CN107086085A - A kind of plasma graphene nano silver conductive film and its manufacture craft - Google Patents
A kind of plasma graphene nano silver conductive film and its manufacture craft Download PDFInfo
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- CN107086085A CN107086085A CN201710361846.1A CN201710361846A CN107086085A CN 107086085 A CN107086085 A CN 107086085A CN 201710361846 A CN201710361846 A CN 201710361846A CN 107086085 A CN107086085 A CN 107086085A
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Abstract
A kind of plasma graphene nano silver conductive film and its manufacture craft, are related to conductive membrane technology.A kind of manufacture craft of plasma graphene nano silver conductive film, including：Under conditions of pressure is 120 140Pa, using plasma reinforced chemical vapour deposition method by graphene nano deposition of silver in temperature on 340 360 DEG C of organic substrate.Temperature needed for plasma reinforced chemical vapour deposition method is low, sedimentation rate is fast；Last obtained plasma graphene nano silver conductive film quality is good, and pin hole is less, is not easily cracked.A kind of plasma graphene nano silver conductive film, is made by the manufacture craft of above-mentioned plasma graphene nano silver conductive film.The characteristics of it has pin hole less, is not easily cracked, and sheet resistance is low, conductance is high.
Description
Technical field
The present invention relates to conductive technical field of membrane, and more particularly to a kind of plasma graphene nano silver conductive film and its system
Make technique.
Background technology
Ito thin film is a kind of n-type semiconductor, and with higher conductance, high visible light permeable rate, high machinery is hard
Degree and good chemical stability, but ito thin film resource-constrained, in touch panel and transparent electrode for solar cell,
The ITO materials that graphene is limited as alternate resources, are also sent to great expectations.
Graphene is the hexagonal honeycomb construction formed by carbon atom, is a kind of quasi- two dimension of only one of which atomic layer level thickness
Material, the carrier mobility of graphene is very high, and is ITO preferable alternative materials with high intensity and pliability,
Also there is important application in terms of flexible conductive film material.Preparing grapheme conductive film at present mainly has two class methods：(1) lead to
Cross chemical vapour deposition technique and obtain single-layer graphene, be then transferred into transparent target substrate；(2) first obtained by chemical method
Graphene oxide solution, is then reduced again using masking technique in transparent target substrate after film forming.First method
The graphene film of preparation is easily damaged.Graphene film made from second method has more fault of construction, and resistance is higher.
The content of the invention
It is an object of the invention to provide a kind of manufacture craft of plasma graphene nano silver conductive film, plasma is utilized
It is low that enhancing chemical vapour deposition technique prepares temperature in plasma graphene nano silver conductive film, preparation process；Sedimentation rate is fast；Most
Obtained plasma graphene nano silver conductive film quality is good afterwards, and pin hole is less, is not easily cracked.
Another object of the present invention is to provide a kind of plasma graphene nano silver conductive film, it has pin hole less,
It is not easily cracked, and the characteristics of sheet resistance is low, conductance is high.
The present invention is solved its technical problem and realized using following technical scheme.
The present invention proposes a kind of manufacture craft of plasma graphene nano silver conductive film, including：
It is using plasma reinforced chemical vapour deposition method that graphene nano is silver-colored under conditions of pressure is 120-140Pa
It is deposited on the organic substrate that temperature is 200-260 DEG C.
The present invention also proposes a kind of plasma graphene nano silver conductive film, is led by above-mentioned plasma graphene nano silver
The manufacture craft of electrolemma is made.
The beneficial effect of the embodiment of the present invention is：In a kind of manufacture craft of plasma graphene nano silver conductive film, etc.
Plasma enhanced chemical vapor sedimentation is graphene nano silver is formed gas by microwave or radio frequency etc., and the gas is in local shape
Into plasma, plasma chemistry activity is very strong, the electronic impact that plasma high speed is moved to neutral reacting gas
Molecule, will become neutral reaction gas molecule and fragmentate or the state in activation easily reacts, and ultimately form a large amount of
The silver-colored molecule of the high graphene nano of activity；Finally deposit to formation plasma graphene nano silver conductive film on organic substrate.Deng
It is the graphene nano silver utilized in plasma enhanced chemical vapor sedimentation, graphene nano silver is overall, Nano Silver and graphite
Alkene is mutually merged, and Nano Silver adds the carrier concentration of graphene so that the conductive capability enhancing of graphene.Wherein, pressure
It is maintained at 120-140Pa, the temperature of substrate is maintained at 200-260 DEG C, and to can be obtained by good plasma graphene nano silver thin
Film.
