CN103903819A - Preparation method of flexible transparent conducting film - Google Patents
Preparation method of flexible transparent conducting film Download PDFInfo
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- CN103903819A CN103903819A CN201410149296.3A CN201410149296A CN103903819A CN 103903819 A CN103903819 A CN 103903819A CN 201410149296 A CN201410149296 A CN 201410149296A CN 103903819 A CN103903819 A CN 103903819A
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Abstract
The invention discloses a preparation method of a flexible transparent conducting film. According to the method, LDPE power dissolves in dimethylbenzene, and the LDPE is fully dissolved through magnetic stirring; CNTs is added, the diameter of the CNTs is less than 80 nm, the length of the CNTs ranges from 0.5 mum to 30 mum, dispersing is conducted by the adoption of dodecyl benzene, ultrasonic dispersing is conducted after the magnetic stirring, hot pressing of 4 Mpa to 10 Mpa is conducted, and a thick film product with the thickness of 20 mum to 50 mum is acquired. The carbon nanotube/polyethylene flexible transparent conducting film prepared by the adoption of the method has higher conductibility and good optical property, the volume conductivity can reach 4.68*10<-3>S*m<-1>, the transmittance can reach 62.8%, and the flexible transparent conducting film is suitable for the fields of transparent anti-static films, transparent electrodes, transparent printed circuit boards, touch screens, digital displays, electric windscreens and the like.
Description
Technical field
The present invention relates to the technology of preparing of flexible transparent conducting film, particularly a kind of preparation method of carbon nano-tube/poly ethene flexible transparent conducting film.
Background technology
Transparent conductive material is the novel multifunctional material of a class, and it had both had good optical property, also has higher conductivity.Therefore, they are widely used in the fields such as electromagnetic shielding (transparent anti static film), optoelectronic information (transparency electrode, transparent printed substrate, touch-screen, numeral show), agriculture fishery greenhouse lighting (printing opacity Electric radiant Heating Film), building (transparent area heater), automobile (conduction windscreen).
At present, common transparent conductive material mainly comprises the electro-conductive glass take ITO as representative and the transparent conductive film take zinc oxide as main material.Among nesa coating highly conductive and transparent, but they there is lower frictional resistance and shock resistance poor, main material used is very expensive, and adopt be very complicated magnetron sputtering preparation process.
Flexible transparent conducting film has a series of other type transparent conductive materials and is difficult to alternative advantage.First, compare with zinc-oxide film with electro-conductive glass, it has following advantage:
(1) shock resistance is superior.Due to good pliability, make this class material more safe and reliable in the time of application, and can be reduced in the damage in construction transportation, save cost;
(2) machine-shaping is easy, light;
(3) cost of raw material is not high;
(4) processing cost of material is far below electro-conductive glass and the conventional magnetron sputtering of zinc-oxide film, more energy-conservation aborning.
Conventionally, flexible conductive film is in polymeric matrix, to add conductive filler and the conductive plastics film made, and according to the difference of conductive filler, flexible conductive film can be divided into metal filled series and material with carbon element is filled series.
In order to realize the conductivity that composite conductive film is higher, the loading of required metal-powder or carbon black, graphite large (general volume ratio is 10%～40%), this can cause its mechanical property to have reduction in various degree (pliability decline, become fragile and frangible) on the one hand; On the other hand, this can cause the transparency of film very low (almost cannot printing opacity).Therefore, larger conductive filler content can have influence on the practical application of flexible conductive film and limit their possibilities as nesa coating.
Summary of the invention
The object of the present invention is to provide one to prepare the method for carbon nano-tube (CNTs)/polyethylene flexible transparent conducting film, this flexible transparent conducting film has larger volume conductance and higher visible light transmittance rate, is applicable to preparing transparency electrode or the antireflective coating of solar cell.
The preparation method of a kind of flexible transparent conducting film provided by the invention, is characterized in that, the method comprises the steps:
The 1st step is dissolved in LDPE powder in paraxylene, and magnetic agitation is fully dissolved LDPE;
The 2nd step is according to LDPE-xwt%CNTs formula, and in formula, 0.1 < x≤1, is placed in solution prepared by the 1st step by CNTs and obtains dispersion liquid, and wherein the diameter of CNTs is less than 80nm, and length is 0.5 μ m～30 μ m;
The 3rd step is dissolved in neopelex in solution prepared by the 2nd step, CNTs is effectively disperseed, with volume conductance and visible light transmittance rate;
The 4th step dispersion liquid that at normal temperatures prepared by magnetic agitation the 3rd step, disperses CNTs completely;
The ultrasonic dispersion of dispersion liquid 2h～6h that the 5th step is prepared the 4th step, fully disperses CNTs;
The solution that the 6th step is prepared the 5th step is placed in glass horizontal container, is placed in vacuum drying chamber, at 80～110 ℃, is dried, and makes solvent evaporates, obtains the thick thick film initial sample of 20 μ m～50 μ m;
The initial thick film sample that the 7th step obtains the 6th step, is placed in hot pressing die, carries out hot pressing at 110～120 ℃, and pressure is 4MPa～10MPa, obtains the thick final thick film products of 20 μ m～50 μ m; Hot pressing makes thick film products finer and close, is not affecting under the prerequisite of light transmittance, and its conductivity is further improved.
