CN111900065A - Carbon nanotube slurry with strong adhesion and preparation method thereof - Google Patents
Carbon nanotube slurry with strong adhesion and preparation method thereof Download PDFInfo
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- CN111900065A CN111900065A CN202010758240.3A CN202010758240A CN111900065A CN 111900065 A CN111900065 A CN 111900065A CN 202010758240 A CN202010758240 A CN 202010758240A CN 111900065 A CN111900065 A CN 111900065A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/02—Main electrodes
- H01J1/30—Cold cathodes, e.g. field-emissive cathode
- H01J1/304—Field-emissive cathodes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
- H01J9/022—Manufacture of electrodes or electrode systems of cold cathodes
- H01J9/025—Manufacture of electrodes or electrode systems of cold cathodes of field emission cathodes
Abstract
The invention relates to a carbon nanotube slurry with strong adhesion, which comprises the following raw materials in percentage by mass: 89% -95% of first mixed solvent and 5% -11% of carbon nano tube subjected to grinding and dispersing treatment; the first mixed solvent comprises the following raw materials in percentage by mass: 50-70% of second mixed solvent, 9-20% of ferric oxide, 0.31-0.62% of dispersant, 0.05-0.1% of flatting agent, 0.02-0.04% of surfactant and 14-28% of binder; the second mixed solvent comprises a dispergator and deionized water, wherein the dispergator enables the pH value of the second mixed solvent to be 7-11. The carbon nanotube slurry provided by the invention effectively solves the problems that the traditional carbon nanotube slurry has poor adhesion to a glass substrate, is easy to scratch and is easy to strike fire, discharge, ablate and fall off under high pressure, and greatly improves the adhesion of the slurry to the glass substrate. In addition, the invention also relates to a preparation method of the carbon nanotube slurry with strong adhesion.
Description
Technical Field
The invention belongs to the technical field of carbon nanotube slurry, and particularly relates to carbon nanotube slurry with strong adhesion and a preparation method thereof.
Background
The carbon nano tube has a unique one-dimensional nano structure, large specific surface area, high mechanical strength, stable chemical properties and good axial conductivity, is favorable for electron transportation, and the defects of the tip and the tube wall of the nano scale form a good electron emission end, thereby being the most potential field emission cathode material. When the carbon nanotube coating is prepared, the carbon nanotube slurry using the traditional formula has weak adhesion to a substrate and is easy to scratch and wear. Therefore, it is a key to solve the above problems to prepare a carbon nanotube paste having strong adhesion to a substrate.
Disclosure of Invention
The invention aims to solve the technical problems of poor adhesion and easy scratch of the traditional slurry on a substrate in the prior art, and provides the carbon nanotube slurry with strong adhesion and the preparation method thereof.
In order to solve the technical problem, an embodiment of the present invention provides a carbon nanotube slurry with strong adhesion, which includes the following raw materials by mass: 89% -95% of first mixed solvent and 5% -11% of carbon nano tube subjected to grinding and dispersing treatment;
the first mixed solvent comprises the following raw materials in percentage by mass: 50-70% of second mixed solvent, 9-20% of ferric oxide, 0.31-0.62% of dispersant, 0.05-0.1% of flatting agent, 0.02-0.04% of surfactant and 14-28% of binder; the second mixed solvent comprises a dispergator and deionized water, wherein the dispergator enables the pH value of the second mixed solvent to be 7-11.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the ferric oxide is ferric oxide powder.
Further, the dispersant is lignosulfonate.
Further, the dispersant is sodium methyl lignin (CMC) or sodium calcium lignosulfonate (C-21).
Further, the leveling agent is ethylene glycol.
Further, the surfactant is a nonionic surfactant.
Further, the non-ionic surfactant is tween-20 or tween-80.
Further, the dispergator is ammonia water.
Further, the dispergator enables the pH value of the deionized water to be 10.
Further, the binder is sodium silicate and potassium silicate.
Further, the carbon nanotube is any one of single-arm or multi-arm carbon nanotubes prepared by any one of an arc discharge method, a laser ablation method, a solid phase pyrolysis method, an electrolysis method and a chemical vapor deposition method.
Further, the grinding dispersion treatment employs a grinding bowl or a ball mill.
