CN111211301A - Flexible organic compound/biomass carbon fiber composite material and preparation method thereof - Google Patents
Flexible organic compound/biomass carbon fiber composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a flexible organic compound/biomass carbon fiber composite material and a preparation method thereof. The invention is based on the phase-change method of solution, the raw materials for preparation are easy to purchase, the process is simple and convenient, and the cost is lower. The flexible organic compound/biomass carbon fiber composite material prepared by the method greatly improves the conductivity of the lithium battery, prevents the organic compound from being dissolved in electrolyte in the charging and discharging processes, has excellent flexibility, can be used for preparing the lithium ion battery, has excellent rate capability and cycle stability as the anode material of the lithium ion battery, and does not have any capacity attenuation under the bending condition.
Description
Technical Field
The invention relates to the field of lithium ion battery anode materials, in particular to a flexible organic compound/biomass carbon fiber composite material.
Background
Lithium ion batteries have enjoyed great success in the field of energy storage devices over decades of development. At present, most of electrode materials of lithium ion batteries are inorganic materials, but the application and development of inorganic materials have some inevitable problems, such as: the pollution of waste batteries to the environment, the rising of the price of cobalt-based lithium ion batteries and the like. Therefore, it is a development trend of the present lithium ion battery to search for a substance that can replace an inorganic material in the lithium ion battery. In recent years, the use of organic materials has developed in a well-jet manner, such as; in the fields of photovoltaics, light emitting diodes, field effect transistors and the like, the organic electrochemical active substance is a practical novel anode battery material.
The traditional positive electrode material needs higher production cost, and because the traditional positive electrode material occupies more important components in the lithium ion battery, the preparation of the organic positive electrode material with high performance and low cost is the key for realizing the organic lithium ion battery. The design of the electrode material of the organic lithium ion battery can fully exert the advantages of the organic electrochemical active substance in the aspects of effectively constructing various organic devices, low cost, strong flexibility, solution processability and the like. Compared with the anode of the traditional inorganic lithium ion battery, the organic material has the main characteristic of good compatibility with the flexible polymer, and the anode can work in a bent state, so that the flexibility of the anode material is shown. The organic compound with electrochemical activity and the adhesive are not conductive components in the flexible positive electrode material of the lithium ion battery, so the introduction of the carbon-based conductive agent is an essential part in the positive electrode material of the lithium ion battery.
Carbon black is one of the most commonly used conductive agents in positive electrode materials because of its significant advantages in terms of cost and processability. However, in the current organic electrode materials, the specific gravity of carbon black is high, so that the loading amount of the organic active material is too low. Conversely, nanocarbons with high aspect ratios and high specific surface areas, such as carbon nanotubes and graphene, can easily form an interconnected conductive network or scaffold. The high cost of the nano carbon limits the practical application of the nano carbon in flexible organic cathode materials. Therefore, the development of carbon materials having a high aspect ratio, high conductivity and low cost is an urgent need for the development of a positive electrode material for a flexible organic lithium ion battery.
Disclosure of Invention
Aiming at the defects of the prior art and the requirements of the development of the future lithium ion battery, the application provides the flexible organic compound/biomass carbon fiber composite material for the lithium battery and the preparation method thereof. The flexible organic compound/biomass carbon fiber composite material prepared by the method is used as the anode material of the lithium battery, the conductivity of the lithium battery is greatly improved, the phenomenon that the organic compound is dissolved in electrolyte in the charging and discharging processes is prevented, and more importantly, the flexible organic compound/biomass carbon fiber composite material can keep excellent electrochemical performance under bending.
The invention is realized by the following technical scheme:
a preparation method of a flexible organic compound/biomass carbon fiber composite material comprises the steps of mixing an organic compound, biomass carbon fibers, a binder, a conductive agent and an organic solvent, carrying out ultrasonic treatment, heating and stirring to obtain a suspension, coating, removing the solvent, and carrying out vacuum drying to obtain the flexible organic compound/biomass carbon fiber composite material.
The biomass carbon fiber is obtained by performing anaerobic carbonization on pretreated biomass under oxygen-free airflow, wherein the biomass comprises any one of cotton fiber, bamboo fiber and hemp fiber. Preferably, the biomass carbon fiber obtained by anaerobic carbonization is ground, and the particle size of the biomass carbon fiber is 5-15 microns.
