CN106554660A - A kind of method that inkjet printing prepares carbon nanotube conductive thin film - Google Patents
A kind of method that inkjet printing prepares carbon nanotube conductive thin film Download PDFInfo
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- CN106554660A CN106554660A CN201611118411.6A CN201611118411A CN106554660A CN 106554660 A CN106554660 A CN 106554660A CN 201611118411 A CN201611118411 A CN 201611118411A CN 106554660 A CN106554660 A CN 106554660A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/324—Inkjet printing inks characterised by colouring agents containing carbon black
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention discloses a kind of method that inkjet printing prepares carbon nanotube conductive thin film, CNT can uniformly be disperseed in finished product ink after modification by the present invention, effectively reduce reunion, CNT has good electric conductivity simultaneously, can be very good to improve ink jet ink electrical conductivity of water, improve the electric conductivity of finished films, the ink-jet ink good stability of the present invention, adopt the alcoholic solution of naphthenic soap effectively improve the viscosity and mobility of ink for viscosity-controlling agent, improve the stability on thin film after ink-jet.
Description
Technical field
The invention mainly relates to inkjet printing field, more particularly to a kind of inkjet printing prepares carbon nanotube conductive thin film
Method.
Background technology
The methods such as the method for making at present thin film includes sputtering, is deposited with, silk-screen, spin coating, blade coating, coating and inkjet printing,
High cost is wherein sputtered and is deposited with, silk-screen thickness and precision are bad controllable, and spin coating is unsuitable for large-scale production, coating and ink-jet
Printing is applicable in low cost, continuous, large-area scale industrial production.Compared with coating, the thickness of inkjet printing and
Position control is accurate, with micrometer resolution, is capable of achieving digital images outputting, can be flexible to the course of processing by computer
High-precision control;
On CNT, the P of carbon atom electronically forms large-scale delocalized pi-bond, and due to conjugation significantly, CNT has
Some special electrical properties, CNT have good electric conductivity, due to the lamella of the structure and graphite of CNT
Structure is identical, so having good electric property.Its electric conductivity of theoretical prediction is depending on its caliber and the helical angle of tube wall.
When the caliber of CNT is more than 6nm, electric conductivity declines;When caliber is less than 6nm, CNT can be seen as to be had
The One-dimensional Quantum wire of excellent conductive performance.It was reported that by calculating, Huang thinks that the CNT of a diameter of 0.7nm has
Superconductivity, although its superconducting transition temperature only has 1.5 × 10-4K, imply that CNT is front in the application of superconductivity
Scape.
The content of the invention
The object of the invention is exactly for the defect for making up prior art, there is provided a kind of inkjet printing prepares carbon nanotube conducting
The method of thin film.
The present invention is achieved by the following technical solutions:
A kind of method that inkjet printing prepares carbon nanotube conductive thin film, comprises the following steps:
(1)The preparation of ink-jet ink:Described ink-jet ink is made up of the raw material of following weight parts:
CNT 57-60, naphthenic soap 1-2, the tert-butyl group are to biphenol 0.4-1, N-Methyl pyrrolidone 36-40, dialkyl group
Zinc dithiophosphate 1-2, zirconium carbonate ammonium 3-5, oleamide 1-2, abienol 3-4, stannous sulfide 0.1-0.3, water and Firebrake ZB
2-3, calcium ricinoleate 0.5-1, polyurethanes 2-3, alkenyl succinic anhydride 0.8-1, tetrakis hydroxymetyl phosphonium sulfuric 1-2, hexadecane
Base trimethyl ammonium chloride 0.8-1, Sodium fluoroborate 1-2, sodium laurylsulfate 0.5-1, appropriate dehydrated alcohol;
The preparation method of described ink-jet ink is comprised the following steps:
A, above-mentioned CNT is added to mass ratio for 3-4:In 1 sulphuric acid, the mixed solution of nitric acid, described sulfuric acid concentration
For 95-97%, described concentration of nitric acid is 96-98%, is sent in reactor, and the ultrasound 3-5 hours at 100-120 DEG C are filtered, will