A kind of plasma graphene nano silver conductive film, by the making work of above-mentioned plasma graphene nano silver conductive film
Skill is made.The characteristics of plasma graphene nano silver conductive film has pin hole less, is not easily cracked, and sheet resistance is low, conductance is high.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are the conventional production that can be obtained by commercially available purchase
Product.
A kind of plasma graphene nano silver conductive film and its manufacture craft of the embodiment of the present invention are carried out specifically below
Explanation.
A kind of manufacture craft of plasma graphene nano silver conductive film, including：
It is using plasma reinforced chemical vapour deposition method that graphene nano is silver-colored under conditions of pressure is 120-140Pa
It is deposited on the organic substrate that temperature is 200-260 DEG C.
Inventors herein have recognized that, graphene is coated on after being dried on organic substrate, then nano silver wire is coated on
Mode on organic substrate, because it plays the still nano silver wire of main conductive, its electric conductivity is not very good.And coating
The mode of (including spin coating, dip-coating, blade coating etc.) be difficult by graphene and nano silver wire it is uniform, be preferably coated on substrate, be coated with
Mode very likely cause the defect of conducting film.
Embodiments of the invention are using plasma reinforced chemical vapour deposition method by graphene nano deposition of silver in organic group
On piece.Plasma reinforced chemical vapour deposition method is graphene nano silver is formed gas, the gas by microwave or radio frequency etc.
Plasma is being partially formed, plasma chemistry activity is very strong, the electronic impact that plasma high speed is moved to neutrality
Reactant gas molecules, will become neutral reaction gas molecule and fragmentate or the state in activation easily reacts, finally
Form the silver-colored molecule of the high graphene nano of a large amount of activity；Formation plasma graphene nano silver on organic substrate is finally deposited to lead
Electrolemma, the conducting film, which is not required to be shifted again, can be used, and the basic zero defect of conducting film.Plasma reinforced chemical vapour deposition
It is the graphene nano silver utilized in method, graphene nano silver is overall, and Nano Silver is mutually merged with graphene, Nano Silver increase
The carrier concentration of graphene so that the conductive capability enhancing of graphene.Wherein, pressure is maintained at 120-140Pa, substrate
Temperature is maintained at 200-260 DEG C and can be obtained by good plasma graphene nano Ag films.In the present embodiment, substrate is selected
Select PET.In other embodiments, the material of substrate can be selected voluntarily as needed, and other transparent polyphosphazene polymers may be selected
Compound.Preferably, the temperature of substrate is 220-240 DEG C, and pressure is 130-135Pa.
In an embodiment of the present invention, graphene nano silver is mainly prepared by following methods：It is 2~4g by ratio:
1L graphene after being mixed with water ultrasonically treated 150-200min obtain the first mixed liquor；Sodium hydroxide solution is molten with silver nitrate
Ammoniacal liquor is instilled after liquid mixing until solution clarifies the sodium hydroxide and silver nitrate solution obtained in silver ammino solution, sodium hydroxide solution
In silver nitrate mass ratio be 0.5~1.5:3.It is 1 by mass ratio：10~15:220~300 tartaric acid, glucose and water
The second mixed liquor is mixed to get, the second mixed liquor is cooled to 25~30 after insulation 30-40min at a temperature of 100~120 DEG C
DEG C, the second mixed liquor and ethanol are then mixed to get the 3rd mixed liquor, the volume ratio of the second mixed liquor and ethanol is 1~8:
16.Silver ammino solution, the 3rd mixed liquor are carried out with the first mixed liquor successively to be blended in the ultrasound condition that power is 2000-3000W
Lower reaction 1-4min, is then filtered, is cleaned, is dried；The mol ratio of silver ammino solution and the 3rd mixed liquor is 1:1.1~1.3,
The mass ratio of silver nitrate and graphene is 1:0.5~2.Preferably, cleaning process is to carry out repeatedly alternating clearly using second alcohol and water
Wash.The temperature of drying course is 40-60 DEG C.