In order to solve the above technical problems, an embodiment of the present invention provides a method for preparing a carbon nanotube slurry with strong adhesion, including the following steps:
preparing a first mixed solvent: adding a second mixed solvent with the mass percentage of 50% -70%, ferric oxide with the mass percentage of 9% -20%, a dispersing agent with the mass percentage of 0.31% -0.62%, a flatting agent with the mass percentage of 0.05% -0.1%, a surface active agent with the mass percentage of 0.02% -0.04% and a bonding agent with the mass percentage of 14% -28% into a stirrer for first mixing treatment to obtain a first mixed solvent, wherein the second mixed solvent comprises a dispergator and deionized water, and the dispergator enables the pH value of the second mixed solvent to be 7-11;
preparing carbon nanotube slurry: and adding 89-95% by mass of the first mixed solvent and 5-11% by mass of the carbon nano tube subjected to grinding and dispersing treatment into a stirrer for second mixing treatment to obtain the carbon nano tube slurry.
Further, the first mixing treatment comprises heating and stirring in a water bath in the stirrer, wherein the rotating speed of the stirrer is 800-.
And/or the second mixing treatment comprises heating and stirring in a water bath in the stirrer, wherein the rotating speed of the stirrer is 800-.
Further, the stirrer is a constant-temperature heating magnetic stirrer.
Furthermore, the model of the constant-temperature heating magnetic stirrer is a DF-101S heat collection type constant-temperature heating magnetic stirrer.
The invention has the beneficial effects that: according to the carbon nanotube slurry with strong adhesion, the adhesive is mainly utilized to be further chemically bonded with the substrate, the generated product is deposited in the pores and firmly combined with the substrate, so that sufficient adhesive force is generated between a coating prepared from the carbon nanotube slurry and the substrate, the adhesion of the carbon nanotube slurry to the substrate is greatly improved, in addition, the CNTs particles are positive due to the addition of the ferric oxide, and the dispergator enables deionized water to be alkaline, so that like charges are mutually exclusive, and colloidal particles are prevented from aggregating and precipitating; the dispersing agent and the surface active agent wrap the CNTs molecules, so that the CNTs molecules are uniformly dispersed and changed from hydrophobic to hydrophilic; the leveling agent enables the surface of the coating to be smoother. In conclusion, the carbon nanotube slurry with strong adhesion overcomes the problems that the traditional carbon nanotube slurry has poor adhesion to a substrate, is easy to scratch and is easy to strike fire, discharge, ablate and fall off under high pressure. The slurry is suitable for preparing a carbon nanotube coating with strong adhesion on a substrate made of glass materials such as ITO glass.
Drawings
FIG. 1 is an SEM image of the surface topography after emission of a field emission cathode prepared based on a carbon nanotube slurry with strong adhesion in example 1 of the present invention;
fig. 2 is an SEM image of the surface topography of a field emission cathode prepared based on a conventional carbon nanotube slurry after emission.
Detailed Description
The principles and features of this invention are described below in conjunction with embodiments, which are included to explain the invention and not to limit the scope of the invention.
The invention provides a carbon nanotube slurry with strong adhesion, which comprises the following raw materials in percentage by mass: 89% -95% of first mixed solvent and 5% -11% of carbon nano tube subjected to grinding and dispersing treatment;
the first mixed solvent comprises the following raw materials in percentage by mass: 50-70% of second mixed solvent, 9-20% of ferric oxide, 0.31-0.62% of dispersant, 0.05-0.1% of flatting agent, 0.02-0.04% of surfactant and 14-28% of binder; the second mixed solvent comprises a dispergator and deionized water, wherein the dispergator enables the pH value of the second mixed solvent to be 7-11.
Optionally, the ferric oxide is ferric oxide powder.
Optionally, the dispersant is a lignosulfonate.
Optionally, the dispersant is sodium methyl lignin (CMC) or sodium calcium lignosulfonate (C-21).
Optionally, the leveling agent is ethylene glycol.
Optionally, the surfactant is a nonionic surfactant.
Optionally, the non-ionic surfactant is tween-20 or tween-80.
Optionally, the debonder is aqueous ammonia.
Optionally, the debonder provides a PH of 10 for the deionized water.
Optionally, the binder is sodium silicate and potassium silicate.
Optionally, the carbon nanotube is any one selected from single-arm or multi-arm carbon nanotubes prepared by any one of arc discharge method, laser ablation method, solid phase pyrolysis method, electrolysis method and chemical vapor deposition method.
Alternatively, the grinding dispersion treatment employs a grinding bowl or a ball mill.