Precipitation washing 3-4 time, is vacuum dried 1-2 hours at 100-110 DEG C, obtains acidifying CNT;
B, above-mentioned zirconium carbonate ammonium, water and Firebrake ZB are mixed, be added to compound weight 20-30 times, concentration be 10-20%
In hydrochloric acid solution, it is 65-70 DEG C to rise high-temperature, adds above-mentioned sodium laurylsulfate, insulated and stirred 10-20 minute, adds above-mentioned
Acidifying CNT, continues insulated and stirred 30-40 minute, filters, and by precipitation washing 2-3 time, normal temperature drying, must be combined acidifying carbon
Nanotube;
C, by above-mentioned zinc dialkyl dithiophosphate, the tert-butyl group to biphenol mix, be added in above-mentioned N-Methyl pyrrolidone,
It is 76-80 DEG C to rise high-temperature, insulated and stirred 10-20 minute, adds above-mentioned calcium ricinoleate, stirs to room temperature, obtain alkanone dispersion liquid;
D, above-mentioned naphthenic soap is added in the dehydrated alcohol of its weight 4-6 times, the insulated and stirred 4-7 minute at 80-90 DEG C,
Above-mentioned abienol is added, is stirred to room temperature, is obtained viscosity-controlling agent;
E, by above-mentioned Sodium fluoroborate, Compound-acid carbon nano tube, hexadecyltrimethylammonium chloride mixing, be added to compound weight
In the ethanol solution of the 70-75% of 1-2 times of amount, it is 50-60 DEG C to rise high-temperature, adds the above-mentioned tert-butyl group to biphenol, insulated and stirred
3-5 minutes, above-mentioned oleamide is added, ultrasonic agitation 2-3 minute, is filtered, by precipitation washing 3-4 time, in 50-60 DEG C of baking oven
In be dried 1-2 hours, discharge, cooling, obtain modified carbon nano-tube;
F, by above-mentioned modified carbon nano-tube, tetrakis hydroxymetyl phosphonium sulfuric mix, be added to the dehydrated alcohol of compound weight 1-1.7 times
In, stir, it is 70-76 DEG C to rise high-temperature, adds above-mentioned polyurethanes, insulated and stirred 10-20 minute, adds above-mentioned
Alkanone dispersion liquid, mixed grinding 20-30 minutes, sends in ball grinder, adds viscosity-controlling agent and its remaining each raw material, add agate
Seal after Nao balls, 1000-1200 rev/min of ball milling 24-26 hour obtains final product the ink-jet ink;
(2)Above-mentioned ink is injected in print cartridge, is deposited to by predetermined pattern using typical inkjet printing technique and is anticipated
Substrate on;
(3)The above-mentioned thin film deposited on substrate is placed in after being dried in baking oven, after heat treatment forms carbon nanotube conducting thin
Film.
A kind of method that inkjet printing prepares carbon nanotube conductive thin film, described heat treatment temperature are 200-270 DEG C, when
Between be 20-40 minutes.
It is an advantage of the invention that:
CNT can uniformly be disperseed in finished product ink after modification by the present invention, the group of effectively reducing
It is poly-, while CNT has good electric conductivity, can be very good to improve ink jet ink electrical conductivity of water, improve finished films
Electric conductivity, the ink-jet ink good stability of the present invention adopts the alcoholic solution of naphthenic soap can be effective for viscosity-controlling agent
The viscosity and mobility that improve ink, improve stability on thin film after ink-jet.
Specific embodiment
A kind of method that inkjet printing prepares carbon nanotube conductive thin film, comprises the following steps:
(1)The preparation of ink-jet ink:Described ink-jet ink is made up of the raw material of following weight parts:
CNT 60, the naphthenic soap 1, tert-butyl group are to biphenol 0.4, N-Methyl pyrrolidone 40, dialkyl dithiophosphoric acid
Zinc 2, zirconium carbonate ammonium 5, oleamide 2, abienol 3, stannous sulfide 0.3, water and Firebrake ZB 2, calcium ricinoleate 0.5, poly- amino first
Acid esters 3, alkenyl succinic anhydride 0.8, tetrakis hydroxymetyl phosphonium sulfuric 1, hexadecyltrimethylammonium chloride 0.8, Sodium fluoroborate 1, Laurel
Alcohol sodium sulfate 0.5, appropriate dehydrated alcohol;
The preparation method of described ink-jet ink is comprised the following steps:
A, above-mentioned CNT is added to mass ratio for 4:In 1 sulphuric acid, the mixed solution of nitric acid, described sulfuric acid concentration is
97%, described concentration of nitric acid is 98%, is sent in reactor, and ultrasound 3 hours at 120 DEG C are filtered, and will precipitate washing 4 times,