The preparation method of the graphene nano silver of the present embodiment will not destroy the structure of graphene, so as to keep excellent
Electric conductivity；And graphene and Nano Silver can be closely contacted, Nano Silver can also play its superior electric conductivity, most
Cause the electric conductivity enhancing of conducting film eventually.
In addition, in the present embodiment, graphene is mainly made by following preparation method：To 20- under 1-3 DEG C of water bath condition
The graphite powder of 1-1.1 parts by weight and the mixture of 0.5-0.55 parts by weight sodium nitrate are added in the 25mL concentrated sulfuric acid, then is slowly added
Enter the potassium permanganate reaction 100-150min of 2.9-3.1 parts by weight, then the water-bath 20-35min at a temperature of 35-40 DEG C
Obtain the 4th mixed liquor；75-82mL deionized water is added in the 4th mixed liquor, 28- is reacted at a temperature of 92-97 DEG C
33min；Then 60-62mL deionized water stopped reaction is added, the mass concentration for adding 14-15mL is more than 30% hydrogen peroxide
The mass concentration for reacting addition 38-42mL after 14-20min is 36%~38% hydrochloric acid solution；Then low-speed centrifugal is carried out to wash
Wash and remove excessive acid and accessory substance, the graphite oxide after washing is scattered in deionized water, after ultrasonically treated 40-45min
Add in hydrazine hydrate solution, 5-5.5h is reacted under 95-98 DEG C of water-bath conditional.
It is molten that graphite oxide after ultrasonically treated is easily dispersed into uniform single-layer graphene oxide in deionized water
Liquid, then it is reduced into graphene with hydration hydrazine reaction.Wherein, in an embodiment of the present invention, the mass concentration of hydrazine hydrate solution
For 76-82%.In addition, in an embodiment of the present invention, the granularity for preparing the graphite powder used in graphene is less than 30 μm, carbon content
For 99.85%；The mass concentration of the concentrated sulfuric acid is 95%~98%.
A kind of plasma graphene nano silver conductive film, by the making work of above-mentioned plasma graphene nano silver conductive film
Skill is made.The characteristics of it has pin hole less, is not easily cracked, and sheet resistance is low, conductance is high.
The feature and performance to the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of manufacture craft of plasma graphene nano silver conductive film, including：To 20mL's under 1 DEG C of water bath condition
The graphite powder of 1 parts by weight and the mixture of 0.52 parts by weight sodium nitrate are added in the concentrated sulfuric acid, the Gao Meng of 3 parts by weight is slow added into
Sour nak response 100min, then water-bath 20min obtains the 4th mixed liquor at a temperature of 40 DEG C；Add in the 4th mixed liquor
Enter 82mL deionized water, 33min is reacted at a temperature of 92 DEG C；Then 62mL deionized water stopped reaction is added, is added
The hydrochloric acid solution that the mass concentration that 15mL mass concentration is more than addition 42mL after 30% hydrogen peroxide reaction 14min is 37%；
Then carry out low-speed centrifugal washing and remove excessive acid and accessory substance, the graphite oxide after washing is scattered in deionized water,
Added after ultrasonically treated 40min in hydrazine hydrate solution, 5.2h is reacted under 95 DEG C of water-bath conditional and obtains graphene.
It is 4g by ratio:1L graphene after being mixed with water ultrasonically treated 150min obtain the first mixed liquor；By hydroxide
Sodium solution instills ammoniacal liquor until solution clarifies the hydrogen-oxygen obtained in silver ammino solution, sodium hydroxide solution after being mixed with silver nitrate solution
The mass ratio for changing sodium and the silver nitrate in silver nitrate solution is 1:2.It is 1 by mass ratio：15:300 tartaric acid, glucose and water
The second mixed liquor is mixed to get, 28 DEG C are cooled to after the second mixed liquor is incubated into 40min at a temperature of 120 DEG C, then by the
Two mixed liquors and ethanol are mixed to get the 3rd mixed liquor, and the volume ratio of the second mixed liquor and ethanol is 1:16.By silver ammino solution,
Three mixed liquors carry out being blended under the ultrasound condition that power is 2000W successively with the first mixed liquor reacts 4min, then carries out
Filter, using second alcohol and water carry out 5 alternately cleaning, at a temperature of 45 DEG C drying obtain graphene nano silver.Wherein, silver ammino solution with
The mol ratio of 3rd mixed liquor is 1:1.1, the mass ratio of silver nitrate and graphene is 1:1.5.
