CN103426498A - Carbon nanotube conductive slurry and method for preparing carbon nanotube conductive slurry - Google Patents
Carbon nanotube conductive slurry and method for preparing carbon nanotube conductive slurry Download PDFInfo
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Abstract
The invention belongs to the technical field of electrochemical materials, and particularly relates to carbon nanotube conductive slurry and a method for preparing the carbon nanotube conductive slurry. The carbon nanotube conductive slurry is mainly composed of carbon nanotubes, other conductive fillers, dispersing auxiliaries and a solvent, and the carbon nanotube conductive slurry comprises the components, by mass, 0.5-15% of the carbon nanotubes, 0.1-2% of the other conductive substances, 0.1-5% of the dispersing auxiliaries and the balance being solvent. The method for preparing the carbon nanotube conductive slurry includes the steps that firstly the dispersing auxiliaries are dissolved in the solvent, then, the carbon nanotubes and the other conductive fillers are added under the stirring condition, after the carbon nanotubes and the other conductive fillers are fully immersed, a sand mill is utilized to grind the slurry, and the stable and dispersing carbon nanotube conductive slurry can be obtained after the slurry is grinded for a few hours. The method is simple and free of damaging the structures and the electrical conductivity of the carbon nanotubes, the prepared carbon nanotube conductive slurry has good electrical conductivity and is stable and uniform in property, and the stability of the slurry is larger than 90% after standing for 3 months.
Description
Technical field
The invention belongs to the electrochemical material technical field, be specifically related to a kind of carbon nanotube conducting slurry and preparation method thereof, this material can be used as the negative or positive electrode that conductive agent is applied to lithium rechargeable battery, capacitor.
Background technology
In the preparation process of lithium rechargeable battery and capacitor, often need in the both positive and negative polarity batching, add a certain amount of conductive agent.Conductive agent can effectively contact with the both positive and negative polarity active material, forms good conductive network, thereby improves the high rate performance of battery.But add too much conductive agent, certainly will reduce electrode active material content, reduce capacity and the energy density of battery.For high performance electronic equipment, select suitable conductive agent particularly important.
Carbon nano-tube is in recent years emerging conductive agent, its general diameter is in 5 ~ 60 nanometer left and right, length reaches 10 ~ 20 microns, it not only can serve as the effect of " wire " in conductive network, and it also has the electric double layer effect simultaneously, the high magnification characteristic of performance ultracapacitor, heat radiation when its good heat conductivility also helps battery charging and discharging, reduce the polarization of battery, improve the high temperature performance of battery, extend the life of a cell.
(Journal of Power Sources 2008,184 522-526.) has reported the C-LiFePO that multi-walled carbon nano-tubes (MWNTs) and carbon black are conductive agent to the people such as Liu
4/ graphite battery performance.With carbon black, compare, the battery that the MWNTs of take is additive has more excellent chemical property: it is 94.6% of 0.1C that 50 circulation volume conservation rates reach 99.2%, 1C discharge capacity.Polarizing voltage has been reduced to 0.2V from 0.3V, and impedance has been reduced to 36.88 Ω from 423.2 Ω.Positive electrode LiFePO after circulation
4Crystal formation keep also better.The people such as Jin (Journal of Solid State Electrochemistry 2008,12,1549-1554.) studied employing acetylene black and MWNTs as anodal conductive agent to LiFePO
4The impact of-C positive electrode chemical property.Add the LiFePO of 5wt% MWNTs
4-C/Li battery performance is the most excellent, and under room temperature, 0.25C can reach the reversible capacity of 142mAh/g.
Yet, because carbon nano-tube has stronger Van der Waals force each other, can mutual entanglement aggregate (Fig. 1) together, be difficult to be dispersed in the positive and negative electrode material, thus affected carbon nano-tube conductive can performance.Therefore, how preparing homodisperse carbon nanotube conducting slurry is a major obstacle that limits its commercial application.At present, solve the carbon nanotube dispersed problem and mainly contain chemistry and two kinds of methods of physics.Although chemical method can obtain the good carbon nano-tube of dispersive property as the acid with strong oxidizing property processing method, the structure that strong acid also can destroying carbon nanometer tube, shortening carbon nano-tube, thus affect the conductivity of carbon nano-tube and as the performance of conductive agent.More ultrasonic processing method efficiency is low, dispersion effect is poor, stability as adopted for physical method, and the carbon nano tube dispersion liquid concentration obtained is difficult to prepare on a large scale the dispersed paste of carbon nano-tube lower than 5mg/mL.
In the present invention, we have proposed a kind of simple new method for preparing the carbon nanotube conducting slurry, and preparation process is reproducible, and the carbon nanotube conducting slurry solid content made is high, the stable in properties homogeneous, and after standing 3 months, Stability of Slurry > 90%.