It is vacuum dried 2 hours at 110 DEG C, obtains acidifying CNT;
B, above-mentioned zirconium carbonate ammonium, water and Firebrake ZB are mixed, hydrochloric acid that be added to 20 times of compound weight, that concentration is 20% is molten
In liquid, it is 65-70 DEG C to rise high-temperature, adds above-mentioned sodium laurylsulfate, insulated and stirred 10 minutes to add above-mentioned acidifying carbon nanometer
Pipe, continues insulated and stirred 40 minutes, filters, and by precipitation washing 2 times, normal temperature drying obtains Compound-acid carbon nano tube;
C, by above-mentioned zinc dialkyl dithiophosphate, the tert-butyl group to biphenol mix, be added in above-mentioned N-Methyl pyrrolidone,
It is 80 DEG C to rise high-temperature, and insulated and stirred 10 minutes adds above-mentioned calcium ricinoleate, stirs to room temperature, obtain alkanone dispersion liquid;
D, above-mentioned naphthenic soap is added in the dehydrated alcohol of 4 times of its weight, insulated and stirred 4 minutes at 90 DEG C, in addition
Abienol is stated, is stirred to room temperature, is obtained viscosity-controlling agent;
E, by above-mentioned Sodium fluoroborate, Compound-acid carbon nano tube, hexadecyltrimethylammonium chloride mixing, be added to compound weight
In the ethanol solution of the 75% of 1-2 times of amount, it is 50 DEG C to rise high-temperature, the above-mentioned tert-butyl group of addition to biphenol, insulated and stirred 3 minutes,
Add above-mentioned oleamide, ultrasonic agitation 3 minutes to filter, by precipitation washing 3 times, 1-2 hours be dried in 60 DEG C of baking oven,
Discharging, cooling, obtains modified carbon nano-tube;
F, by above-mentioned modified carbon nano-tube, tetrakis hydroxymetyl phosphonium sulfuric mix, be added to the dehydrated alcohol of 1.7 times of compound weight
In, stir, it is 76 DEG C to rise high-temperature, adds above-mentioned polyurethanes, insulated and stirred 10 minutes to add above-mentioned alkanone point
Dispersion liquid, mixed grinding 30 minutes are sent in ball grinder, add viscosity-controlling agent and its remaining each raw material, close after addition agate ball
Envelope, 1200 revs/min of ball millings 24 hours, obtains final product the ink-jet ink;
(2)Above-mentioned ink is injected in print cartridge, is deposited to by predetermined pattern using typical inkjet printing technique and is anticipated
Substrate on;
(3)The above-mentioned thin film deposited on substrate is placed in after being dried in baking oven, after heat treatment forms carbon nanotube conducting thin
Film.
A kind of method that inkjet printing prepares carbon nanotube conductive thin film, described heat treatment temperature are 270 DEG C, and the time is
40 minutes.
Claims (2)
1. a kind of method that inkjet printing prepares carbon nanotube conductive thin film, it is characterised in that comprise the following steps:
(1)The preparation of ink-jet ink:Described ink-jet ink is made up of the raw material of following weight parts:
CNT 57-60, naphthenic soap 1-2, the tert-butyl group are to biphenol 0.4-1, N-Methyl pyrrolidone 36-40, dialkyl group
Zinc dithiophosphate 1-2, zirconium carbonate ammonium 3-5, oleamide 1-2, abienol 3-4, stannous sulfide 0.1-0.3, water and Firebrake ZB
2-3, calcium ricinoleate 0.5-1, polyurethanes 2-3, alkenyl succinic anhydride 0.8-1, tetrakis hydroxymetyl phosphonium sulfuric 1-2, hexadecane
Base trimethyl ammonium chloride 0.8-1, ammonium fluoroborate 1-2, sodium laurylsulfate 0.5-1, appropriate dehydrated alcohol;
The preparation method of described ink-jet ink is comprised the following steps:
A, above-mentioned CNT is added to mass ratio for 3-4:In 1 sulphuric acid, the mixed solution of nitric acid, described sulfuric acid concentration
For 95-97%, described concentration of nitric acid is 96-98%, is sent in reactor, and the ultrasound 3-5 hours at 100-120 DEG C are filtered, will
Precipitation washing 3-4 time, is vacuum dried 1-2 hours at 100-110 DEG C, obtains acidifying CNT;
B, above-mentioned zirconium carbonate ammonium, water and Firebrake ZB are mixed, be added to compound weight 20-30 times, concentration be 10-20%
In hydrochloric acid solution, it is 65-70 DEG C to rise high-temperature, adds above-mentioned sodium laurylsulfate, insulated and stirred 10-20 minute, adds above-mentioned
Acidifying CNT, continues insulated and stirred 30-40 minute, filters, and by precipitation washing 2-3 time, normal temperature drying, must be combined acidifying carbon