The biomass is preferably cotton fiber. The cotton fiber comprises any one of cotton ball, medical absorbent cotton and cotton linter, the bamboo fiber comprises bamboo chopsticks or bamboo, and the hemp fiber comprises any one of ramie, jute, ramie, hemp, flax, apocynum venetum and hibiscus hemp.
The method for pretreating biomass includes any one of a distilled water washing method, an acid water-distilled water washing method, and an alkaline water-distilled water washing method, and preferably a distilled water washing method. The acid used in the acid water comprises any one of dilute sulfuric acid, dilute hydrochloric acid, dilute nitric acid, dilute acetic acid, dilute hypochlorous acid, carbonic acid and dilute formic acid; the alkali used in the alkaline water comprises any one of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, cesium carbonate, potassium bicarbonate and ammonia water; the concentration of the acid water and the alkaline water is 0.5-20 wt%.
The oxygen-free gas flow comprises any one of nitrogen, carbon dioxide, argon, ammonia and methane, and is preferably nitrogen.
The temperature rise speed in the carbonization process is 5-30 ℃/min, preferably 5 ℃/min, the carbonization temperature is 400-1200 ℃, and preferably 700-900 ℃; the carbonization time is 0.5-6 h, preferably 2 h.
The biomass carbon fiber obtained by carbonization has larger specific surface area and higher aspect ratio, so that the conductivity of the biomass carbon fiber is enhanced on one hand, and the biomass carbon fiber is beneficial to being in full contact with organic compounds and enhancing the conductivity of materials on the other hand.
The organic compound comprises any one of perylene diimides, thiazines, anthraquinones, indigoids or phthalocyanines, the perylene diimides comprise perylene diimide or perylene diimide derivatives, the thiazines are DPP pigments, the anthraquinones comprise anthraquinone or RSN reduction blue, the indigoids comprise any one of indigotin, reduction blue 2B, reduction pink R, reduction purple BBF, reduction scarlet R or reduction black B, and the phthalocyanines comprise any one of nickel phthalocyanine, copper phthalocyanine or iron phthalocyanine.
The binder comprises an oily binder or a water-based binder, the oily binder comprises any one of polyvinylidene fluoride, thermoplastic polyurethane, polytetrafluoroethylene, polyethylene and derivatives thereof and polybutyl acrylate-polyacrylonitrile, and the water-based binder comprises any one of carboxymethyl cellulose, styrene-butadiene rubber, polyacrylic acid and salt binders thereof, polyvinyl alcohol or acrylonitrile multipolymer.
The conductive agent comprises conductive carbon black (Super P), any one of graphene, graphene oxide, reduced graphene, multi-walled carbon nanotubes or single-walled carbon nanotubes, and is preferably conductive carbon black (Super P).
The organic solvent comprises any one of methanol, ethanol, dichloromethane, ethyl acetate, petroleum ether, N-dimethylformamide, N-dimethylacetamide, dimethyl sulfoxide, 1, 2-dichloroethane, acetone, isopropanol, tert-butanol, quinoline and distilled water, and preferably N, N-dimethylformamide.
The volume ratio of the total mass of the organic compound, the biomass carbon fiber, the binder and the conductive agent to the organic solvent is 1 mg: (5-10) mu L.
The mass of the organic compound, the biomass carbon fiber, the binder and the conductive agent in the suspension is (2-4): (2-4): (2-4): 1, preferably 3:3:3: 1.
the ultrasonic time is 20-60 min, the suspension heating mode is oil bath heating, water bath heating, tank heating or electric jacket heating, the heating temperature is 20-90 ℃, the preferred heating temperature is 70 ℃, and the heating and stirring time is 8-20 h.
The coating adopts a wet film preparation device, and the coating thickness is 50-200 mu m, preferably 100-150 mu m.
The solvent is removed by adopting a water bath method, wherein the water bath heating temperature is 25-80 ℃, the preferred temperature is 40 ℃, and the water bath time is 2-8 h.
The vacuum drying temperature is 40-80 ℃, preferably 45 ℃, and the vacuum drying time is 10-20 h.
The organic compound/biomass carbon fiber composite material keeps good mechanical flexibility under the action of the binder and the biomass carbon fiber. The organic compound, the biomass carbon fiber, the binder and the conductive agent are fully mixed in a solution state, and all the components are uniformly dispersed, so that the organic compound is wrapped by the biomass carbon fiber and the conductive agent.
The invention also provides a flexible organic compound/biomass carbon fiber composite material prepared by any one of the methods.
