CN110335764B - Pre-sodium treatment method for efficiently constructing sodium ion capacitor - Google Patents
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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Abstract
The invention discloses a pre-sodium method for efficiently constructing a sodium ion capacitor. The method comprises the steps of coating organic sodium salt and activated carbon as active substances, a binder and a conductive agent on a metal current collector by a coating method to prepare a composite positive electrode; with anatase TiO2Or a porous carbon material is used as an active substance, a binder and a conductive agent and is coated on a metal current collector by a coating method to prepare a negative electrode; after the composite positive electrode and the negative electrode are assembled into a sodium ion capacitor, charge and discharge circulation is carried out through a cyclic voltammetry method, and pre-sodium treatment of the negative electrode is realized. The method utilizes organic sodium salt as a positive active substance to construct the sodium ion capacitor, realizes effective and safe pre-sodium treatment of a negative electrode through an electrochemical method, and obtains the sodium ion capacitor with excellent electrochemical performance and good circulation stability.
Description
Technical Field
The invention relates to a sodium ion capacitor cathode pre-sodium treatment method, in particular to a method for obtaining a sodium ion capacitor with good electrochemical performance and good circulation stability by constructing a sodium ion capacitor to carry out high-efficiency pre-sodium treatment on a cathode, and belongs to the technical field of electrochemical energy storage.
Background
The novel ionic capacitor (lithium ion capacitor or sodium ion capacitor) is composed of a battery type cathode and a capacitance type anode, and has huge application prospect in the fields of electric automobiles, medical equipment, national power grids and aerospace and aviation due to the advantages of high energy density, high power density and long cycle stability. However, in order to enlarge the voltage window of the novel ion capacitor to reduce the electrolyte digestion in the electrolyte, the negative electrode must be subjected to pre-intercalation ion treatment. Currently, commercial lithium ion capacitors can achieve a prelithiation process by applying stable and passivated metallic lithium particles to the surface of the negative electrode graphite layer. The lithium ion capacitor obtained by the method has good and stable electrochemical performance. Currently, sodium ion capacitors are receiving widespread attention and have bright commercial prospects because of their lithium ion-like physicochemical properties and abundant storage in the earth's crust. However, the melting point of the metal sodium is low, the texture is soft and the hardness is low, no technology can be used for producing metal sodium sheets for laboratory use or commercialization in the current market, particularly, the metal sodium is used as one of alkali metal elements, the chemical property is extremely active, and the metal sodium can react with water to generate hydrogen, so that the potential safety hazard is caused. At present, an effective method for constructing a sodium ion capacitor by utilizing a pre-sodium treatment technology does not exist.
Disclosure of Invention
Aiming at the defects in the prior art, the first purpose of the invention is to provide a method for constructing a sodium ion capacitor by using an organic sodium salt as a positive active material, realizing effective and safe pre-sodium treatment of a negative electrode through an electrochemical method, and obtaining the sodium ion capacitor with good electrochemical performance and good circulation stability.
In order to achieve the technical purpose, the invention provides a pre-sodium treatment method for efficiently constructing a sodium ion capacitor, which comprises the following steps:
1) coating organic sodium salt and activated carbon as active substances, a binder and a conductive agent on a metal current collector by a coating method to prepare a composite positive electrode;
2) with anatase TiO2Or a porous carbon material is used as an active substance, a binder and a conductive agent and is coated on a metal current collector by a coating method to prepare a negative electrode;
3) after the composite positive electrode and the negative electrode are assembled into a sodium ion capacitor, charge and discharge circulation is carried out through a cyclic voltammetry method, and pre-sodium treatment of the negative electrode is realized.
In a preferred embodiment, the organic sodium salt includes at least one of sodium rose bengal, disodium crotonate, 1, 2-dicarbonyl-3, 4-dihydroxy-3-cyclobutene disodium salt, tetrahydroxybenzoquinone disodium salt, and tetrahydroxybenzoquinone tetrasodium salt. The preferable organic sodium salt is strong polar organic sodium salt which is not easy to dissolve in the electrolyte solvent, and the reduction product formed after sodium removal is generally neutral organic matter and can be well dissolved in the electrolyte solvent, thereby ensuring the smooth proceeding of sodium dissociation and pre-sodium treatment reaction. In addition, the preferred organic sodium salts have a relatively large theoretical specific capacity (about 250mAh g)-1) And has low price and easy preparation.
In a preferred embodiment, the composite positive electrode comprises the following active materials in percentage by mass: 30 to 70 percent of organic sodium salt; 70-30% of activated carbon (commercial product).
