CN111500120A - Nano carbon conductive ink suitable for fabric screen printing and preparation method thereof - Google Patents
Nano carbon conductive ink suitable for fabric screen printing and preparation method thereof Download PDFInfo
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- CN111500120A CN111500120A CN202010324621.0A CN202010324621A CN111500120A CN 111500120 A CN111500120 A CN 111500120A CN 202010324621 A CN202010324621 A CN 202010324621A CN 111500120 A CN111500120 A CN 111500120A
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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
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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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
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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Abstract
The invention discloses a nano carbon conductive ink suitable for fabric screen printing and a preparation method thereof. The raw materials of the nano carbon conductive ink comprise nano carbon conductive materials, polyurethane elastomers, solvents, defoaming agents and flatting agents in percentage by mass. The preparation method comprises the following steps: under the condition of heating and stirring, adding polyurethane elastomer particles into a solvent, and fully stirring to obtain a polymer matrix solution; adding a nano carbon conductive material, a defoaming agent and a flatting agent into the polymer matrix solution, and carrying out room-temperature stirring and bath ultrasonic treatment to prepare the uniformly dispersed nano carbon conductive ink. The conductive ink can be used for screen printing on flexible printing substrates such as fabrics, films and paper, has the advantages of uniform dispersion, simple preparation method, low production cost, large-scale production and the like, and can provide a good substrate for flexible intelligent textile materials.
Description
Technical Field
The invention belongs to the field of functional printing ink and preparation thereof, and particularly relates to a preparation method of nano carbon conductive printing ink suitable for fabric screen printing.
Background
In recent years, with the rapid development of the internet of things and intelligent interaction technology, the development and application of flexible wearable electronic equipment are receiving wide attention, and especially the demand of the flexible wearable electronic equipment in the application fields of national defense and military, medical monitoring, intelligent sensing and the like is increasing continuously. Compared with flexible base materials such as silicon rubber and plastic films, textiles which are visible everywhere in life have ideal physical and mechanical properties, air permeability and durability, and can bear twisting and bending actions at any angle, so that the textile can better fit human body curves and meet the requirements of human body movement, and therefore the application of the textile base materials can better meet the research and development targets of wearable electronic equipment. Among various preparation methods of the conductive fabric, the silk-screen printing as an additive manufacturing method can realize excellent conductivity and flexibility on the premise of not influencing the mechanical property of a fabric substrate, and has the advantages of low cost, simple preparation flow, large-scale production and the like.
At present, conductive inks used for screen printing are mainly classified into metal-based conductive inks and carbon-based conductive inks. Although metal-based conductive inks such as copper, silver, nickel and the like have good conductive performance, the metal-based conductive inks are high in cost, easy to oxidize, easy to fall off from the surface of a substrate, and cause heavy metal pollution, skin allergy and the like. The carbon-based conductive ink such as graphite, carbon black, carbon nanotubes, graphene and the like has high conductivity and chemical stability and is widely applied to the field of printed electronics, wherein the carbon nanotubes have high conductivity and high length-diameter ratio, and the graphene has excellent mechanical properties and high carrier mobility, so that the carbon-based conductive ink is suitable for forming a stable mesh-shaped conductive network on the surface of a porous rough fabric. Therefore, the preparation of the nano carbon conductive ink suitable for the screen printing of the fabric substrate has important significance for the research and development of flexible wearable electronic equipment.
The existing carbon-based conductive ink technology has the following main problems: a cumbersome pretreatment process is required to improve the uniformity of the conductive ink, or a long treatment process is required to achieve good adhesion of the conductive ink to the substrate. For example, patent CN110358369A discloses a method for preparing graphene and carbon nanotube conductive ink for inkjet, which includes ball-milling carbon-based conductive particles at room temperature, performing primary selection, washing, sorting and collecting on the mixture to obtain a conductive unit mixed dispersion, and adding a linking agent and an auxiliary agent to obtain a conductive ink with uniform mixing and proper viscosity. Patent CN106876155A discloses a preparation method of a conductive cotton fabric based on carbon nano tubes, in the method, the cotton fabric is immersed into carbon nano tube dispersion liquid at 130-140 ℃ for heat treatment for 60-100 min, and then is dried at 100 ℃, although the prepared conductive cotton fabric has excellent conductivity, the inherent mechanical property of the fabric can be seriously influenced by long-time hydrothermal high-temperature treatment.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a nano carbon conductive ink suitable for fabric screen printing and a preparation method thereof, so as to overcome the defect of complicated and long preparation procedures in the prior art.