Carbon nano-tube/poly ethene flexible transparent conducting film prepared by the present invention has higher conductivity and good optical property, its volume conductance can reach 4.68 × 10-3Sm-1, light transmittance can reach 62.8%, is suitable for the fields such as transparent anti static film, transparency electrode, transparent printed substrate, touch-screen, numeral demonstration and conduction windscreen.
Accompanying drawing explanation
Fig. 1 is the process chart that the present invention prepares carbon nano-tube/poly ethene flexible transparent conducting film;
In order to contain 0.9wt%CNTs, (diameter is less than 8nm to Fig. 2, and length 10～30 μ are the FSEM figure of nesa coating m);
In order to contain 0.9wt%CNTs, (diameter is less than 8nm to Fig. 3, the m) translucent effect of nesa coating of length 10～30 μ;
Fig. 4 is for containing 0.8wt%CNTs (diameter 8～30nm, the m) translucent effect of nesa coating of length 10～30 μ;
Fig. 5 is for containing 0.5wt%CNTs (diameter 30～80nm, the m) translucent effect of nesa coating of length 10～30 μ;
In order to contain 0.9wt%CNTs, (diameter is less than 8nm to Fig. 6, the m) translucent effect of nesa coating of length 0.5～10 μ.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described further.It should be noted that at this, be used for helping to understand the present invention for the explanation of these execution modes, but do not form limitation of the invention.In addition,, in each execution mode of described the present invention, involved technical characterictic just can combine mutually as long as do not form each other conflict.
The preparation method that example of the present invention provides comprises:
(1) take the LDPE powder of certain mass, measure the paraxylene of certain volume, LDPE powder is dissolved in paraxylene, adopt magnetic stirring equipment, stir 0.5-2h, LDPE is fully dissolved;
Wherein, the mass ratio of LDPE and paraxylene is preferably 1: 1 to 1: 2.
(2) according to LDPE-x%CNTs formula, in formula, 0.1≤x≤1, takes the CNTs of certain mass, different-shape, and wherein the diameter of CNTs is less than 80nm, and length is 0.5～30 μ m, is placed in the solution of step (1) preparation;
(3) take the neopelex of certain mass, its quality is CNTs 4.5～5.5 times.Neopelex is the dispersant of CNTs, can make CNTs effectively disperse, and improves volume conductance and visible light transmittance rate.The neopelex taking is dissolved in the dispersion liquid that step (2) obtains;
(4) dispersion liquid of being prepared by step (3) adopts magnetic stirring equipment at normal temperatures, stirs 0.5-2h, and CNTs is disperseed;
(5) the ultrasonic dispersion 2～6h of dispersion liquid being prepared by step (4), fully disperses CNTs;
(6) solution of being prepared by step (5) is placed in glass horizontal container, is placed in vacuum drying chamber, under 80～110 degree, is dried, and makes solvent evaporates, obtains the thick film initial sample that 20～50 μ m are thick;
(7) get the thick film initial sample in step (6), be placed in hot pressing die, carry out hot pressing under 110-120 degree, pressure is 4～10MPa, obtains the thick film final products that 20～50 μ m are thick.Heat pressing process can make thick film products finer and close, is not affecting under the prerequisite of light transmittance, and product conductivity is further improved;
(8) get the thick film products in step (7), cut into piece, surperficial evaporation Pt electrode, carries out the measurement of conductivity;
(9) get the product in step (7), carry out the measurement of visible light transmittance rate.
The present invention, by changing mass fraction and the pattern of CNTs, sums up good formula.
Example:
Example 1:
Adopt solution casting blending technology, take the LDPE powder of certain mass, be dissolved in paraxylene solvent, stir 1h, LDPE is fully dissolved, according to LDPE-0.9%CNTs formula, take the CNTs of certain mass, wherein the diameter of CNTs is for being less than 8nm, length is 10～30 μ m, take the neopelex of certain mass, its quality is 5 times of CNTs, add in dispersion liquid, dispersion liquid is adopted to magnetic stirring equipment at normal temperatures, stir 1h, CNTs is disperseed, again by the ultrasonic dispersion of the dispersion liquid 4h of preparation, CNTs is fully disperseed, finally by dispersion liquid as in 5cm*5cm glass horizontal container, be positioned in vacuum drying chamber, under 100 degree, be dried, make solvent evaporates, obtain the thick film sample that 30 μ m are thick, sample is placed in to hot pressing die, under 115 degree, carry out hot pressing, pressure is 7MPa, obtain the final thick film products that 30 μ m are thick, product is cut into 10mm*10mm square, carry out the measurement of visible light transmittance rate, and by product surface evaporation Pt electrode, carry out the measurement of conductivity, example 1 combination property the best, its volume conductance is 4.68 × 10-3Sm-1, light transmittance is 62.8%, its FSEM as shown in Figure 2, translucent effect as shown in Figure 3.