Under conditions of pressure is 125Pa, using plasma reinforced chemical vapour deposition method by graphene nano deposition of silver
In temperature on 240 DEG C of PET substrates.
A kind of plasma graphene nano silver conductive film, is made by above-mentioned manufacture craft.
Embodiment 2
A kind of manufacture craft of plasma graphene nano silver conductive film, including：To 20mL's under 2 DEG C of water bath condition
The graphite powder of 1 parts by weight and the mixture of 0.52 parts by weight sodium nitrate are added in the concentrated sulfuric acid, the height of 2.9 parts by weight is slow added into
Mangaic acid nak response 120min, then water-bath 25min obtains the 4th mixed liquor at a temperature of 35 DEG C；In the 4th mixed liquor
75mL deionized water is added, 30min is reacted at a temperature of 93 DEG C；Then 60mL deionized water stopped reaction is added, plus
The hydrochloric acid that the mass concentration for entering to add 38mL after hydrogen peroxide reaction 15min of the 15mL mass concentration more than 30% is 36% is molten
Liquid；Then carry out low-speed centrifugal washing and remove excessive acid and accessory substance, the graphite oxide after washing is scattered in deionized water
In, added after ultrasonically treated 42min in hydrazine hydrate solution, 5h is reacted under 95 DEG C of water-bath conditional and obtains graphene.
It is 2g by ratio:1L graphene after being mixed with water ultrasonically treated 160min obtain the first mixed liquor；By hydroxide
Sodium solution instills ammoniacal liquor until solution clarifies the hydrogen-oxygen obtained in silver ammino solution, sodium hydroxide solution after being mixed with silver nitrate solution
The mass ratio for changing sodium and the silver nitrate in silver nitrate solution is 1:3.It is 1 by mass ratio：11:250 tartaric acid, glucose and water
The second mixed liquor is mixed to get, 25 DEG C are cooled to after the second mixed liquor is incubated into 32min at a temperature of 100 DEG C, then by the
Two mixed liquors and ethanol are mixed to get the 3rd mixed liquor, and the volume ratio of the second mixed liquor and ethanol is 3:16.By silver ammino solution,
Three mixed liquors carry out being blended under the ultrasound condition that power is 2300W successively with the first mixed liquor reacts 4min, then carries out
Filter, using second alcohol and water carry out 7 alternately cleaning, at a temperature of 60 DEG C drying obtain graphene nano silver.Wherein, silver ammino solution with
The mol ratio of 3rd mixed liquor is 1:1.2, the mass ratio of silver nitrate and graphene is 1:1.
Under conditions of pressure is 120Pa, using plasma reinforced chemical vapour deposition method by graphene nano deposition of silver
In temperature on 220 DEG C of PET substrates.
A kind of plasma graphene nano silver conductive film, is made by above-mentioned manufacture craft.
Embodiment 3
A kind of manufacture craft of plasma graphene nano silver conductive film, including：To 25mL's under 3 DEG C of water bath condition
The graphite powder of 1.1 parts by weight and the mixture of 0.55 parts by weight sodium nitrate are added in the concentrated sulfuric acid, 3.1 parts by weight are slow added into
Potassium permanganate reacts 150min, and then water-bath 28min obtains the 4th mixed liquor at a temperature of 35 DEG C；In the 4th mixed liquor
Middle addition 78mL deionized water, 28min is reacted at a temperature of 95 DEG C；Then 60mL deionized water stopped reaction is added,
The mass concentration for adding addition 40mL after hydrogen peroxide reaction 16min of the 14mL mass concentration more than 30% is molten for 38% hydrochloric acid
Liquid；Then carry out low-speed centrifugal washing and remove excessive acid and accessory substance, the graphite oxide after washing is scattered in deionized water
In, added after ultrasonically treated 44min in hydrazine hydrate solution, 5.5h is reacted under 95 DEG C of water-bath conditional and obtains graphene.
