CN105895266A - Method for improving chemical doping stability of carbon nanotube conductive film - Google Patents
Method for improving chemical doping stability of carbon nanotube conductive film Download PDFInfo
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- CN105895266A CN105895266A CN201610447171.8A CN201610447171A CN105895266A CN 105895266 A CN105895266 A CN 105895266A CN 201610447171 A CN201610447171 A CN 201610447171A CN 105895266 A CN105895266 A CN 105895266A
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- carbon nanotube
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- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
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Abstract
The invention discloses a method for improving the chemical doping stability of a carbon nanotube conductive film. The method comprises the following steps of: uniformly mixing a doped reagent with a material, which can be solidified in a set condition, so as to form a fluid mixed reagent, then, doping the carbon nanotube conductive film by utilizing the mixed reagent, and after that, performing solidification treatment so as to form a protective layer on the surface of the transparent carbon nanotube conductive film; or, after doping the carbon nanotube conductive film by using the doped reagent, at least applying the fluid material, which can be solidified in the set condition, on the surface of the carbon nanotube conductive film, and then, performing solidification treatment so as to form the protective layer on the surface of the carbon nanotube conductive film. According to the method disclosed by the invention, the doped reagent is obstructed by utilizing the structural coating (namely the protective layer); therefore, the doped reagent is not contacted with active substances (oxidized or reduced impurities) in an environment; and thus, the chemical doping stability of the carbon nanotube conductive film can be obviously improved.
Description
Technical field
The present invention be more particularly directed to a kind of method improving CNT (CNTs) conducting film chemical doping stability, belong to nano material
Field.
Background technology
One of flexible touch technology development trend becoming electronic applications.Flexible device requires its core material nesa coating
Need the bent performance with excellence.But tradition ITO conducting film is the most bent, the most urgently develop the replacement material of ITO conducting film
Material.
Carbon nanotube conductive film has the bendable folding endurance of excellence, and has substantially at aspects such as true color, chemical stability and costs
Advantage.SWCN (SWNT), compared with multi-walled carbon nano-tubes (MWNT), has more preferable electric conductivity, the most quilts
It is applied to flexible transparent conducting film.But the single tube material metallic single of current multiple synthetic method synthesis
Pipe forms with semi-conductive single-walled carbon nanotubes.Two kinds of carbon nano-tube conductives are widely different；And connect at random in carbon nano tube network
There is Schottky barrier between the metallicity and the semiconductor carbon nanometer tube that touch, directly affect the electrical properties of carbon nanotube conductive film.Cause
This intrinsic carbon nanotube conductive film cannot meet high-performance conductive film and hinder bottom surface and the requirement of high transmission rate, needs to lead CNT
Electrolemma is modified processing.
Most common method is to be improved the electric conductivity of carbon nano-tube film by chemical doping at present, and chemical doping can effectively reduce expense
Rice energy level, improve carrier concentration the contact resistance reducing between CNT.But chemical doping less stable, this be due to
Cannot effectively contact between adulterant with CNT, limit the electron transfer between adulterant and CNT；Additionally both it
Between faint chemisorbed easily destroyed by active component in surrounding and affect doping effect.It addition, the CNT after Can Za
Conducting film is severe through successive process (such as 150 DEG C of@1H of high-temperature baking) and reliability testing (such as 60 DEG C &90%RH@168H) etc.
During condition at quarter, show poor stability for above-mentioned reasons, it is impossible to realize the actual application of carbon nanotube conductive film.The most such as
What is effectively improved the stably-doped property of carbon nanotube conductive film is to limit its business-like bottleneck problem.
The method improving the stably-doped property of carbon nanotube conductive film mainly has: 1, use the doping reagent that chemical stability is good, such as
MnO3, the conductive network after doping still has preferable stability at 300 DEG C, but the method needs equipment costly and post processing to need
Want 450 DEG C of high temperature, be not suitable for flexible substrate；2. metal nanoparticle doping also can improve stably-doped property, but doping effect is relatively
Chemical reagent doping weak effect；3, carbon nano tube surface is adulterated by covalent bond.
Therefore, industry urgently develops a kind of method improving CNT (CNTs) conducting film chemical doping stability.
Summary of the invention
A kind of method improving carbon nanotube conductive film chemical doping stability of offer is provided, existing to overcome
Deficiency in technology.
