CN107256741B - A kind of method of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance - Google Patents
A kind of method of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance Download PDFInfo
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Abstract
The invention discloses a kind of methods that solvent evaporates annealing enhancing metal nanometer line transparent conductive film performance.The characteristics of this method is generally soluble in polar solvent using metal nanometer line surface ligand PVP, method for annealing is evaporated by low-boiling alcohols solvent to remove metal nanometer line surface ligand PVP, reduce the contact resistance between metal nanometer line, achievees the purpose that the square resistance for reducing metal nanometer line transparent conductive film.The method of the present invention technical process is simple, at low cost, can evaporate annealing time by adjusting solvent, realize the adjusting between contact resistance size metal nanometer line, realize the regulation to metal nanometer line transparent conductive film square resistance；Treated metal nanometer line transparent conductive film, compares untreated original metal nano wire transparent conductive film, and square resistance reduces 8% ~ 50%.
Description
Technical field
The present invention relates to the transparent conductive film preparation technical fields of photoelectric device, and in particular to a kind of solvent evaporation annealing
Enhance the method for metal nanometer line transparent conductive film performance.
Technical background
With the sustained and rapid development of modern opto-electronics, many aspects of the transparent conductive film in social life in recent years
It is applied, and has come into daily life.Transparent conductive film is mainly used in such as FPD, e-book, intelligence
The field of photoelectric devices such as energy mobile phone, intelligent glass, touch screen, light emitting diode and solar battery.It is widely used for currently, comparing
The material of production transparent conductive film is the metal oxide of doping, such as the indium oxide of tin dope（ITO）, aluminium doping zinc oxide
（AZO）With the tin oxide of Fluorin doped（FTO）Deng.Although current commercialized ITO, AZO, FTO transparent conductive film has excellent
Optically and electrically performance, but the increase with industry to transparent conductive electrode demand the miniaturization of photoelectric device and can wear
The appearance of equipment is worn, these three transparent conductive films have been unable to satisfy answering in next-generation consumer electronics and clean energy resource field
With.In recent years, it has been developed that some nano-functional materials replace ITO.The representative are：Conducting polymer, carbon
Nanotube, graphene and metal nanometer line.In these materials, Typical Representative of the silver nanowires as metal nano material, tool
There is the features such as higher conductivity, thermal conductivity, flexibility and solution are processed, it has also become be most hopeful to substitute the electrically conducting transparent electricity of ITO
Pole material.The film build method of common metal nanometer line have very much, as spin-coating method, Meyer stick method, spray coating method, vacuum filtration method and
Roll-to-rool printing etc., these film build methods rapidly develop the preparation of metallic transparent conductive film and application,
But also flexible photoelectric device is possibly realized.
Currently, metal nanometer line using liquid phase low temperature synthetic method can large scale preparation, generally using exhausted in synthesis process
The surface ligand polyvinylpyrrolidone (PVP) of edge regulates and controls its size and dispersibility, and excessive PVP end-capping reagent covering can shield
The surface charge of nano wire causes the Van der Waals force between nano wire to play a major role, and the bundle shape of nano wire is easy to cause to assemble,
Also increase the contact resistance between metal nanometer line simultaneously.Such as：For silver nanowires transparent conductive film, R. M.Mutiso etc.
People combines method by numerical simulation and experiment data to analyze effective contact resistance between AgNWs, and discovery exists for diameter
50 ~ 80 nm range AgNWs conductive films, effective contact resistance is in 1.5 ~ 2.5 K Ω（ACS Nano, 7: 7654
(2013)）.In order to reduce the contact resistance between AgNWs, it is necessary to introduce some post-processing technologies, California, USA university Los Angeles point
The Yang Yang in school（ACS Nano, 5: 9877(2011)）With the Jooho Moon of Univ Yonsei Seoul of South Korea（ACS Nano, 7:
1081(2013)）Equal seminars use oxide nano-particles, as TiO2, ZnO come as node fusion agent or surface capping agents
Improve the contact between AgNWs node.In addition, there are also researchers to use nano-weld technology（Nat. Mater., 11: 241
(2012)）Deng node loose between nano wire is welded, its electric conductivity is increased.But these processing methods generally all mistake
Journey is complicated or at high cost.