It is 3g by ratio:1L graphene after being mixed with water ultrasonically treated 200min obtain the first mixed liquor；By hydroxide
Sodium solution instills ammoniacal liquor until solution clarifies the hydrogen-oxygen obtained in silver ammino solution, sodium hydroxide solution after being mixed with silver nitrate solution
The mass ratio for changing sodium and the silver nitrate in silver nitrate solution is 0.5:3.It is 1 by mass ratio：10:220 tartaric acid, glucose with
Water is mixed to get the second mixed liquor, and the second mixed liquor is cooled into 30 DEG C after insulation 30min at a temperature of 110 DEG C, then will
Second mixed liquor and ethanol are mixed to get the 3rd mixed liquor, and the volume ratio of the second mixed liquor and ethanol is 3:8.By silver ammino solution,
3rd mixed liquor carries out being blended under the ultrasound condition that power is 2500W successively with the first mixed liquor reacts 3min, then carries out
Filtering, using second alcohol and water carry out 9 alternately cleaning, at a temperature of 40 DEG C drying obtain graphene nano silver.Wherein, silver ammino solution
Mol ratio with the 3rd mixed liquor is 1:1.3, the mass ratio of silver nitrate and graphene is 2:1.
Under conditions of pressure is 130Pa, using plasma reinforced chemical vapour deposition method by graphene nano deposition of silver
In temperature on 260 DEG C of PET substrates.
A kind of plasma graphene nano silver conductive film, is made by above-mentioned manufacture craft.
Embodiment 4
A kind of manufacture craft of plasma graphene nano silver conductive film, including：To 23mL's under 3 DEG C of water bath condition
The graphite powder of 1 parts by weight and the mixture of 0.5 parts by weight sodium nitrate are added in the concentrated sulfuric acid, the Gao Meng of 3 parts by weight is slow added into
Sour nak response 140min, then water-bath 35min obtains the 4th mixed liquor at a temperature of 35 DEG C；Add in the 4th mixed liquor
Enter 80mL deionized water, 30min is reacted at a temperature of 97 DEG C；Then 60mL deionized water stopped reaction is added, is added
The hydrochloric acid solution that the mass concentration that 15mL mass concentration is more than addition 39mL after 30% hydrogen peroxide reaction 20min is 36%；
Then carry out low-speed centrifugal washing and remove excessive acid and accessory substance, the graphite oxide after washing is scattered in deionized water,
Added after ultrasonically treated 40min in hydrazine hydrate solution, 5.3h is reacted under 98 DEG C of water-bath conditional and obtains graphene.
It is 3g by ratio:1L graphene after being mixed with water ultrasonically treated 180min obtain the first mixed liquor；By hydroxide
Sodium solution instills ammoniacal liquor until solution clarifies the hydrogen-oxygen obtained in silver ammino solution, sodium hydroxide solution after being mixed with silver nitrate solution
The mass ratio for changing sodium and the silver nitrate in silver nitrate solution is 1:3.It is 1 by mass ratio：10:300 tartaric acid, glucose and water
The second mixed liquor is mixed to get, 27 DEG C are cooled to after the second mixed liquor is incubated into 36min at a temperature of 110 DEG C, then by the
Two mixed liquors and ethanol are mixed to get the 3rd mixed liquor, and the volume ratio of the second mixed liquor and ethanol is 1:2.By silver ammino solution,
Three mixed liquors carry out being blended under the ultrasound condition that power is 3000W successively with the first mixed liquor reacts 1min, then carries out
Filter, using second alcohol and water carry out 10 alternately cleaning, at a temperature of 50 DEG C drying obtain graphene nano silver.Wherein, silver ammino solution
Mol ratio with the 3rd mixed liquor is 1:1.1, the mass ratio of silver nitrate and graphene is 1:2.
Under conditions of pressure is 140Pa, using plasma reinforced chemical vapour deposition method by graphene nano deposition of silver
In temperature on 200 DEG C of PET substrates.
A kind of plasma graphene nano silver conductive film, is made by above-mentioned manufacture craft.