The flexible organic compound/biomass carbon fiber composite material can be used for preparing electrode materials of lithium ion batteries.
The invention also provides a lithium ion battery which comprises the flexible organic compound/biomass carbon fiber composite material.
Compared with the prior art, the invention has the advantages that:
compared with the existing electrode material preparation method, the phase-change method based on the solution realizes one-step preparation of the electrode material, and has the advantages of easily purchased raw materials, simple and convenient process and lower cost. According to the flexible organic compound/biomass carbon fiber composite material prepared by the method, the biomass carbon fiber has a larger specific surface area, so that the conductivity of the electrode material is fully guaranteed, meanwhile, under the action of the binder, the organic compound is in closer contact with the biomass carbon fiber, the conductivity of the organic compound is improved, and the organic compound is prevented from being dissolved in electrolyte in the charging and discharging processes. More importantly, it also exhibits excellent flexibility, maintaining excellent electrochemical performance under bending. Compared with the existing preparation method, the material used as the positive electrode material of the lithium ion battery has excellent rate performance and cycle stability, and does not have any capacity attenuation under the bending condition.
Drawings
Fig. 1 is a process flow chart of a composite flexible organic cathode material prepared from perylene diimide/cotton fibers in example 1 of the present invention.
Fig. 2 is a data diagram of rate capability of a composite flexible organic cathode material prepared from perylene diimide/cotton fibers as a lithium battery cathode material in example 1 of the present invention.
FIG. 3 is a graph of cycle performance data of the perylene diimide/cotton fiber composite flexible material (FOC/CCF) prepared in example 1 of the present invention as a lithium battery positive electrode material.
FIG. 4 is an electron microscope image of the perylene diimide/cotton fiber composite flexible material (FOC/CCF) prepared in example 1 of the present invention, in which FIG. 4(a) is a cross section and FIG. 4(b) is a surface of the material.
FIG. 5 is a flexible display of the perylene diimide/cotton fiber composite flexible material (FOC/CCF) prepared in example 1 of the present invention.
Fig. 6 is a graph of cycle performance data of the perylene diimide/cotton fiber composite flexible material (FOC/CCF) prepared in example 1 of the present invention as a pouch battery positive electrode material under different bending conditions.
FIG. 7 is a molecular structural diagram of the perylene diimide of example 1 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and specific embodiments. It should be understood that the embodiments are illustrative of the invention and are not to be construed as limiting the scope of the invention in any way.
This example is a solution based phase change process. During carbonization, the small molecular compounds in the biomass are pyrolyzed to form a porous structure, and the specific surface area is increased to increase the electrical conductivity of the biomass. In the preparation process of the flexible organic cathode material, N-Dimethylformamide (DMF) is used as a solvent, and an organic compound (perylene diimide), a binder (thermoplastic polyurethane, 100-mesh micro powder from Uniplastication science and technology Co., Ltd. in Dongguan), biomass carbon fiber (cotton fiber) and a conductive agent (conductive carbon black) are combined to form a suspension and coated to form a film, so that the flexible organic cathode material is formed and is directly used for a lithium battery. The polyurethane binder can exhibit good mechanical strength, high resilience, small compression set, high resistance to impact, wear and tear, and the like, which is advantageous for combining the components together, thereby improving the mechanical stability thereof. Compared with the traditional preparation method of the electrode material for coating the active substance on the current collector, the method can greatly increase the mass density of the active substance, reduce the mass of the anode material and increase the use value, and the specific operations are as follows:
(1) adding 100mL of distilled water into a beaker, adding 10g of commercial cotton, stirring for 2 hours at room temperature, filtering and repeatedly washing for 3 times to remove impurities;
(2) putting the washed cotton into a drying oven at 60 ℃ for drying for 12h, putting the dried cotton into a tubular furnace, and carbonizing at the high temperature of 5 ℃/min and 900 ℃ for 2h under the nitrogen airflow;
(3) carbonizing to obtain black biomass carbon fiber, and grinding the biomass carbon fiber clockwise for 10min by using a mortar, wherein the particle size of the biomass carbon fiber is 9 microns. Mixing Perylene Diimide (PDI), biomass carbon fiber, thermoplastic polyurethane and conductive carbon black according to the mass ratio of 3:3:3:1 to obtain a mixture, adding N, N-Dimethylformamide (DMF), wherein the volume ratio of the mass of the mixture to the N, N-Dimethylformamide (DMF) is 1 mg: 6 mu L of the perylene diimide is added into a reaction vessel, is subjected to ultrasonic treatment for 30min, is placed into an oil bath constant temperature heater for heating and stirring, the heating temperature is 70 ℃, the heating and stirring time is 12h, a suspension is prepared, the perylene diimide and the polyurethane are stable and do not react with each other, and therefore, the molecular structure of the perylene diimide is not changed during the preparation process;
(4) uniformly coating the suspension on a polytetrafluoroethylene plate by using a wet film preparation device, wherein the thickness of a coating film is 100 mu m, and then putting the coating film into a water bath kettle, wherein the water bath temperature is 40 ℃, and the water bath time is 8 h.