To achieve these goals, the technical solution used in the present invention is as follows:
Embodiments provide a kind of method improving carbon nanotube conductive film chemical doping stability, including:
Reagent will be adulterated and uniformly can mix at the material of the lower solidification that imposes a condition, form the mix reagent in flow-like, afterwards profit
With described mix reagent, carbon nanotube conductive film is doped process, followed by cured, on carbon nanotube conductive film surface
Form protective layer；
Or, after carbon nanotube conductive film being doped process with the reagent that adulterates, more at least CNT after doping treatment is led
The surface of electrolemma apply in flow-like, cured can be carried out afterwards at the material of lower solidification that imposes a condition, thus receives at carbon
Mitron conducting film surface forms protective layer.
Wherein, described doping reagent includes p-type doping reagent or N-shaped doping reagent etc..
Wherein, described can comprise in acrylic acid, polyurethane, silica column and epoxy resin etc. at the material of the lower solidification that imposes a condition
The combination of any one or more, but be not limited to this.
Compared with prior art, the present invention forms structural type coating (i.e. protective layer) obstruct doping reagent by using, and makes doping try
Agent does not contacts with the active substance (oxidisability or reducing impurity) in environment, can significantly improve carbon nanotube conductive film chemical doping
Stability, such as, through the present invention process carbon nanotube conductive thin film test at high temperature 130 DEG C 1h and ring survey (60 DEG C
&90%RH) test 240H, resistance change rate < 10%；Additionally, CNT also can be effectively improved by the present invention on substrate
Adhesive force, greatly facilitates the industrialization of carbon nanotube conductive film.
Accompanying drawing explanation
In order to be illustrated more clearly that present configuration feature and technical essential, with detailed description of the invention, the present invention is entered below in conjunction with the accompanying drawings
Row describes in detail.
Fig. 1 is the flow chart of the method improving carbon nanotube conductive film chemical doping stability in the present invention one typical embodiments；
Fig. 2 is the schematic diagram of the method improving carbon nanotube conductive film chemical doping stability in the present invention one typical embodiments；
Fig. 3 is carbon nanotube conductive film stability test figure before and after processing through method shown in Fig. 1-Fig. 2.
Detailed description of the invention
In view of deficiency of the prior art, inventor, through studying for a long period of time and putting into practice, is proposed technical scheme, as
Lower will be illustrated.
Referring to is the typical embodiments of the present invention shown in Fig. 1 a, and what it related to a kind of improves carbon nanotube conductive film chemical doping
The method (being defined as " method one ") of stability includes:
Reagent will be adulterated and uniformly can mix at the material of the lower solidification that imposes a condition, form the mix reagent in flow-like, afterwards profit
With described mix reagent, carbon nanotube conductive film is doped process, followed by cured, on carbon nanotube conductive film surface
Form protective layer.
By this embodiment, a step doping treatment to carbon nanotube conductive film and stabilizing treatment can be realized.
Referring to is another typical embodiments of the present invention shown in Fig. 1 b, and its a kind of carbon nanotube conductive film chemistry that improves related to is mixed
The method (being defined as " method two ") of miscellaneous stability includes:
With doping after reagent is doped process to carbon nanotube conductive film, more at least carbon nanotube conductive film after doping treatment
Surface apply in flow-like, cured can be carried out afterwards at the material of lower solidification that imposes a condition, thus leads at CNT
Film surface forms protective layer.
In some more specific embodiment, the method for described raising carbon nanotube conductive film chemical doping stability includes following
Step:
Doping reagent is mixed to form described mix reagent with heat curing-type system or light curable type system；
It is applied to carbon nanotube conductive film surface, it is achieved the doping treatment to carbon nanotube conductive film to mixing described in major general；
And, under conditions of promoting described heat curing-type system or the solidification of light curable type system, make to be distributed in described carbon nanotube conducting
Described mix reagent solidification on film, forms described protective layer.
Described heat curing-type system or light curable type system can mainly by acrylic acid, polyurethane, silica gel, epoxy monomer etc. and be drawn accordingly
Send out the compositions such as agent such as isocyanates, platinum system firming agent, BPO firming agent.
In some more specific embodiment, the method for described raising carbon nanotube conductive film chemical doping stability may also include
Following steps:
With doping reagent, carbon nanotube conductive film is doped process；
At least doped process carbon nanotube conductive film surface apply in flow-like, mainly by polymer monomer and draw accordingly
Send out heat curing-type system or the light curable type system of agent composition, make described heat curing-type system or the solidification of light curable type system afterwards, thus in described
Carbon nanotube conductive film surface forms protective layer.
In some preferred embodiments, described mix reagent is selected from including adulterant, polymer monomer, initiator and diluent
Solution.
Wherein, described doping reagent includes p-type doping reagent or N-shaped doping reagent etc..