Usual PVP layers of metal nanometer line surface ligand is by weak Van der Waals for beam with its metal nanometer line surface
It is tied together, part PVP is generally removed by polar solvent repeated washing and centrifugation, and remove excessive PVP and will lead to AgNWs
Difficulties in dispersion is unfavorable for solution processing and prepares transparent conductive film.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of solvents to evaporate annealing enhancing metal nanometer line electrically conducting transparent
The method of film performance.The characteristics of this method is generally soluble in polar solvent using metal nanometer line surface ligand PVP, by low
The alcohols solvent of boiling point evaporates method for annealing to remove metal nanometer line surface ligand PVP, reduces the contact between metal nanometer line
Resistance achievees the purpose that the square resistance for reducing metal nanometer line transparent conductive film.
The present invention is achieved through the following technical solutions.
A kind of method of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance, includes the following steps：
（1）Metal nanometer line dispersion liquid is prepared into metal nanowire thin-films by solution processing method on substrate, then
Heat treatment removal residual solvent, obtains metal nanometer line transparent conductive film；
（2）Obtained metal nanometer line transparent conductive film is placed in closed container, low-boiling alcohols solvent is added,
Metal nanometer line transparent conductive film is not directly contacted with low-boiling alcohols solvent, carries out solvent evaporation in-situ annealing processing；
Solvent evaporates in in-situ annealing treatment process, and low-boiling alcohols solvent evaporation is formed on metal nanometer line surface
Drop is partly dissolved the surface ligand PVP of metal nanometer line and is detached from PVP from metal nanometer line surface, realizes and reduce metal
Contact resistance between nano wire reduces the purpose of the square resistance of metal nanometer line transparent conductive film；
（3）After solvent evaporation annealing, metal nanometer line transparent conductive film is taken out, is placed in thermal station at heating
Reason removes residual solvent, obtains the metal nanometer line transparent conductive film of performance enhancement.
Further, step（1）In, the metal nanometer line includes that nanowires of gold, silver nanowires, copper nano-wire or nickel are received
Rice noodles.
Further, step（1）In, the mass fraction 0.01% ~ 3% of the metal nanometer line dispersion liquid, dispersion liquid it is molten
Agent includes methanol, ethyl alcohol or isopropanol.
Further, step（1）In, the solution processing method includes spin-coating method, spray coating method, self assembly czochralski method, steps
Stick method or vacuum filtration method.
Further, step（1）In, the substrate is transparent substrates, including glass substrate, polyethylene terephthalate
Rouge substrate, polyimide substrate, dimethyl silicone polymer substrate, polymethyl methacrylate substrate or polycarbonate substrate.
Further, step（1）In, the heat treatment is 10 ~ 20min of heating at 80 ~ 100 DEG C.
Further, step（2）In, the low-boiling alcohols solvent includes methanol, ethyl alcohol or isopropanol etc..
Further, step（2）In, the additive amount of the low-boiling alcohols solvent is the amount of metal nanometer line dispersion liquid
10% ~ 20%.
Further, step（2）In, the solvent evaporation in-situ annealing processing is after low-boiling alcohols solvent will be added
Closed container be placed in room temperature environment and place 1 ~ 3 hour.
Further, step（3）In, the heat treatment is in 70 ~ 100 DEG C of 10 ~ 30min of heating.
Further, finally obtained metal nanometer line transparent conductive film compares untreated original metal nanometer
Line transparent conductive film, square resistance reduce 8% ~ 50%.
Compared with prior art, the invention has the advantages that and beneficial effect：
（1）The method of the present invention has the advantages that technical process is simple, at low cost；
（2）The present invention can evaporate annealing time by adjusting solvent, realize between contact resistance size metal nanometer line
It adjusts, realizes the regulation to metal nanometer line transparent conductive film square resistance；
（3）The method of the present invention treated metal nanometer line transparent conductive film, receives compared to untreated original metal
Rice noodles transparent conductive film, square resistance reduce 8% ~ 50%.
Detailed description of the invention
Fig. 1 a is the high contact resistance between the surface ligand PVP and its silver nanowires of the AgNWs used in specific embodiment
Schematic diagram；
Fig. 1 b is the low contact resistance between the surface ligand PVP and its silver nanowires of the AgNWs used in specific embodiment
Schematic diagram；
Fig. 2 is AgNWs solvent anneal schematic diagram in embodiment 1；
Fig. 3 a and Fig. 3 b are the surface ligand PVP in embodiment 1 before solvent evaporation annealing with AgNWs after solvent evaporation annealing
TEM figure.