Summary of the invention
The object of the present invention is to provide a kind of carbon nanotube conducting slurry.
Another object of the present invention is to provide a kind of preparation method of carbon nanotube conducting slurry.
Carbon nanotube conducting slurry proposed by the invention, its characteristics are that this electrocondution slurry is by carbon nano-tube, other conductive fillers, dispersing aid and solvent composition, its mass percent consists of: carbon nano-tube: 0.5 ~ 15%, other conductive fillers 0.1 ~ 2%, dispersing aid: 0.1 ~ 5%, all the other are solvent.
Described carbon nano-tube is one or both mixing in Single Walled Carbon Nanotube or multi-walled carbon nano-tubes.
Described other conductive fillers are one or more in carbon black, acetylene black, carbon fiber or electrically conductive graphite.
Described dispersing aid is one or more in PVP (PVP), polyvinyl alcohol (PVA) or CMC (CMC).
Described solvent is 1-METHYLPYRROLIDONE (NMP) or water.
The preparation method of carbon nanotube conducting slurry proposed by the invention, its characteristics are that step is as follows: at first dispersing aid is dissolved in solvent, then add carbon nano-tube and other conductive fillers under stirring condition, after carbon nano-tube and other conductive fillers fully infiltrate, adopt sand mill to be ground slurry, can obtain the carbon nanotube conducting slurry of stable dispersion after several hours.Be specially,
(1) take a certain amount of dispersing aid, be dissolved in solvent, be configured to the solution that percentage by weight is 0.1 ~ 5%; Under the mechanical agitation condition, add the mixture of other conductive fillers that carbon nano-tube that percentage by weight is 0.5 ~ 15% or carbon nano-tube and percentage by weight are 0.1 ~ 2%, fully stir, make the pressed powder complete wetting, make the carbon nano-tube pre-dispersed liquid.
(2) the carbon nano-tube pre-dispersed liquid is used to sand mill grinding distribution 0.5 ~ 8 hour, can obtain the carbon nanotube conducting slurry of stable dispersion.
The diameter of described sand mill zirconia ball used is 0.1 ~ 3mm.
The inventive method is simple, not destroying carbon nanometer tube structure and conductivity, and prepared carbon nanotube conducting slurry has good conductivity, and the stable in properties homogeneous, after standing 3 months, Stability of Slurry > 90%.
Compare the strong acid oxidation or the ultrasonic aid dispersion method that adopt at present both at home and abroad, the present invention has following characteristics: (1) is the destroying carbon nanometer tube structure not, can effectively open the aggregation (Fig. 2) of carbon nano-tube; (2) the carbon nanotube conducting size performance obtained stable (after standing 3 months, stability > 90%), have higher solid content (0.5 ~ 15%).
The accompanying drawing explanation
Fig. 1. carbon nanotube agglomerate SEM photo.This result shows the easy reunion of carbon nano-tube together, the aggregation that the formation diameter is 10-1000 μ m.
Fig. 2. carbon nanotube conducting slurry SEM photo.This result shows that in prepared carbon nano tube paste, carbon nanotube agglomerate is fully opened, and forms the carbon nanotube conducting network be closely connected.
Fig. 3 .(A-F) carbon nano-tube premix slurry and 1-5 hour ground slurry coating post-drying photo.The premix pulp surface is coarse, and obvious caking phenomenon is arranged, and along with milling time increases, the slurry coating surface is tending towards smooth, homogeneous.This result shows the growth along with milling time, and the carbon nanotube conducting slurry disperses more even.
Fig. 4. carbon nano-tube upper strata slurry solid content variation diagram.Inactive slurry 40 days or adopt respectively 3000,6000,12000rpm centrifugal treating slurry, the solid content of measuring the upper strata slurry changes little with initial solid content.This result shows that prepared carbon nano tube paste has good stability.
Fig. 5. based lithium-ion battery positive plate SEM photo.From photo, see, even carbon nanotube is dispersed between the iron phosphate serving as positive active material particle, has formed three-dimensional conductive network.
Embodiment
Embodiment 1: in the container of 20 liters, add the 9.25kg 1-METHYLPYRROLIDONE as solvent carrier, add wherein the 0.15kg PVP as auxiliary agent.In under 6000rpm mechanical agitation condition, PVP fully being dissolved in to 1-METHYLPYRROLIDONE.Then add the 0.6kg multi-walled carbon nano-tubes in solution in batches, after added pressed powder is fully wetting by solvent, add again the remainder carbon nano-tube.After all adding, continue mechanical agitation 15min, obtain pre-dispersed slurry.The pre-dispersed slurry of carbon nano-tube is transferred in nanometer sand mill, adopts the zirconia ball that diameter is 1mm, under 2400rpm, grind and within 2 hours, obtain carbon nano tube paste.