More preferred, described p-type doping reagent at least may include but be not limited to NO2、Br2、HNO3、SOCl2、H2SO4、H2O2、
OA (chlordene metaantimmonic acid triethyl group oxygen), MoO3、FeCl3、AuCl3、KMnO4The combination of any one or more in Deng.
More preferred, described N-shaped doping reagent at least may include but be not limited to any one in hydrazine hydrate, ammonia, ethylenediamine etc.
Or two or more combinations.
More preferred, described can at least may include but be not limited to acrylic acid, polyurethane, silicon at the material of the lower solidification that imposes a condition
The combination of any one or more in gum resin and epoxy resin etc..
In some preferred embodiments, described method may also include that at least selects drip washing, spraying, spin coating, blade coating, slotdie
Any one mode in (slit die head is extrusion coated), nick printing etc. is by described mix reagent, described doping reagent or described
Can be applied on carbon nanotube conductive film at the material of the lower solidification that imposes a condition.
More preferred, the thickness of described carbon nanotube conductive film is 2-1000nm, a length of 10-100 μm.
In some embodiments, described carbon nanotube conductive film covers in flexible transparent substrate, and described flexible transparent substrate is at least
May include but be not limited to any one or more in PET substrate, PI substrate, PDMS substrate, PMMA substrate and PC substrate etc.
Combination.
In some embodiments, described carbon nanotube conductive film is the conduction of the CNT coating solution after being dispersed through agent dispersion
Film.
In some embodiments, described carbon nanotube conductive film is the conducting film that aerosol deposition is formed in flexible transparent substrate.
More preferred, the thickness of described protective layer is 0.01-1 μm, in order to intercept the active substance in environment and doping reagent reacting.
Wherein, any one or two kinds of during described CNT includes SWCN, double-walled carbon nano-tube and multi-walled carbon nano-tubes
Above combination.
By the method improving carbon nanotube conductive film chemical doping stability of the present invention, refer to Fig. 2, can be at the chemistry formed
The carbon nanotube conductive film surface of doping forms very thin protective layer (being also regarded as a kind of structural type coating), and this layer of coating will not increase
Add carbon nanotube conductive film face resistance, but can intercept doping reagent and make its not with active substance (oxidisability or the reproducibility in environment
Impurity) contact, thus significantly improve the chemical doping stability of carbon nanotube conductive film.And the existence of this coating can also promote carbon
Nanotube films is combined with the fastening of substrate.
It addition, found by test of many times, refer to Fig. 3, by the raising carbon nano tube transparent conducting film chemical doping of the present invention
The carbon nanotube conductive film that the method for stability processed compares with undressed carbon nanotube conductive film, surveys (60 DEG C at ring
&90%RH) test 240H, resistance stability be improved significantly.
In conjunction with accompanying drawing and some embodiments, this technical scheme, its implementation process and principle etc. will be further explained as follows.
Embodiment 1
A) on metal pliable substrate, SWCN conducting film is prepared by CVD, by the single wall carbon on metal pliable substrate
Nanotube conductive film is transferred to flexible transparent substrate surface through volume to volume form and prepares carbon nano tube transparent conducting film (reference
CN103031531A etc.)；
B) water-soluble acrylic thermosets ethanol is configured to the coating fluid of solid content about 1%；
C) above-mentioned coating fluid is mixed according to the ratio of 1: 1 with the dispersion prepared chlorauric acid solution (concentration 20mM) in ethanol
Uniformly, thus be configured to adulterate reagent；
D) with above-mentioned doping reagent, carbon nano tube transparent conducting film being doped process, doping way is spin coating；
E) the carbon nano tube transparent conducting film after doping being carried out at 130 DEG C cured 2min, the carbon obtaining improved stability is received
Mitron nesa coating, this carbon nano tube transparent conducting film ring surveys (60 DEG C &90%RH) test 240H, resistance variations < 10%.
Embodiment 2
A) SWCN conducting film transfer PET substrate coated face is prepared with the single-walled carbon nanotube dispersion liquid of 1mg/mL through sucking filtration,
The SWCN conducting film (with reference to CN102602118A, CN102110489B etc.) prepared；
B) water-soluble acrylic thermosets ethanol is configured to the coating fluid of solid content about 1%；
C) above-mentioned coating fluid is mixed homogeneously with the dispersion prepared chlorauric acid solution (concentration 20mM) 1: 1 in ethanol, preparation
Become doping reagent；
D) with above-mentioned doping reagent, carbon nanotube conductive film being doped process, doping way is spin coating；
E) at 130 DEG C, the carbon nanotube conductive film after doping being carried out cured 2min, the CNT obtaining improved stability is led
Electrolemma, described conducting film ring surveys (60 DEG C &90%RH) test 240H, resistance variations < 10%.