Specific embodiment
To evaporate solvent of the present invention annealing enhancing metal nanometer line electrically conducting transparent below in conjunction with specific embodiment
Film performance and preparation method thereof is described in further detail.But protection scope of the presently claimed invention is not limited to embodiment
Related range.
Solvent evaporation annealing technology of the present invention is existed using low boiling points alcohols solvents such as methanol, ethyl alcohol or isopropanols
It volatilizees in closed container, then dissolves the surface ligand PVP of metal nanometer line at droplet in metal nanometer line surface aggregation,
Cause PVP ligand to be detached to reduce the contact resistance between metal nanometer line from metal nanometer line surface, realizes that reducing metal receives
The purpose of rice noodles transparent membrane square resistance.
The silver nanowires used in the specific embodiment of the invention（AgNWs）Surface ligand PVP and its silver nanowires between
High and low contact resistance schematic diagram is shown as illustrated in figs. 1A and ib respectively, as can be seen from figs. 1a and 1b, the surface ligand of AgNWs
When PVP layers thicker, the contact resistance between silver nanowires is larger；PVP layers of surface ligand of AgNWs it is relatively thin when, between silver nanowires
Contact resistance is low.
Embodiment 1
A kind of method of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance, includes the following steps：
（1）It uses isopropanol for solvent, silver nanowires is made into the silver nanowires solution that mass fraction is 1%, silver nanowires
Partial size length be 10 ~ 50 μm, diameter is 20 ~ 80 nm, and after being shaken up with shaking table, be filtered by vacuum, obtained with miillpore filter
To dispersion liquid evenly dispersed and without the silver nanowires isopropanol obviously reunited；
（2）Cleaning is successively followed the steps below to glass substrate：Washing lotion ultrasound 10 minutes, acetone ultrasound 10 minutes, go from
It is sub- water ultrasound 10 minutes, isopropanol ultrasound 10 minutes, stand-by after drying；
（3）The dispersion liquid of silver nanowires isopropanol is then spin-coated on glass lined by glass progress oxygen plasma cleaning
On bottom, spin coating revolving speed is 2500 r/min, and spin-coating time is 60 s, thin in the silver nanowires that glass substrate surface covers 120 nm
Film heats 15 minutes for 80 DEG C in thermal station, obtains silver nanowires transparent conductive film；
（4）Prepared silver nanowires transparent conductive film is placed in closed container, it is molten that methanol is added dropwise in a reservoir
Agent（Dispersion liquid spin coating amount relative to silver nanowires isopropanol is 10%）, silver nanowires transparent conductive film and methanol is not direct
Contact, then closes the lid；It is placed 3 hours under room temperature environment, so that methanol solvate is carried out solvent evaporation annealing, partially go
Except the surface ligand PVP of silver nanowires；Methanol solvate evaporation annealing schematic diagram it is as shown in Figure 2, metal nanowire thin-films as
Low-boiling alcohols solvent is added in bottom in closed container, while in container, evaporates to form gas to alcohols solvent；Metal
After nano wire film stands 3 hours in the steam of alcohols solvent, i.e. expression solvent evaporation annealing；
（5）After solvent evaporation annealing, silver nanowires transparent conductive film is taken out, is placed in thermal station at heating
Reason places 80 DEG C of heating in thermal station and removes remaining methanol solvate in 30 minutes, obtains the silver nanowires electrically conducting transparent of performance enhancement
Film.
Fig. 3 a and Fig. 3 b are respectively that the surface of the silver nanowires before carrying out methanol solvate evaporation annealing and gone out after managing is matched
The TEM of body PVP schemes, after will become apparent from methanol solvate evaporation annealing from TEM test result, the surface ligand of silver nanowires
It is transparent to be finally substantially reduced silver nanowires so that the contact resistance between making silver nanowires reduces for the removal effect highly significant of PVP
The square resistance of conductive film；Initial light transmittance of the silver nanowires transparent conductive film at 550 nm is 90 %, by methanol
Solvent evaporation annealing can make its square resistance be reduced to 24.7 Ω/ from 44.1 Ω/, in addition, molten after 3 hours
Agent evaporation annealing technology does not influence the light transmittance of silver nanowires transparent conductive film.