(5) And (3) peeling off the membrane from the polytetrafluoroethylene plate, and drying in a vacuum drying oven at the drying temperature of 60 ℃ for 12 hours to obtain the perylene diimide/cotton fiber composite flexible organic cathode material (FOC/CCF), as shown in FIG. 4.
As can be seen from FIG. 4(a), the thickness of the perylene diimide/cotton fiber composite flexible material is less than 100 μm and about 52 μm; fig. 4(b) shows that the surface of the electrode exhibits a certain roughness, which is related to the volume change of the material during the DMF solvent removal process, and is favorable for the penetration of the electrolyte into the organic cathode material. From the electron microscope image of the cross section, the perylene diimide, the biomass carbon fiber, the thermoplastic polyurethane and the conductive carbon black are uniformly distributed in the composite material, wherein the perylene diimide is wrapped by the biomass carbon fiber and the conductive carbon black under the action of the polyurethane, so that the flexibility is enhanced while the conductivity of the perylene diimide is greatly improved. The FOC/CCF composite flexible material prepared by the embodiment is used as a positive electrode material of a lithium ion battery for testing, and shows excellent rate performance and cycle stability, as shown in fig. 2 and 3.
As can be seen from FIG. 2, when the current density was 0.05A g-1、0.10A g-1、0.20A g-1、0.50A g-1、1.0A g-1And 2.0A g-1When FOC/CCF is directly used as the anode material of the lithium battery, the specific discharge capacity is respectively 135 mA.h.g-1、122mA·h·g-1、122mA·h·g-1、115mA·h·g-1、110mA·h·g-1And 101 mA. h.g-1。
When the current density is 0.05A g-1The FOC/CCF composite flexible material (the mass contents of perylene diimide and biomass carbon fiber are both 30%) shows excellent specific capacity of 135 mA.h.g-1Close to the theoretical value (137 mA. h.g) of Perylene Diimide (PDI)-1)。
When the current density is 2.0A g-1In time, the specific capacity of the FOC/CCF composite flexible material directly used as the lithium battery anode material can also show 101 mA.h.g-1Has a high reversible specific capacity of 0.05A g-1The specific capacitance under the current density is 75%, which shows that the lithium battery with the FOC/CCF composite flexible material directly used as the anode material has stronger stability under the heavy current and has good cruising ability.
As can be seen from FIG. 3, it is 0.5A g-1Under the condition of charge/discharge current density, the specific capacity of the FOC/CCF composite flexible material directly used as the lithium battery anode material still maintains 102 mA.h.g-1After 600 times of charge-discharge circulation, the specific capacity retention rate is as high as 90.5%, and no obvious decline phenomenon exists.
As can be seen from FIG. 6, the FOC/CCF composite flexible material is assembled into a bag-type battery. When under different bending conditions (0-90-180) and then to original state, the capacity is 0.5A g-1Current ofThe density is always kept at 108 mA.h.g-1And no attenuation shows that the FOC/CCF composite flexible material has excellent flexibility and electrochemical performance.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. A preparation method of a flexible organic compound/biomass carbon fiber composite material is characterized by comprising the steps of mixing an organic compound, biomass carbon fibers, a binder, a conductive agent and an organic solvent, carrying out ultrasonic treatment, heating and stirring to obtain a suspension, coating a film, removing the solvent, and carrying out vacuum drying to obtain the flexible organic compound/biomass carbon fiber composite material;
the biomass carbon fiber is obtained by performing anaerobic carbonization on pretreated biomass under oxygen-free airflow, wherein the biomass comprises any one of cotton fiber, bamboo fiber and hemp fiber;
the organic compound comprises any one of perylene diimides, thiazines, anthraquinones, indigoids or phthalocyanines, the perylene diimides comprise perylene diimide or perylene diimide derivatives, the thiazines are DPP pigments, the anthraquinones comprise anthraquinone or RSN reduction blue, the indigoids comprise any one of indigotin, reduction blue 2B, reduction pink R, reduction purple BBF, reduction scarlet R or reduction black B, and the phthalocyanines comprise any one of nickel phthalocyanine, copper phthalocyanine or iron phthalocyanine.