Embodiment 3
A) on metal pliable substrate, SWCN conducting film is prepared by CVD, by the single wall carbon on metal pliable substrate
Nanotube conductive film is transferred to flexible transparent substrate surface through volume to volume form, thus prepares carbon nano tube transparent conducting film (reference
CN103031531A etc.)；
B) gold chloride is dissolved in ethanol, is made into the doping reagent of concentration 10mM；
C) with above-mentioned doping reagent, carbon nano tube transparent conducting film being doped process, doping way is drip washing；
D) water-soluble acrylic thermosets ethanol is configured to the coating fluid of solid content about 0.5%；
E) above-mentioned coating fluid bar is scratched the carbon nano tube transparent conducting film surface after doping；
F) carrying out cured 2min at 130 DEG C, obtain the carbon nano tube transparent conducting film of improved stability, this CNT is saturating
Bright conducting film ring surveys (60 DEG C &90%RH) test 240H, resistance variations < 10%.
Embodiment 4
A) on metal pliable substrate, SWCN conducting film is prepared by CVD, by the single wall carbon on metal pliable substrate
Nanotube conductive film is transferred to flexible transparent substrate surface through volume to volume form, thus prepares carbon nanotube conductive film (reference
CN103031531A etc.)；
B) as doping reagent, carbon nanotube conductive film being doped process with concentrated nitric acid, doping way is drip washing；
C) water-soluble acrylic UV shaped material ethanol is configured to the coating fluid of solid content about 0.5%；
D) above-mentioned coating fluid bar is scratched the carbon nanotube conductive film surface after doping；
E) solvent is dried at 80 DEG C by above-mentioned conducting film, cured 2min the most under w light, obtain improved stability
Carbon nanotube conductive film, described conducting film is 240H, resistance variations < 10% under the conditions of 60 DEG C &90%RH.
Embodiment 5
A) SWCN conducting film transfer PET substrate coated face is prepared with the single-walled carbon nanotube dispersion liquid of 1mg/mL through sucking filtration,
The SWCN nesa coating (with reference to CN102602118A, CN102110489B etc.) prepared；
B) as doping reagent, carbon nano tube transparent conducting film being doped process with concentrated nitric acid, doping way is drip washing；
C) water-soluble acrylic UV shaped material ethanol is configured to the coating fluid of solid content about 0.5%；
D) above-mentioned coating fluid bar is scratched the carbon nano tube transparent conducting film surface after doping；
E) solvent is dried at 80 DEG C by above-mentioned conducting film, cured 2min the most under w light, obtain improved stability
Carbon nano tube transparent conducting film, this carbon nano tube transparent conducting film ring surveys (60 DEG C &90%RH) test 240H, resistance variations < 10%.
Above-mentioned detailed description of the invention, is only technology design and the architectural feature of the explanation present invention, it is therefore intended that allow and be familiar with technique
Stakeholder can implement according to this, but above said content is not limiting as protection scope of the present invention, every spirit according to the present invention
Any equivalence that essence is made changes or modifies, and all should fall under the scope of the present invention.
Claims (12)
1. the method improving carbon nanotube conductive film chemical doping stability, it is characterised in that including:
Reagent will be adulterated and uniformly can mix at the material of the lower solidification that imposes a condition, form the mix reagent in flow-like, afterwards profit
With described mix reagent, carbon nanotube conductive film is doped process, followed by cured, on carbon nanotube conductive film surface
Form protective layer；
Or, after carbon nanotube conductive film being doped process with the reagent that adulterates, more at least CNT after doping treatment is led
The surface of electrolemma apply in flow-like, cured can be carried out afterwards at the material of lower solidification that imposes a condition, thus receives at carbon
Mitron conducting film surface forms protective layer.
The method of raising carbon nanotube conductive film chemical doping stability the most according to claim 1, it is characterised in that including:
Doping reagent is mixed to form described mix reagent with heat curing-type system or light curable type system；
It is applied to carbon nanotube conductive film surface, it is achieved the doping treatment to carbon nanotube conductive film to mixing described in major general；
And, under conditions of promoting described heat curing-type system or the solidification of light curable type system, make to be distributed in described carbon nanotube conducting
Described mix reagent solidification on film, forms described protective layer.
The method of raising carbon nanotube conductive film chemical doping stability the most according to claim 1, it is characterised in that described
Mix reagent is selected from the solution including adulterant, polymer monomer, initiator and diluent.