Embodiment 5
A kind of manufacture craft of plasma graphene nano silver conductive film, including：To 23mL's under 3 DEG C of water bath condition
The graphite powder of 1 parts by weight and the mixture of 0.54 parts by weight sodium nitrate are added in the concentrated sulfuric acid, the Gao Meng of 3 parts by weight is slow added into
Sour nak response 120min, then water-bath 32min obtains the 4th mixed liquor at a temperature of 36 DEG C；Add in the 4th mixed liquor
Enter 77mL deionized water, 30min is reacted at a temperature of 96 DEG C；Then 60mL deionized water stopped reaction is added, is added
The hydrochloric acid solution that the mass concentration that 15mL mass concentration is more than addition 38mL after 30% hydrogen peroxide reaction 16min is 37%；
Then carry out low-speed centrifugal washing and remove excessive acid and accessory substance, the graphite oxide after washing is scattered in deionized water,
Added after ultrasonically treated 45min in hydrazine hydrate solution, 5.2h is reacted under 96 DEG C of water-bath conditional and obtains graphene.
It is 2g by ratio:1L graphene after being mixed with water ultrasonically treated 160min obtain the first mixed liquor；By hydroxide
Sodium solution instills ammoniacal liquor until solution clarifies the hydrogen-oxygen obtained in silver ammino solution, sodium hydroxide solution after being mixed with silver nitrate solution
The mass ratio for changing sodium and the silver nitrate in silver nitrate solution is 1.3:3.It is 1 by mass ratio：12:280 tartaric acid, glucose with
Water is mixed to get the second mixed liquor, and the second mixed liquor is cooled into 28 DEG C after insulation 38min at a temperature of 120 DEG C, then will
Second mixed liquor and ethanol are mixed to get the 3rd mixed liquor, and the volume ratio of the second mixed liquor and ethanol is 5:16.By silver ammino solution,
3rd mixed liquor carries out being blended under the ultrasound condition that power is 2800W successively with the first mixed liquor reacts 2min, then carries out
Filtering, using second alcohol and water carry out 4 alternately cleaning, at a temperature of 55 DEG C drying obtain graphene nano silver.Wherein, silver ammino solution
Mol ratio with the 3rd mixed liquor is 1:1.1, the mass ratio of silver nitrate and graphene is 1:1.2.
Under conditions of pressure is 130Pa, using plasma reinforced chemical vapour deposition method by graphene nano deposition of silver
In temperature on 250 DEG C of PET substrates.
A kind of plasma graphene nano silver conductive film, is made by above-mentioned manufacture craft.
Test example
1. sheet resistance：The sheet resistance of embodiment 1-5 plasma graphene nano silver conductive film is surveyed using four probe method
Examination, its result is recorded in table 1.
2. light transmittance：Embodiment 1-5 plasma graphene nano silver conductive film is existed using spectrophotometer measurement
Light transmittance at 550nm wavelength is tested, and its result is recorded in table 1.
The performance test of the embodiment 1-5 of table 1 plasma graphene nano silver conductive film
It can be drawn from the data of table 1, the sheet resistance of embodiment 1-5 plasma graphene nano silver conductive film is smaller,
Its conductive capability is preferable；And light transmittance is all higher than 90%, light transmittance is preferable.Illustrate, the plasma graphite of the embodiment of the present invention
Alkene nano-silver conductive film production technique can prepare the plasma graphene nano silver conductive film that conductive capability is good, performance is excellent.
In summary, a kind of plasma graphene nano silver conductive film and its manufacture craft of the embodiment of the present invention, wait from
In the manufacture craft of sub- graphene nano silver conductive film, plasma reinforced chemical vapour deposition method is made by microwave or radio frequency etc.
Graphene nano silver forms gas, and the gas is being partially formed plasma, and plasma chemistry activity is very strong, in plasma
The electronic impact of high-speed motion will become neutral reaction gas molecule and fragmentate or in sharp to neutral reactant gas molecules
State living easily reacts, and ultimately forms the silver-colored molecule of the high graphene nano of a large amount of activity；Finally deposit to organic substrate
Upper formation plasma graphene nano silver conductive film.It is the graphene nano utilized in plasma reinforced chemical vapour deposition method
Silver, graphene nano silver is overall, and Nano Silver is mutually merged with graphene, and Nano Silver adds the carrier concentration of graphene,
So that the conductive capability enhancing of graphene.Wherein, pressure is maintained at 120-140Pa, and the temperature of substrate is maintained at 200-260 DEG C just
Good plasma graphene nano Ag films can be obtained.