2. The preparation method of the flexible organic compound/biomass carbon fiber composite material according to claim 1, wherein the oxygen-free gas flow comprises nitrogen, carbon dioxide, argon, ammonia and methane, the temperature rise rate in the carbonization process is 5-30 ℃/min, the carbonization temperature is 400-1200 ℃, and the carbonization time is 0.5-6 h.
3. The flexible organic compound/biomass charcoal fiber composite material for a lithium battery according to claim 1, wherein the binder comprises an oily binder or an aqueous binder, the oily binder comprises any one of polyvinylidene fluoride, thermoplastic polyurethane, polytetrafluoroethylene, polyethylene and derivatives thereof, and polybutyl acrylate-polyacrylonitrile, and the aqueous binder comprises any one of carboxymethyl cellulose, styrene-butadiene rubber, binders of polyacrylic acid and salts thereof, polyvinyl alcohol, or acrylonitrile multipolymer;
the conductive agent comprises any one of conductive carbon black, graphene oxide, reduced graphene, multi-walled carbon nanotubes or single-walled carbon nanotubes;
the organic solvent comprises any one of methanol, ethanol, dichloromethane, ethyl acetate, petroleum ether, N-dimethylformamide, N-dimethylacetamide, dimethyl sulfoxide, 1, 2-dichloroethane, acetone, isopropanol, tert-butanol, quinoline and distilled water.
4. The flexible organic compound/biomass charcoal fiber composite material for a lithium battery according to claim 1, wherein the volume ratio of the total mass of the organic compound, the biomass charcoal fiber, the binder and the conductive agent to the organic solvent is 1 mg: (5-10) mu L.
5. The flexible organic compound/biomass charcoal fiber composite material for the lithium battery as claimed in claim 1, wherein the mass of the organic compound, the biomass charcoal fiber, the binder and the conductive agent in the suspension is (2-4): (2-4): (2-4): 1.
6. the preparation method of the flexible organic compound/biomass carbon fiber composite material as claimed in claim 1, wherein the ultrasonic time is 20-60 min, the suspension heating mode is oil bath heating, water bath heating, closed tank heating or electric jacket heating, the heating temperature is 20-90 ℃, the heating and stirring time is 8-20 h, the coating film is prepared by a wet film preparation device, and the coating film thickness is 50-200 μm.
7. The preparation method of the flexible organic compound/biomass carbon fiber composite material according to claim 1, wherein the solvent removing method adopts a water bath method, wherein the water bath heating temperature is 25-80 ℃, the water bath time is 2-8 h, the vacuum drying temperature is 40-80 ℃, and the vacuum drying time is 10-20 h.
8. A flexible organic compound/biomass carbon fiber composite material, characterized in that it is prepared by the method of any one of claims 1 to 7.
9. The use of the flexible organic compound/biomass charcoal fiber composite material of claim 8 in the preparation of lithium ion battery electrode materials.
10. A lithium ion battery comprising using the flexible organic compound/biomass charcoal fiber composite material according to claim 8.
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| CN111900482A (en) * | 2020-06-22 | 2020-11-06 | 武汉瑞科美新能源有限责任公司 | Production method of flexible integrated battery cell |
| CN114031076A (en) * | 2021-11-09 | 2022-02-11 | 四川金时新能科技有限公司 | Biomass superstructure carbon, and preparation method and application thereof |
| CN114204019A (en) * | 2021-11-23 | 2022-03-18 | 五邑大学 | Battery positive electrode material and preparation method and application thereof |
| CN115532238A (en) * | 2022-09-13 | 2022-12-30 | 徐州工程学院 | Agricultural wastewater modified biological adsorbent and preparation method and application thereof |
| US11721455B1 (en) | 2023-01-19 | 2023-08-08 | King Abdulaziz University | Organic resistor |
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| CN115532238B (en) * | 2022-09-13 | 2023-10-27 | 徐州工程学院 | Agricultural wastewater modified biological adsorbent and preparation method and application thereof |
| US11721455B1 (en) | 2023-01-19 | 2023-08-08 | King Abdulaziz University | Organic resistor |
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