Nanotube;
C, by above-mentioned zinc dialkyl dithiophosphate, the tert-butyl group to biphenol mix, be added in above-mentioned N-Methyl pyrrolidone,
It is 76-80 DEG C to rise high-temperature, insulated and stirred 10-20 minute, adds above-mentioned calcium ricinoleate, stirs to room temperature, obtain alkanone dispersion liquid;
D, above-mentioned naphthenic soap is added in the dehydrated alcohol of its weight 4-6 times, the insulated and stirred 4-7 minute at 80-90 DEG C,
Above-mentioned abienol is added, is stirred to room temperature, is obtained viscosity-controlling agent;
E, by above-mentioned tetrakis hydroxymetyl phosphonium sulfuric, Compound-acid carbon nano tube, hexadecyltrimethylammonium chloride mixing, be added to mixed
In the ethanol solution of the 70-75% for closing material weight 1-2 times, it is 50-60 DEG C to rise high-temperature, adds the above-mentioned tert-butyl group to biphenol, protects
Temperature stirring 3-5 minutes, above-mentioned oleamide is added, ultrasonic agitation 2-3 minute, is filtered, by precipitation washing 3-4 time, at 50-60 DEG C
Baking oven in be dried 1-2 hours, discharge, cooling, obtain modified carbon nano-tube;
F, by above-mentioned modified carbon nano-tube, ammonium fluoroborate mix, be added in the dehydrated alcohol of compound weight 1-1.7 times, stir
Mix uniform, it is 70-76 DEG C to rise high-temperature, add above-mentioned polyurethanes, insulated and stirred 10-20 minute, add above-mentioned alkanone
Dispersion liquid, mixed grinding 20-30 minutes, sends in ball grinder, adds viscosity-controlling agent and its remaining each raw material, add agate ball
After seal, 1000-1200 rev/min of ball milling 24-26 hour obtains final product the ink-jet ink;
(2)Above-mentioned ink is injected in print cartridge, is deposited to by predetermined pattern using typical inkjet printing technique and is anticipated
Substrate on;
(3)The above-mentioned thin film deposited on substrate is placed in after being dried in baking oven, after heat treatment forms carbon nanotube conducting thin
Film.
2. the method that a kind of inkjet printing according to claim 1 prepares carbon nanotube conductive thin film, it is characterised in that:Institute
The heat treatment temperature stated is 200-270 DEG C, and the time is 20-40 minutes.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108610744A (en) * | 2018-04-27 | 2018-10-02 | 佛山市智巢电子科技有限公司 | A kind of preparation method of spray printing polyester electric conduction film |
CN109065211A (en) * | 2018-05-30 | 2018-12-21 | 查公祥 | A kind of poly closes composite conducting additive and preparation method thereof |
CN114496354A (en) * | 2022-01-21 | 2022-05-13 | 深圳市飞墨科技有限公司 | Preparation method and application of transparent conductive film |
CN114496354B (en) * | 2022-01-21 | 2024-04-30 | 深圳市飞墨科技有限公司 | Preparation method and application of transparent conductive film |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101754584A (en) * | 2008-12-12 | 2010-06-23 | 清华大学 | Method for preparing conducting lines |
CN103189311A (en) * | 2010-10-29 | 2013-07-03 | 东丽株式会社 | Method for manufacturing liquid dispersion of carbon-nanotube aggregates |
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2016
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101754584A (en) * | 2008-12-12 | 2010-06-23 | 清华大学 | Method for preparing conducting lines |
CN103189311A (en) * | 2010-10-29 | 2013-07-03 | 东丽株式会社 | Method for manufacturing liquid dispersion of carbon-nanotube aggregates |
Non-Patent Citations (1)
Title |
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凌云星等: "《实用油墨技术指南》", 30 November 2007, 印刷工业出版社 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108610744A (en) * | 2018-04-27 | 2018-10-02 | 佛山市智巢电子科技有限公司 | A kind of preparation method of spray printing polyester electric conduction film |
WO2019205190A1 (en) * | 2018-04-27 | 2019-10-31 | 佛山市智巢电子科技有限公司 | Method for preparing jet-printed polyester conductive thin film |
CN109065211A (en) * | 2018-05-30 | 2018-12-21 | 查公祥 | A kind of poly closes composite conducting additive and preparation method thereof |
CN114496354A (en) * | 2022-01-21 | 2022-05-13 | 深圳市飞墨科技有限公司 | Preparation method and application of transparent conductive film |
CN114496354B (en) * | 2022-01-21 | 2024-04-30 | 深圳市飞墨科技有限公司 | Preparation method and application of transparent conductive film |
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