In order to solve the technical problems, the invention provides a nano carbon conductive ink suitable for fabric screen printing, which is characterized in that raw materials comprise, by mass, 0.5-15% of a nano carbon conductive material, 10-20% of a polyurethane elastomer, 70-80% of a solvent, 0.2-1% of a defoaming agent and 0.2-1% of a leveling agent.
Preferably, the nanocarbon conductive material includes at least one of carbon nanotubes and graphene.
More preferably, the carbon nano tube has an outer diameter of 8-15nm, an inner diameter of 3-6nm and a length of 3-12 μm; the thickness of the graphene is 3-8nm, and the sheet diameter is 20-50 mu m.
Preferably, the polyurethane elastomer is a thermoplastic polyurethane elastomer.
The polyurethane elastomer is thermoplastic polyurethane elastomer particles, is a conventional commercially available product, and is preferably a polyester type thermoplastic polyurethane elastomer in consideration of tensile properties and wear resistance of the cured conductive ink.
Preferably, the solvent is any one of N-methylpyrrolidone and dimethylformamide, which are commercially available products, and N-methylpyrrolidone is preferred in view of stability and safety of the conductive ink, and is available from national chemical agents ltd.
Preferably, the defoaming agent is BYK-052N or BYK-065.
Preferably, the leveling agent is BYK-333.
The invention also provides a preparation method of the nano carbon conductive ink suitable for the fabric screen printing, which comprises the following steps:
step 1): under the condition of heating and stirring, adding polyurethane elastomer particles into a solvent, and fully stirring to obtain a polymer matrix solution;
step 2): adding a nano carbon conductive material, a defoaming agent and a flatting agent into the polymer matrix solution, and carrying out room-temperature stirring and bath ultrasonic treatment to prepare the uniformly dispersed nano carbon conductive ink.
Preferably, the heating temperature in the step 1) is 30-60 ℃, the stirring speed is 500-1000 rpm, and the stirring time is 1-2 h.
Preferably, the stirring time in the step 2) is 1-2 h; the ultrasonic treatment time is 30-90 min, and the treatment temperature is 20-40 ℃.
The nano carbon conductive material comprises at least one of carbon nano tubes and graphene. Wherein the preferred sizes of the carbon nanotubes are: the outer diameter is 8-15nm, the inner diameter is 3-6nm, and the length is 3-12 mu m; preferred dimensions of the graphene are: the thickness is 3-8nm and the sheet diameter is 20-50 μm.
The polyurethane elastomer is thermoplastic polyurethane elastomer particles, is a conventional commercial product, is preferably a polyester type thermoplastic polyurethane elastomer in view of tensile property and wear resistance of the cured conductive ink, and is purchased from basf, germany.
The solvent is one of N-methyl pyrrolidone and dimethylformamide, is a commercially available product, and is preferably N-methyl pyrrolidone which is purchased from national chemical agents, Inc. in consideration of stability and safety of the conductive ink.
The defoaming agent is BYK-052N or BYK-065, is purchased from BYK company in Germany, can effectively eliminate bubbles generated in the ink in the stirring and printing processes, and improves the uniformity and the evenness of a printing film layer.
The leveling agent is BYK-333, is purchased from BYK company in Germany, can improve the leveling performance of the printing ink, and can prevent the defects of shrinkage cavity, orange peel and the like during printing.
The conductive ink has the advantages of simple preparation process, low cost, proper viscosity and uniformity, and suitability for screen printing process of flexible substrates such as fabrics. The nano carbon conductive ink prepared by the invention has excellent conductivity, stability, dispersion uniformity and proper viscosity, and does not generate layering of the conductive ink or agglomeration of conductive particles after being stored for a long time, thereby being very suitable for a screen printing process of a flexible substrate.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method disclosed by the invention is short in preparation flow, convenient in process operation, low in equipment and material cost, small in environmental pollution, suitable for large-scale green production and good in engineering significance and economic benefit.
(2) The invention adopts the nano carbon material as the conductive filler, and has excellent conductive performance, mechanical property and stability due to the unique structure and the single carbon element. Compared with metal conductive ink, the nano carbon conductive ink has higher oxidation resistance and corrosion resistance, can form a highly interconnected conductive network, and reduces the surface resistance by 8-10 orders of magnitude after screen printing on the surface of porous rough fabric.