The second aspect of the present invention provides a method for preparing a carbon nanotube slurry having strong adhesiveness, comprising the steps of:
preparing a first mixed solvent: adding a second mixed solvent with the mass percentage of 50% -70%, ferric oxide with the mass percentage of 9% -20%, a dispersing agent with the mass percentage of 0.31% -0.62%, a flatting agent with the mass percentage of 0.05% -0.1%, a surface active agent with the mass percentage of 0.02% -0.04% and a bonding agent with the mass percentage of 14% -28% into a stirrer for first mixing treatment to obtain a first mixed solvent, wherein the second mixed solvent comprises a dispergator and deionized water, and the dispergator enables the pH value of the second mixed solvent to be 7-11;
preparing carbon nanotube slurry: and adding 89-95% by mass of the first mixed solvent and 5-11% by mass of the carbon nano tube subjected to grinding and dispersing treatment into a stirrer for second mixing treatment to obtain the carbon nano tube slurry.
Optionally, the first mixing treatment comprises heating and stirring in a water bath in the stirrer, wherein the rotating speed of the stirrer is 800-.
And/or the second mixing treatment comprises heating and stirring in a water bath in the stirrer, wherein the rotating speed of the stirrer is 800-.
Optionally, the stirrer is a constant temperature heating magnetic stirrer.
Optionally, the model of the constant-temperature heating magnetic stirrer is a DF-101S heat collection type constant-temperature heating magnetic stirrer.
The present invention will be described in detail below by way of examples.
Example 1
Preparing carbon nano tube slurry according to the following mass percentages: 5.84% of carbon nano tubes and 94.16% of first mixed solvent; the first mixed solvent is prepared from the following components in percentage by mass: 69.77% of a second mixed solvent, 9.85% of ferric oxide, 0.31% of a dispersing agent, 0.05% of a flatting agent, 0.02% of a surfactant and 14.16% of a binder, wherein the second mixed solvent comprises a dispergator and deionized water, and the pH value of the second mixed solvent is 10 due to the dispergator.
Preferably, 19.68g of ferric oxide, 0.62g of CMC, 0.04g of Tween-80, 28.28g of potassium silicate, 0.1g of ethylene glycol and 145.8g of deionized water with pH 10 prepared by ammonia water are mixed and put into a heat collection type constant temperature heating magnetic stirrer, the rotating speed is 860r/min, the mixture is heated in a water bath at 60 ℃ and stirred for 30min until the solution is clear and transparent, and a first mixed solvent is obtained;
taking out 18.34g of the first mixed solvent for standby;
and manually grinding 1.166g of single-arm carbon nanotube for 5min by using an agate mortar, mixing with 18.34g of the first mixed solvent, continuously using a heat collection type constant-temperature heating magnetic stirrer at the rotating speed of 1000r/min, heating in a water bath at 60 ℃ and stirring for 2h to obtain the final carbon nanotube slurry with strong adhesion.
Fig. 1 and fig. 2 show SEM images of the surface topography of a carbon nanotube field emission cathode prepared on an ITO substrate based on a carbon nanotube slurry with strong adhesion and a carbon nanotube field emission cathode prepared on a conventional carbon nanotube slurry according to example 1 of the present invention after the same field emission test, respectively, as can be seen from fig. 1 and fig. 2, under the same emission conditions, a large number of cracks are obviously formed and the carbon nanotube field emission cathode prepared by using the conventional carbon nanotube slurry falls off obviously; the carbon nanotube field emission cathode prepared by the carbon nanotube slurry with strong adhesiveness has the advantages of insignificant shedding and rubbing phenomena and stronger adhesiveness.
Example 2:
preparing carbon nano tube slurry according to the following mass percentages: 10.56% of carbon nano tube and 89.44% of first mixed solvent; the first mixed solvent is prepared from the following components in percentage by mass: the composite material comprises 50% of a second mixed solvent, 18.68% of ferric oxide, 0.62% of a dispersing agent, 0.1% of a flatting agent, 0.04% of a surfactant and 20% of a binder, wherein the second mixed solvent comprises a dispergator and deionized water, and the pH value of the second mixed solvent is 10 due to the dispergator.
Preferably, 18.68g of ferric oxide, 0.62g of CMC, 0.04g of Tween-80, 20g of potassium silicate, 0.1g of ethylene glycol and 50g of deionized water with pH 10 prepared by ammonia water are mixed and put into a heat collection type constant temperature heating magnetic stirrer, the rotating speed is 860r/min, the mixture is heated in a water bath at 60 ℃ and stirred for 30min until the solution is clear and transparent, and a first mixed solvent is obtained;
8.944g of the first mixed solvent is taken out for standby;
manually grinding 1.056g of single-arm carbon nanotube for 5min by using an agate mortar, mixing with 8.944g of the first mixed solvent, continuously using a heat collection type constant-temperature heating magnetic stirrer at the rotating speed of 1000r/min, heating in a water bath at 60 ℃ and stirring for 2h to obtain the final carbon nanotube slurry with strong adhesion.