The pre-dispersed slurry of carbon nano-tube per hour reaches ground slurry and coats the rear photo of slide oven dry as shown in Figure 3.Adopt respectively centrifugal and standing survey upper strata slurry solid content method to characterize carbon nano tube paste stability, as shown in Figure 4.
Embodiment 2: in the container of 20 liters, add 9.4kg water as solvent carrier, add wherein the 0.1kg CMC as auxiliary agent.Under 5000rpm mechanical agitation condition, CMC fully is dissolved in the water.Then add 0.17kg Super-p nanometer acetylene black conductor and 0.33kg Single Walled Carbon Nanotube in solution in batches, after added pressed powder is fully wetting by solvent, add again the remainder combined conductive agent.After all adding, continue mechanical agitation 15min, obtain pre-dispersed slurry.The pre-dispersed slurry of carbon nano-tube is transferred in sand mill, adopts the zirconia ball that diameter is 0.3mm, under 1800rpm, grind and within 5 hours, obtain carbon nano-tube composite conducting slurry.
Embodiment 3: take the 9.4kg deionized water as solvent carrier in the container of 20 liters, add wherein the 0.1kg PVP as auxiliary agent.Under 3000rpm mechanical agitation condition, PVP fully is dissolved in the water.Then add the 0.5kg multi-walled carbon nano-tubes in solution in batches, after added pressed powder is fully wetting by solvent, add again the remainder carbon nano-tube.After all adding, continue mechanical agitation 15min, obtain pre-dispersed slurry.The pre-dispersed slurry of carbon nano-tube is transferred in sand mill, adopts the zirconia ball that diameter is 0.6mm, under 1500rpm, grind and within 0.5 hour, obtain carbon nano-tube composite conducting slurry.
Embodiment 4: take the 9.4kg 1-METHYLPYRROLIDONE as solvent carrier in the container of 20 liters, add wherein the 0.1kg polyvinyl alcohol as auxiliary agent.In under 4000rpm mechanical agitation condition, polyvinyl alcohol fully being dissolved in to 1-METHYLPYRROLIDONE.Then add 0.17kg Super-p nanometer acetylene black conductor and 0.33kg multi-walled carbon nano-tubes in solution in batches, after added pressed powder is fully wetting by solvent, add again the remainder combined conductive agent.After all adding, continue mechanical agitation 30min, obtain pre-dispersed slurry.The pre-dispersed slurry of carbon nano-tube is transferred in sand mill, adopts the zirconia ball that diameter is 0.8mm, under 1200rpm, grind and within 6 hours, obtain carbon nano-tube composite conducting slurry.
Embodiment 5: take 9.4kg water as solvent carrier in the container of 20 liters, add wherein 0.05kg polyvinyl alcohol and 0.05kg PVP as auxiliary agent.Under 4000rpm mechanical agitation condition, polyvinyl alcohol and PVP fully are dissolved in the water.Then add 0.17kg Super-p nanometer acetylene black conductor and 0.33kg multi-walled carbon nano-tubes in solution in batches, after added pressed powder is fully wetting by solvent, add again the remainder combined conductive agent.After all adding, continue mechanical agitation 5min, obtain pre-dispersed slurry.The pre-dispersed slurry of carbon nano-tube is transferred in sand mill, adopts the zirconia ball that diameter is 0.2mm, under 1900rpm, grind and within 4.5 hours, obtain carbon nano-tube composite conducting slurry.
Claims (2)
1. a carbon nanotube conducting slurry, it is characterized in that, this electrocondution slurry is mainly by carbon nano-tube, other conductive fillers, dispersing aid and solvent composition, its mass percent consists of: carbon nano-tube: 0.5～15%, other conductive materials 0.1～2%, dispersing aid: 0.1～5%, all the other are solvent, described carbon nano-tube can stably be dispersed in solvent, sedimentation rate in 3 months<10%;
Wherein, carbon nano-tube is one or both mixing in Single Walled Carbon Nanotube or multi-walled carbon nano-tubes;
Other conductive fillers are one or more in carbon black, acetylene black, carbon fiber or electrically conductive graphite;
Dispersing aid is one or more in PVP, polyvinyl alcohol or CMC;
Described solvent is 1-METHYLPYRROLIDONE or water.
2. the preparation method of a carbon nanotube conducting slurry as claimed in claim 1, is characterized in that, it comprises step:
(1) take a certain amount of dispersing aid, be dissolved in solvent, be configured to the solution that contains dispersing aid; Under the mechanical agitation condition, add carbon nano-tube or carbon nano-tube and other conductive fillers, fully stir, make the pressed powder complete wetting, make the carbon nano-tube pre-dispersed liquid.
(2) the carbon nano-tube pre-dispersed liquid is used to sand mill grinding distribution 0.5～8 hour, make the carbon nanotube conducting slurry of stable dispersion; Wherein the diameter of sand mill zirconia ball used is 0.1～3mm.
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