nanometer sheet |
| CN110976907A (en) * | 2019-12-23 | 2020-04-10 | 华南理工大学 | Preparation method of silver nanowire with high length-diameter ratio |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106735294A (en) * | 2016-12-11 | 2017-05-31 | 浙江大学 | The preparation method of nano silver wire |
| CN107335811A (en) * | 2017-06-21 | 2017-11-10 | 天津宝兴威科技股份有限公司 | A kind of preparation method of high-purity nano silver wires with high length-diameter ratio |
| CN107486561A (en) * | 2017-07-27 | 2017-12-19 | 南京邮电大学 | A kind of method that extensive normal pressure prepares and separates nano silver wire |
| CN107486561B (en) * | 2017-07-27 | 2020-09-15 | 南京邮电大学 | Method for preparing and separating silver nanowires at large scale and normal pressure |
| CN108262487A (en) * | 2018-01-20 | 2018-07-10 | 浙江大学 | The method that minor diameter nano silver wire is prepared using mixed alcohol |
| CN108436102A (en) * | 2018-05-28 | 2018-08-24 | 陕西科技大学 | A kind of preparation method of nano silver wires with high length-diameter ratio |
| CN109346242A (en) * | 2018-09-29 | 2019-02-15 | 华南理工大学 | A kind of transparent electrode and preparation method thereof based on silver nanowires |
| CN109261982A (en) * | 2018-11-07 | 2019-01-25 | 暨南大学 | A kind of method of simple and quick preparation silver nanowires |
| CN109926597A (en) * | 2019-02-20 | 2019-06-25 | 中国科学院金属研究所 | A kind of method that oil bath heating prepares tin nanometer sheet |
| CN109926597B (en) * | 2019-02-20 | 2021-07-27 | 中国科学院金属研究所 | Method for preparing tin nanosheet by oil bath heating |
| CN110976907A (en) * | 2019-12-23 | 2020-04-10 | 华南理工大学 | Preparation method of silver nanowire with high length-diameter ratio |
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