Example 2-6:
Adopt solution casting blending technology, according to formula LDPE-x%CNTs proportioning dispersion liquid, wherein the diameter of CNTs is for being less than 8nm, and length is 10～30 μ m, x=0.1, and 0.4,0.5,0.7,1, as table 1, all the other are with example 1.Its performance is in table 2.
Table 1
Table 2
Example 7-12: adopt solution casting blending technology, according to formula LDPE-x%CNTs proportioning dispersion liquid, wherein the diameter of CNTs is 8～30nm, and length is 10～30 μ m, x=0.1,0.3,0.5,0.6,0.7,0.8, as table 3, all the other are with example 1.Its performance is in table 4, wherein example 11 combination property the bests, and translucent effect is as shown in Figure 4.
Table 3
Table 4
Example 13-18: adopt solution casting blending technology, according to formula LDPE-x%CNTs proportioning dispersion liquid, wherein the diameter of CNTs is 30～80nm, and length is 10～30 μ m, x=0.1,0.2,0.3,0.4,0.5,0.6, as table 5, all the other are with example 1.Its performance is in table 6, wherein example 17 combination property the bests, and translucent effect is as shown in Figure 5.
Table 5
Table 6
Example 19-24: adopt solution casting blending technology, according to formula LDPE-x%CNTs proportioning dispersion liquid, wherein the diameter of CNTs is for being less than 8nm, and length is 0.5～10 μ m, x=0.3,0.6,0.7,0.8,0.9,1.0, as table 7, all the other are with example 1.Its performance is in table 8, wherein example 23 combination property the bests, and translucent effect is as shown in Figure 6.
Table 7
Table 8
The above is preferred embodiment of the present invention, but the present invention should not be confined to the disclosed content of this embodiment and accompanying drawing.Do not depart from the equivalence completing under spirit disclosed in this invention so every or revise, all falling into the scope of protection of the invention.
Claims (2)
1. a preparation method for flexible transparent conducting film, is characterized in that, the method comprises the steps:
The 1st step is dissolved in LDPE powder in paraxylene, and magnetic agitation is fully dissolved LDPE;
The 2nd step is according to LDPE-xwt%CNTs formula, and in formula, 0.1 < x≤1, is placed in solution prepared by the 1st step by CNTs and obtains dispersion liquid, and wherein the diameter of CNTs is less than 80nm, and length is 0.5 μ m～30 μ m;
The 3rd step is dissolved in neopelex in solution prepared by the 2nd step, CNTs is effectively disperseed, with volume conductance and visible light transmittance rate;
The 4th step dispersion liquid that at normal temperatures prepared by magnetic agitation the 3rd step, disperses CNTs completely;
The ultrasonic dispersion of dispersion liquid 2h～6h that the 5th step is prepared the 4th step, fully disperses CNTs;
The solution that the 6th step is prepared the 5th step is placed in horizontal vessel, and vacuumize at 80～110 ℃, makes solvent evaporates, obtains the thick thick film initial sample of 20 μ m～50 μ m;
The initial thick film products that the 7th step obtains the 6th step, is placed in hot pressing die, carries out hot pressing at 110～120 ℃, and pressure is 4MPa～10MPa, obtains the thick final thick film products of 20 μ m～50 μ m; Hot pressing makes thick film products finer and close, is not affecting under the prerequisite of light transmittance, and its conductivity is further improved.
2. the preparation method of flexible transparent conducting film according to claim 1, is characterized in that, in the 1st step, the mass ratio of LDPE and paraxylene is preferably 1: 1 to 1: 2.
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| CN104851515A (en) * | 2014-12-31 | 2015-08-19 | 东莞市纳利光学材料有限公司 | Preparation method for conductive film |
| CN107964178A (en) * | 2017-12-05 | 2018-04-27 | 无锡盛雅生物科技有限公司佛山分公司 | A kind of preparation method of conductive film |
| CN109971018A (en) * | 2019-04-04 | 2019-07-05 | 陕西师范大学 | A kind of composite and flexible resistive film, preparation method and its application |
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| CN107964178A (en) * | 2017-12-05 | 2018-04-27 | 无锡盛雅生物科技有限公司佛山分公司 | A kind of preparation method of conductive film |
| CN109971018A (en) * | 2019-04-04 | 2019-07-05 | 陕西师范大学 | A kind of composite and flexible resistive film, preparation method and its application |
| CN109971018B (en) * | 2019-04-04 | 2020-09-11 | 陕西师范大学 | Composite flexible resistive film, preparation method and application thereof |
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Application publication date: 20140702 |