(3) The conductive ink prepared by the invention is suitable for a screen printing process, is simple to operate, has low cost, is not limited by the size and the shape of a printing stock, can be printed on the surfaces of various flexible base materials such as common fabrics, films, paper and the like, and has the advantages of simple and easy curing mode and high production efficiency. The screen printing precision and the quality of the ink are high, and when the printing line width of the fabric surface is 0.3mm, a continuous conductive path can be formed.
(4) The nano carbon conductive ink adopts the thermoplastic polyurethane elastomer as the matrix, has proper viscosity, good printing film forming property and strong adhesive force with the fabric base material, and the printed film layer has excellent flexibility and wear resistance.
Drawings
FIG. 1 shows the surface resistance of the original fabric and the conductive ink prepared in examples 1 to 4 after screen printing on the surface of the fabric substrate;
FIG. 2 is a comparative scanning electron micrograph of the conductive inks prepared according to examples 1-4 after screen printing on a surface of a textile substrate;
FIG. 3 is a representation of the conductive ink prepared in example 3 after screen printing on a nylon coated fabric surface;
FIG. 4 is a graph showing the surface resistance change of the nylon fabric of example 5 after screen printing.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
The polyester-type thermoplastic polyurethane elastomers employed in examples 1-5 were obtained from basf, germany; the solvent is N-methyl pyrrolidone, and is purchased from national chemical reagent limited company; the defoaming agent is BYK-052N or BYK-065 which is purchased from BYK company in Germany; the leveling agent was BYK-333, available from BYK, Germany.
Example 1
A nano carbon conductive ink suitable for fabric screen printing and a preparation method thereof are disclosed:
step (1): under the condition of heating and stirring at 40 ℃, thermoplastic polyurethane elastomer particles are added into the N-methyl pyrrolidone solution, the adding proportion is 25 wt% of the N-methyl pyrrolidone solution (if the N-methyl pyrrolidone is 10g, the thermoplastic polyurethane elastomer particles are added by 2.5g), and the mixture is stirred for 1h, so that the polymer matrix solution is obtained.
Step (2): and (2) mixing the polymer matrix solution obtained in the step (1), a multi-walled carbon nanotube conductive material (with the outer diameter of 10-14nm, the inner diameter of 4-6nm and the length of 8-12 mu m), a defoaming agent and a flatting agent according to the mass ratio of 98: 1: 0.6: 0.4, magnetically stirring for 1h at room temperature, and performing bath ultrasonic treatment for 30min to obtain the carbon nanotube conductive ink.
And (3): the prepared carbon nano tube conductive ink is used for a screen printing process, and a printing substrate is a nylon plain weave fabric (the warp density is 670 pieces/cm, the weft density is 470 pieces/cm, and the gram weight per unit area is 63.23g/m2) And nylon coated fabric (unit)The areal gram weight is 65g/m2The coating material is calcium carbonate), a semi-automatic screen printer is adopted for printing, the mesh number of the screen is 200 meshes, the angle between a scraper and the screen is 85 degrees, and the printing speed is 16.9 cm/s.
And (4): and (3) drying and curing the printed sample for 1h at the temperature of 80 ℃. The printed samples were tested for electrical properties using a multimeter according to AATCC76-2005 textile surface resistance test method, the results of which are shown in fig. 1. Microscopic morphology of the printed film layer on the surface of the nylon plain weave fabric was observed using Hitachi TM3000 scanning electron microscope, as shown in FIG. 2 (a).
Example 2
A nano carbon conductive ink suitable for fabric screen printing and a preparation method thereof are disclosed:
step (1): under the condition of heating and stirring at 40 ℃, thermoplastic polyurethane elastomer particles are added into the N-methyl pyrrolidone solution, the adding proportion is 25 percent of the N-methyl pyrrolidone solution (if the N-methyl pyrrolidone is 10g, the thermoplastic polyurethane elastomer particles are added by 2.5g), and the stirring is carried out for 1h, so as to obtain the polymer matrix solution.
Step (2): and (2) mixing the polymer matrix solution obtained in the step (1), a multi-walled carbon nanotube conductive material (with the outer diameter of 10-14nm, the inner diameter of 4-6nm and the length of 8-12 mu m), a defoaming agent and a flatting agent according to the mass ratio of 96: 3: 0.6: 0.4, magnetically stirring for 1h at room temperature, and performing bath ultrasonic treatment for 30min to obtain the carbon nanotube conductive ink.