Example 3:
preparing carbon nano tube slurry according to the following mass percentages: 8.35% of carbon nano tube and 91.65% of first mixed solvent; the first mixed solvent is prepared from the following components in percentage by mass: 58% of a second mixed solvent, 13.07% of ferric oxide, 0.48% of a dispersing agent, 0.07% of a flatting agent, 0.03% of a surfactant and 20% of a binder, wherein the second mixed solvent comprises a dispergator and deionized water, and the pH value of the second mixed solvent is 10 due to the dispergator.
Preferably, 13.07g of ferric oxide, 0.48g of CMC, 0.03g of Tween-80, 20g of potassium silicate, 0.1g of ethylene glycol and 58g of deionized water with pH 10 prepared by ammonia water are mixed and put into a heat collection type constant temperature heating magnetic stirrer, the rotating speed is 860r/min, the mixture is heated in a water bath at 60 ℃ and stirred for 30min until the solution is clear and transparent, and a first mixed solvent is obtained;
taking out 18.33g of the first mixed solvent for standby;
and manually grinding 1.67g of single-arm carbon nano tube for 5min by using an agate mortar, mixing with 18.33g of the first mixed solvent, continuously using a heat collection type constant-temperature heating magnetic stirrer at the rotating speed of 1000r/min, heating in a water bath at 60 ℃ and stirring for 2h to obtain the final carbon nano tube slurry with strong adhesion.
The carbon nanotube slurry provided by the invention effectively solves the problems that the traditional carbon nanotube slurry has poor adhesion to a glass substrate, is easy to scratch and is easy to strike fire, discharge, ablate and fall off under high pressure, and greatly improves the adhesion of the slurry to the glass substrate.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The carbon nanotube slurry with strong adhesion is characterized by comprising the following raw materials in percentage by mass: 89% -95% of first mixed solvent and 5% -11% of carbon nano tube subjected to grinding and dispersing treatment;
the first mixed solvent comprises the following raw materials in percentage by mass: 50-70% of second mixed solvent, 9-20% of ferric oxide, 0.31-0.62% of dispersant, 0.05-0.1% of flatting agent, 0.02-0.04% of surfactant and 14-28% of binder; the second mixed solvent comprises a dispergator and deionized water, wherein the dispergator enables the pH value of the second mixed solvent to be 7-11.
2. The carbon nanotube slurry with strong adhesion according to claim 1, wherein the ferric oxide is ferric oxide powder.
3. The carbon nanotube slurry with strong adhesion according to claim 1, wherein the dispersant is sodium methyl lignin or sodium calcium lignosulfonate.
4. The carbon nanotube slurry with strong adhesion according to claim 1, wherein the leveling agent is ethylene glycol.
5. The carbon nanotube slurry with strong adhesion according to claim 1, wherein the surfactant is a nonionic surfactant.
6. The carbon nanotube slurry with strong adhesion according to claim 1, wherein the debonder is ammonia.
7. The carbon nanotube slurry with strong adhesion according to claim 1, wherein the binder is sodium silicate and potassium silicate.
8. The carbon nanotube slurry with strong adhesion according to claim 1, wherein the carbon nanotubes are any one selected from single-arm carbon nanotubes and multi-arm carbon nanotubes prepared by any one of arc discharge, laser ablation, solid phase pyrolysis, electrolysis and chemical vapor deposition.
9. A preparation method of carbon nanotube slurry with strong adhesion is characterized by comprising the following steps:
preparing a first mixed solvent: adding a second mixed solvent with the mass percentage of 50% -70%, ferric oxide with the mass percentage of 9% -20%, a dispersing agent with the mass percentage of 0.31% -0.62%, a flatting agent with the mass percentage of 0.05% -0.1%, a surface active agent with the mass percentage of 0.02% -0.04% and a bonding agent with the mass percentage of 14% -28% into a stirrer for first mixing treatment to obtain a first mixed solvent, wherein the second mixed solvent comprises a dispergator and deionized water, and the dispergator enables the pH value of the second mixed solvent to be 7-11;
preparing carbon nanotube slurry: and adding 89-95% by mass of the first mixed solvent and 5-11% by mass of the carbon nano tube subjected to grinding and dispersing treatment into a stirrer for second mixing treatment to obtain the carbon nano tube slurry.
10. The method as claimed in claim 1, wherein the first mixing process comprises heating and stirring in water bath in the stirrer, wherein the rotation speed of the stirrer is 800-.
And/or the second mixing treatment comprises heating and stirring in a water bath in the stirrer, wherein the rotating speed of the stirrer is 800-.
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