Embodiment 2
A kind of method of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance, includes the following steps：
（1）It uses ethyl alcohol for solvent, silver nanowires is made into the silver nanowires solution that mass fraction is 0.01%, silver nanoparticle
The partial size length of line is 10 ~ 50 μm, diameter is 20 ~ 80 nm, and after being shaken up with shaking table, is filtered by vacuum with miillpore filter,
Obtain dispersion liquid evenly dispersed and without the silver nanowires ethyl alcohol obviously reunited；
（2）Cleaning is successively followed the steps below to glass substrate：Washing lotion ultrasound 10 minutes, acetone ultrasound 10 minutes, go from
It is sub- water ultrasound 10 minutes, isopropanol ultrasound 10 minutes, stand-by after drying；
（3）The dispersion liquid of silver nanowires ethyl alcohol is then spin-coated on glass substrate by glass progress oxygen plasma cleaning
On, spin coating revolving speed is 2500 r/min, and spin-coating time is 60 s, thin in the silver nanowires that glass substrate surface covers 120 nm
Film heats 8 minutes for 100 DEG C in thermal station, obtains silver nanowires transparent conductive film；
（4）Prepared silver nanowires transparent conductive film is placed in closed container, it is molten that methanol is added dropwise in a reservoir
Agent（Dispersion liquid spin coating amount relative to silver nanowires isopropanol is 15%）, silver nanowires transparent conductive film and methanol is not direct
Contact, then closes the lid；It is placed 1 hour under room temperature environment, so that methanol solvate is carried out solvent evaporation annealing, partially go
Except the surface ligand PVP of silver nanowires；Methanol solvate evaporation annealing schematic diagram it is as shown in Figure 2, metal nanowire thin-films as
Low-boiling alcohols solvent is added in bottom in closed container, while in container, evaporates to form gas to alcohols solvent；Metal
After nano wire film stands 1 hour in the steam of alcohols solvent, i.e. expression solvent evaporation annealing；
（5）After solvent evaporation annealing, silver nanowires transparent conductive film is taken out, is placed in thermal station at heating
Reason places 70 DEG C of heating in thermal station and removes remaining methanol solvate in 25 minutes, obtains the silver nanowires electrically conducting transparent of performance enhancement
Film.
After methanol solvate evaporation annealing, the removal effect highly significant of the surface ligand PVP of silver nanowires, to make
Contact resistance between silver nanowires reduces, and is finally substantially reduced the square resistance of silver nanowires transparent conductive film；Initial silver is received
Light transmittance of the rice noodles transparent conductive film at 550 nm is 86 %, can be with after methanol solvate evaporation annealing 1 hour
Its square resistance is set to be reduced to 37.6 Ω/ from 42.3 Ω/, in addition, solvent evaporates annealing technology to silver nanowires
The light transmittance of transparent conductive film does not influence.
Embodiment 3
A kind of method of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance, includes the following steps：
（1）It uses methanol for solvent, silver nanowires is made into the silver nanowires solution that mass fraction is 3%, silver nanowires
Partial size length is 10 ~ 50 μm, diameter is 20 ~ 80 nm, and after being shaken up with shaking table, is filtered by vacuum, is obtained with miillpore filter
Dispersion liquid evenly dispersed and without the silver nanowires methanol obviously reunited；
（2）Cleaning is successively followed the steps below to glass substrate：Washing lotion ultrasound 10 minutes, acetone ultrasound 10 minutes, go from
It is sub- water ultrasound 10 minutes, isopropanol ultrasound 10 minutes, stand-by after drying；
（3）The dispersion liquid of silver nanowires methanol is then spin-coated on glass substrate by glass progress oxygen plasma cleaning
On, spin coating revolving speed is 2500 r/min, and spin-coating time is 60 s, thin in the silver nanowires that glass substrate surface covers 120 nm
Film heats 20 minutes for 85 DEG C in thermal station, obtains silver nanowires transparent conductive film；
（4）Prepared silver nanowires transparent conductive film is placed in closed container, it is molten that methanol is added dropwise in a reservoir
Agent（Dispersion liquid spin coating amount relative to silver nanowires isopropanol is 20%）, silver nanowires transparent conductive film and methanol is not direct
Contact, then closes the lid；It is placed 2 hours under room temperature environment, so that methanol solvate is carried out solvent evaporation annealing, partially go
Except the surface ligand PVP of silver nanowires；Methanol solvate evaporation annealing schematic diagram it is as shown in Figure 2, metal nanowire thin-films as
Low-boiling alcohols solvent is added in bottom in closed container, while in container, evaporates to form gas to alcohols solvent；Metal
After nano wire film stands 2 hours in the steam of alcohols solvent, i.e. expression solvent evaporation annealing；
（5）After solvent evaporation annealing, silver nanowires transparent conductive film is taken out, is placed in thermal station at heating
Reason places 100 DEG C of heating in thermal station and removes remaining methanol solvate in 10 minutes, obtains the silver nanowires electrically conducting transparent of performance enhancement
Film.