And (3): the prepared carbon nano tube conductive ink is used for a screen printing process, and a printing substrate is a nylon plain weave fabric (the warp density is 670 pieces/cm, the weft density is 470 pieces/cm, and the gram weight per unit area is 63.23g/m2) And nylon coated fabric (grammage 65 g/m)2The coating material is calcium carbonate), a semi-automatic screen printer is adopted for printing, the angle between a scraper and a screen plate is 85 degrees, and the printing speed is 16.9 cm/s.
And (4): and (3) drying and curing the printed sample for 1h at the temperature of 80 ℃. The printed samples were tested for electrical properties using a multimeter according to AATCC76-2005 textile surface resistance test method, the results of which are shown in fig. 1. Microscopic morphology of the printed film layer on the surface of the nylon scrim was observed using Hitachi TM3000 scanning electron microscope, as shown in FIG. 2 (b).
Example 3
A nano carbon conductive ink suitable for fabric screen printing and a preparation method thereof are disclosed:
step (1): under the condition of heating and stirring at 40 ℃, thermoplastic polyurethane elastomer particles are added into the N-methyl pyrrolidone solution, the adding proportion is 25 percent of the N-methyl pyrrolidone solution (if the N-methyl pyrrolidone is 10g, the thermoplastic polyurethane elastomer particles are added by 2.5g), and the stirring is carried out for 1h, so as to obtain the polymer matrix solution.
Step (2): mixing the polymer matrix solution obtained in the step (1), a multi-walled carbon nanotube conductive material (with the outer diameter of 10-14nm, the inner diameter of 4-6nm and the length of 8-12 mu m), a defoaming agent and a flatting agent according to the mass ratio of 94: 5: 0.6: 0.4, magnetically stirring for 1h at room temperature, and performing bath ultrasonic treatment for 30min to obtain the carbon nanotube conductive ink.
And (3): the prepared carbon nano tube conductive ink is used for a screen printing process, and a printing substrate is a nylon plain weave fabric (the warp density is 670 pieces/cm, the weft density is 470 pieces/cm, and the gram weight per unit area is 63.23g/m2) And nylon coated fabric (grammage 65 g/m)2The coating material is calcium carbonate), a semi-automatic screen printer is adopted for printing, the angle between a scraper and a screen plate is 85 degrees, and the printing speed is 16.9 cm/s.
And (4): and (3) drying and curing the printed sample for 1h at the temperature of 80 ℃. The printed samples were tested for electrical properties using a multimeter according to AATCC76-2005 textile surface resistance test method, the results of which are shown in fig. 1. Microscopic morphology of the printed film layer on the surface of the nylon scrim was observed using Hitachi TM3000 scanning electron microscope, as shown in FIG. 2 (c).
Example 4
Step (1): adding thermoplastic polyurethane elastomer particles into the N-methylpyrrolidone solution under the condition of heating and stirring at 40 ℃, adding 20% of dimethylformamide solution (if 10g of dimethylformamide is added, 2g of thermoplastic polyurethane elastomer particles are added), and stirring for 1h to obtain a polymer matrix solution.
Step (2): and (2) mixing the polymer matrix solution obtained in the step (1), graphene (with the thickness of 4-6nm and the sheet diameter of 30-40 microns), a defoaming agent and a flatting agent according to a mass ratio of 89: 10: 0.6: mixing the components according to the proportion of 0.4, magnetically stirring the mixture for 1 hour at room temperature, and then carrying out bath ultrasonic treatment for 30min to obtain the graphene conductive ink.
And (3): the prepared graphene conductive ink is used for a screen printing process, and a printing substrate is a nylon plain weave fabric (the warp density is 670 pieces/cm, the weft density is 470 pieces/cm, and the gram weight per unit area is 63.23 g/m)2) And nylon coated fabric (grammage 65 g/m)2The coating material is calcium carbonate), a semi-automatic screen printer is adopted for printing, the angle between a scraper and a screen plate is 85 degrees, and the printing speed is 16.9 cm/s.
And (4): and (3) drying and curing the printed sample for 1h at the temperature of 100 ℃. The printed samples were tested for electrical properties using a multimeter according to AATCC76-2005 textile surface resistance test method, the results of which are shown in fig. 1. Microscopic morphology of the printed film layer on the surface of the nylon scrim was observed using Hitachi TM3000 scanning electron microscope, as shown in FIG. 2 (d).
Example 5
A nano carbon conductive ink suitable for fabric screen printing and a preparation method thereof are disclosed:
step (1): the conductive ink prepared in example 3 was used in a screen printing process, and the printing substrate was a nylon plain weave fabric (a warp density of 670 pieces/cm, a weft density of 470 pieces/cm, a basis weight of 63.23 g/m)2). Printing by using a semi-automatic screen printer, wherein the angle between a scraper and a screen is 85 degrees, and the printing speed is 16.9 cm/s;
step (2): and (3) drying and curing the printed sample (figure 3) at 80 ℃ for 1 h. The electrical properties of the printed samples were tested using a multimeter according to the AATCC76-2005 textile surface resistance test method.