The method of raising carbon nanotube conductive film chemical doping stability the most according to claim 1, it is characterised in that including:
With doping reagent, carbon nanotube conductive film is doped process；
At least surface at the carbon nanotube conductive film of doped process applies the heat curing-type system in flow-like or light curable type system, it
After make described heat curing-type system or light curable type system solidification, thus in described carbon nanotube conductive film surface formed protective layer.
5. according to the method improving carbon nanotube conductive film chemical doping stability according to any one of claim 1-4, its feature
It is: described doping reagent includes p-type doping reagent or N-shaped doping reagent.
The method of raising carbon nanotube conductive film chemical doping stability the most according to claim 5, it is characterised in that:
Described p-type doping reagent includes NO2、Br2、HNO3、SOCl2、H2SO4、H2O2, chlordene metaantimmonic acid triethyl group oxygen, MoO3、
FeCl3、AuCl3、KMnO4In the combination of any one or more；
Or, described N-shaped doping reagent includes the combination of any one or more in hydrazine hydrate, ammonia, ethylenediamine.
7. according to the method improving carbon nanotube conductive film chemical doping stability according to any one of claim 1-4, its feature
Be: described can the material of the lower solidification that imposes a condition comprise in acrylic acid, polyurethane, silica column and epoxy resin arbitrary
Kind or two or more combinations.
The method of raising carbon nanotube conductive film chemical doping stability the most according to claim 1, it is characterised in that including:
At least select that drip washing, spraying, spin coating, blade coating, slit die head is extrusion coated, any one mode in nick printing will described be mixed
Close reagent, described doping reagent or described can be applied on carbon nanotube conductive film at the material of the lower solidification that imposes a condition.
The method of raising carbon nanotube conductive film chemical doping stability the most according to claim 1, it is characterised in that: described
The thickness of carbon nanotube conductive film is 2-1000nm, a length of 10-100 μm.
The method of raising carbon nanotube conductive film chemical doping stability the most according to claim 1, it is characterised in that described
Carbon nanotube conductive film covers in flexible transparent substrate, described flexible transparent substrate include PET substrate, PI substrate, PDMS substrate,
The combination of any one or more in PMMA substrate and PC substrate.
The method of 11. raising carbon nanotube conductive film chemical doping stability according to claim 1, it is characterised in that described
Protective layer used to intercept the active substance in environment and doping reagent reacting, its thickness is 0.01-1 μm.
The method of 12. raising carbon nanotube conductive film chemical doping stability according to claim 1, it is characterised in that described
CNT includes the combination of any one or more in SWCN, double-walled carbon nano-tube and multi-walled carbon nano-tubes.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106752383A (en) * | 2016-12-08 | 2017-05-31 | 广东轻工职业技术学院 | A kind of method that spray printing prepares solar battery thin film |
| CN113165877A (en) * | 2018-10-04 | 2021-07-23 | 伍兹有限责任公司 | Carbon nanotube product manufacturing system and manufacturing method thereof |
| CN114132918A (en) * | 2021-12-31 | 2022-03-04 | 西安交通大学 | Preparation method of mass-produced high-conductivity multi-walled carbon nanotube film material |
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| CN102224596A (en) * | 2008-06-09 | 2011-10-19 | 三星电子株式会社 | Improved cnt/topcoat processes for making a transplant conductor |
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| WO2008054472A2 (en) * | 2006-03-09 | 2008-05-08 | Battelle Memorial Institute | Methods of dispersing carbon nanotubes |
| CN102224596A (en) * | 2008-06-09 | 2011-10-19 | 三星电子株式会社 | Improved cnt/topcoat processes for making a transplant conductor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106752383A (en) * | 2016-12-08 | 2017-05-31 | 广东轻工职业技术学院 | A kind of method that spray printing prepares solar battery thin film |
| CN113165877A (en) * | 2018-10-04 | 2021-07-23 | 伍兹有限责任公司 | Carbon nanotube product manufacturing system and manufacturing method thereof |
| CN113165877B (en) * | 2018-10-04 | 2024-04-19 | 伍兹有限责任公司 | System and method for manufacturing carbon nanotube product |
| CN114132918A (en) * | 2021-12-31 | 2022-03-04 | 西安交通大学 | Preparation method of mass-produced high-conductivity multi-walled carbon nanotube film material |
| CN114132918B (en) * | 2021-12-31 | 2023-10-20 | 西安交通大学 | Preparation method of mass-produced high-conductivity multi-wall carbon nano tube film material |
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