After methanol solvate evaporation annealing, the removal effect highly significant of the surface ligand PVP of silver nanowires, to make
Contact resistance between silver nanowires reduces, and is finally substantially reduced the square resistance of silver nanowires transparent conductive film；Initial silver is received
Light transmittance of the rice noodles transparent conductive film at 550 nm is 92 %, can be with after methanol solvate evaporation annealing 2 hours
Its square resistance is set to be reduced to 23.7 5 Ω/ from 43.5 Ω/, in addition, solvent evaporates annealing technology to silver nanowires
The light transmittance of transparent conductive film does not influence.
Claims (8)
1. a kind of method of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance, which is characterized in that including such as
Lower step：
（1）Metal nanometer line dispersion liquid is prepared into metal nanowire thin-films by solution processing method on substrate, then at heat
Reason removal residual solvent, obtains metal nanometer line transparent conductive film；The solution processing method include spin-coating method, spray coating method,
Self assembly czochralski method, Meyer stick method or vacuum filtration method；
（2）Obtained metal nanometer line transparent conductive film is placed in closed container, low-boiling alcohols solvent, metal is added
Nano wire transparent conductive film is not directly contacted with low-boiling alcohols solvent, carries out solvent evaporation in-situ annealing processing；It is described
Solvent evaporation in-situ annealing processing is the closed container after low-boiling alcohols solvent will be added to be placed in room temperature environment to place 1 ~ 3
Hour；
（3）Solvent evaporates in-situ annealing after treatment, takes out metal nanometer line transparent conductive film, is placed in thermal station at heating
Reason removes residual solvent, obtains the metal nanometer line transparent conductive film of performance enhancement.
2. a kind of side of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance according to claim 1
Method, which is characterized in that step（1）In, the metal nanometer line includes nanowires of gold, silver nanowires, copper nano-wire or nickel nanometer
Line；The mass fraction 0.01% ~ 3% of the metal nanometer line dispersion liquid, the solvent of dispersion liquid include methanol, ethyl alcohol or isopropanol.
3. a kind of side of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance according to claim 1
Method, which is characterized in that step（1）In, the substrate is transparent substrates, including glass substrate, polyethylene terephthalate
Substrate, polyimide substrate, dimethyl silicone polymer substrate, polymethyl methacrylate substrate or polycarbonate substrate.
4. a kind of side of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance according to claim 1
Method, which is characterized in that step（1）In, the heat treatment is 8 ~ 20min of heating at 80 DEG C ~ 100 DEG C.
5. a kind of side of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance according to claim 1
Method, which is characterized in that step（2）In, the low-boiling alcohols solvent includes methanol, ethyl alcohol or isopropanol.
6. a kind of side of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance according to claim 1
Method, which is characterized in that step（2）In, the additive amount of the low-boiling alcohols solvent is the amount of metal nanometer line dispersion liquid
10%~20%。
7. a kind of side of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance according to claim 1
Method, which is characterized in that step（3）In, the heat treatment is in 70 ~ 100 DEG C of 10 ~ 30min of heating.
8. a kind of side of solvent evaporation annealing enhancing metal nanometer line transparent conductive film performance according to claim 1
Method, which is characterized in that finally obtained metal nanometer line transparent conductive film, it is saturating compared to untreated original metal nano wire
Bright conductive film, square resistance reduce 8% ~ 50%.
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| CN114843035B (en) * | 2022-05-23 | 2024-06-21 | 中国人民解放军国防科技大学 | Curved surface crack template preparation method based on reverse pulling method and metal grid conductive film preparation method |
| CN115995311B (en) * | 2023-03-21 | 2023-05-23 | 浙江大华技术股份有限公司 | Silver nanowire transparent conductive film and preparation method and application thereof |
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| JP6053246B1 (en) * | 2015-07-30 | 2016-12-27 | バンドー化学株式会社 | Electrode manufacturing method |
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