A kind of plasma graphene nano silver conductive film, by the making work of above-mentioned plasma graphene nano silver conductive film
Skill is made.The characteristics of plasma graphene nano silver conductive film has pin hole less, is not easily cracked, and sheet resistance is low, conductance is high.
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of manufacture craft of plasma graphene nano silver conductive film, it is characterised in that including：
Under conditions of pressure is 120-140Pa, using plasma reinforced chemical vapour deposition method by graphene nano deposition of silver
In temperature on 200-260 DEG C of organic substrate.
2. the manufacture craft of plasma graphene nano silver conductive film according to claim 1, it is characterised in that the temperature
Spend for 220-240 DEG C.
3. the manufacture craft of plasma graphene nano silver conductive film according to claim 1, it is characterised in that the pressure
It is 130-135Pa by force.
4. the manufacture craft of plasma graphene nano silver conductive film according to claim 1, it is characterised in that the stone
Black alkene Nano Silver is mainly prepared by following methods：
It is 2~4g by ratio:1L graphene after being mixed with water ultrasonically treated 150-200min obtain the first mixed liquor；By hydrogen-oxygen
Change and instill ammoniacal liquor after sodium solution is mixed with silver nitrate solution until solution clarification is obtained in silver ammino solution, the sodium hydroxide solution
Sodium hydroxide and the silver nitrate solution in the mass ratio of silver nitrate be 0.5~1.5:3；
It is 1 by mass ratio：10~15:220~300 tartaric acid, glucose and water is mixed to get the second mixed liquor, by described
Two mixed liquors are cooled to 25~30 DEG C after insulation 30-40min at a temperature of 100~120 DEG C, then by second mixed liquor
The 3rd mixed liquor is mixed to get with ethanol, the volume ratio of second mixed liquor and ethanol is 1~8:16；
The silver ammino solution, the 3rd mixed liquor with first mixed liquor be blended in power for 2000- successively
1-4min is reacted under 3000W ultrasound condition, is then filtered, cleaned, dried；The silver ammino solution is mixed with the described 3rd
The mol ratio of liquid is 1:1.1~1.3, the mass ratio of the silver nitrate and the graphene is 1:0.5~2.
5. the manufacture craft of plasma graphene nano silver conductive film according to claim 4, it is characterised in that described clear
The process washed is to carry out repeatedly alternately cleaning using second alcohol and water.
6. the manufacture craft of plasma graphene nano silver conductive film according to claim 4, it is characterised in that the baking
The temperature of dry process is 40-60 DEG C.
7. the manufacture craft of plasma graphene nano silver conductive film according to claim 4, it is characterised in that the stone
Black alkene is mainly made by following preparation method：1-1.1 weights are added into the 20-25mL concentrated sulfuric acid under 1-3 DEG C of water bath condition
The graphite powder of part and the mixture of 0.5-0.55 parts by weight sodium nitrate are measured, the potassium permanganate of 2.9-3.1 parts by weight is slow added into
100-150min is reacted, then water-bath 20-35min obtains the 4th mixed liquor at a temperature of 35-40 DEG C；The described 4th
75-82mL deionized water is added in mixed liquor, 28-33min is reacted at a temperature of 92-97 DEG C；Then add 60-62mL's
Deionized water stopped reaction, 38- is added after adding hydrogen peroxide reaction 14-20min of the 14-15mL mass concentration more than 30%
42mL mass concentration is 36%~38% hydrochloric acid solution；Then carry out low-speed centrifugal washing and remove excessive acid and by-product
Thing, the graphite oxide after washing is scattered in deionized water, is added after ultrasonically treated 40-45min in hydrazine hydrate solution,
5-5.5h is reacted under 95-98 DEG C of water-bath conditional.
8. the manufacture craft of plasma graphene nano silver conductive film according to claim 7, it is characterised in that the stone
The granularity of ink powder is less than 30 μm.
9. the manufacture craft of plasma graphene nano silver conductive film according to claim 7, it is characterised in that the water
The mass concentration for closing hydrazine solution is 76-82%.
10. a kind of plasma graphene nano silver conductive film, it is characterised in that as the grade described in claim any one of 1-9 from
The manufacture craft of sub- graphene nano silver conductive film is made.
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