And (3): and (3) repeating the step (1) and the step (2) on the surface of the printed sample until 8 layers of conductive ink are printed on the surface of the substrate. The results of the electrical property tests of the samples are shown in fig. 4.
Claims (10)
1. The nano-carbon conductive ink suitable for fabric screen printing is characterized by comprising, by mass, 0.5-15% of a nano-carbon conductive material, 10-20% of a polyurethane elastomer, 70-80% of a solvent, 0.2-1% of a defoaming agent and 0.2-1% of a leveling agent.
2. The nanocarbon conductive ink of claim 1, wherein the nanocarbon conductive material comprises at least one of carbon nanotubes and graphene.
3. The nanocarbon conductive ink of claim 2, wherein the carbon nanotubes have an outer diameter of 8 to 15nm, an inner diameter of 3 to 6nm, and a length of 3 to 12 μm; the thickness of the graphene is 3-8nm, and the sheet diameter is 20-50 mu m.
4. The nanocarbon conductive ink of claim 1, wherein the polyurethane elastomer is a thermoplastic polyurethane elastomer.
5. The nanocarbon conductive ink according to claim 1, wherein the solvent is any one of N-methylpyrrolidone and dimethylformamide.
6. The nanocarbon conductive ink of claim 1, wherein the antifoaming agent is BYK-052N or BYK-065.
7. The nanocarbon conductive ink of claim 1, wherein the leveling agent is BYK-333.
8. The method for preparing the nanocarbon conductive ink suitable for screen printing of fabrics according to any one of claims 1 to 7, comprising:
step 1): under the condition of heating and stirring, adding polyurethane elastomer particles into a solvent, and fully stirring to obtain a polymer matrix solution;
step 2): adding a nano carbon conductive material, a defoaming agent and a flatting agent into the polymer matrix solution, and carrying out room-temperature stirring and bath ultrasonic treatment to prepare the uniformly dispersed nano carbon conductive ink.
9. The preparation method of claim 8, wherein the heating temperature in the step 1) is 30-60 ℃, the stirring speed is 500-1000 rpm, and the stirring time is 1-2 h.
10. The method for preparing the nanocarbon conductive ink according to claim 8, wherein the stirring time in the step 2) is 1-2 hours; the ultrasonic treatment time is 30-90 min, and the treatment temperature is 20-40 ℃.
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| CN113549374A (en) * | 2021-08-26 | 2021-10-26 | 武汉大学 | High-elasticity water-based conductive ink for fabric, printing stretchable electronic fabric, and preparation method and application thereof |
| CN115172071A (en) * | 2022-08-04 | 2022-10-11 | 东华大学 | Self-integrated flexible supercapacitor based on fabric and preparation method thereof |
| CN116179015A (en) * | 2023-02-10 | 2023-05-30 | 深圳烯湾科技有限公司 | Polyurethane composite material, preparation method thereof and product |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112778840A (en) * | 2021-01-25 | 2021-05-11 | 中科院长春应化所黄埔先进材料研究院 | Conductive ink and preparation method thereof |
| CN113549374A (en) * | 2021-08-26 | 2021-10-26 | 武汉大学 | High-elasticity water-based conductive ink for fabric, printing stretchable electronic fabric, and preparation method and application thereof |
| CN115172071A (en) * | 2022-08-04 | 2022-10-11 | 东华大学 | Self-integrated flexible supercapacitor based on fabric and preparation method thereof |
| CN115172071B (en) * | 2022-08-04 | 2023-12-26 | 东华大学 | Self-integrated flexible supercapacitor based on fabric and preparation method thereof |
| CN116179015A (en) * | 2023-02-10 | 2023-05-30 | 深圳烯湾科技有限公司 | Polyurethane composite material, preparation method thereof and product |
| CN116179015B (en) * | 2023-02-10 | 2023-12-01 | 深圳烯湾科技有限公司 | Polyurethane composite material, preparation method thereof and product |
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Inventor after: Yan Xiong Inventor after: Jiang Lihong Inventor after: Hu Jiyong Inventor before: Yan Xiong Inventor before: Jiang Hongli Inventor before: Hu Jiyong |
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Application publication date: 20200807 |