In a preferred embodiment, the negative electrode comprises the following active materials in percentage by mass: 65-75% of active substance, 15-25% of conductive agent and 5-15% of binder.
In a preferred scheme, the composite positive electrode comprises the following active substances, a binder and a conductive agent in percentage by mass: 70-90% of active substance, 5-15% of conductive agent and 5-15% of binder.
In a more preferred embodiment, the conductive agent in the composite positive electrode and negative electrode is conductive carbon black (a commercial product)
More preferably, the binder in the negative electrode is CMCC (carboxymethyl cellulose).
In a more preferred embodiment, the binder in the composite positive electrode is PVDF (polyvinylidene fluoride).
More preferably, the porous carbon material is prepared by the following method: calcining, carbonizing and pickling the ethylenediaminetetraacetic acid tetrasodium salt at 700-900 ℃ in a protective atmosphere to obtain the ethylenediaminetetraacetic acid tetrasodium salt. The carbonization time is 1-3 hours. The porous carbon material prepared by directly carbonizing the ethylenediaminetetraacetic acid tetrasodium salt has excellent performance, is particularly suitable for serving as a negative active material of a sodium-ion battery, and does not need to additionally add a template agent, a catalyst and other organic carbon sources in the preparation process.
In the preferred scheme, the charge-discharge cycle is carried out by cyclic voltammetry, and the conditions for realizing the pre-sodium treatment of the cathode are as follows: selecting Cyclic Voltammetry (CV) method at a scanning speed of 5mV s-1In the voltage range of 0-4V (for carbon material) or 2-4.5V (for TiO)2) And scanning for 5 circles, and standing for 10-15 hours after scanning.
According to the technical scheme, the organic sodium salt is used as an active substance of the anode material and is added into the anode active carbon material, so that the organic sodium salt is introduced into a sodium ion capacitor system, and sodium ions dissociated by the organic sodium salt enter the cathode material in the charge-discharge process of the sodium ion capacitor, so that the pre-sodium treatment process of the cathode material is realized. Compared with the prior art, the pre-sodium treatment process has more convenient operation condition and easy operation, can be carried out under the external atmospheric condition, does not need to be carried out in a specific anhydrous and anaerobic environment, and is safe and effective; the applicable variety of the organic sodium salt can be expanded, the organic sodium salt which is dissolved or not dissolved in the electrolyte can be selected to adapt, most of the existing organic sodium salts are polar ionic compounds and are not easy to dissolve in a nonpolar electrolyte solvent, and the selected variety of the organic sodium salt can be expanded by compounding the organic sodium salt serving as a positive electrode active substance with an active carbon material; and the sodium ion capacitor which can be used and has stable cycle performance is obtained after pre-sodium treatment.
Compared with the prior art, the technical scheme of the invention has the following advantages:
1. the organic sodium salt adopted by the invention is used as a pre-sodium source, compared with metal sodium, the organic sodium salt is safe and low in cost, the generated economic value benefit is high, the sodium source is not limited to sodium salt with good solubility in electrolyte, and the selection range of the organic sodium salt is expanded.
2. The pre-sodium treatment process adopted by the invention is completed in one step, and the method has the advantages of simple operation, short period and low cost, and meets the requirements of industrial production.
3. The sodium ion capacitor subjected to pre-sodium treatment has good electrochemical performance and stable cycle performance.
Drawings
Figure 1 shows the electrochemical behavior diagram of sodium rose bengal: (a) at 5mV s-1CV plot at scan speed, (b) at 25mAg-1GCD plot at current density.
Figure 2 is an ex-situ X-ray powder diffraction pattern of the sodium rose-bengal acid positive electrode at different voltages during the first charge-discharge cycle.
[ FIG. 3 ] NHPC-800// AC/Na2C6O6CV activation pattern of assembled sodium ion capacitor.
FIG. 4 (a) NHPC-800// AC/Na2C6O6CV plot at different scanning speeds of SIC-40%, (b) NHPC-800// AC/Na2C6O6GCD plot at different current densities of SIC-40%, (c) NHPC-800// AC/Na2C6O6Ragon comparison graph of sodium ion capacitor for different ratios and pre-modified NHPC-800// AC.
FIG. 5 (a) TiO2//AC/Na2C6O6CV activation pattern of assembled sodium ion capacitor. (b) TiO 22//AC/Na2C6O6And pre-modified TiO2Ragon comparison of sodium ion capacitor of// AC.
Detailed Description
The present invention will be further described with reference to the following specific examples. These examples are to be construed as merely illustrative and not limitative of the remainder of the disclosure in any way whatsoever. After reading the description of the present invention, various changes or modifications made based on the principle of the present invention also fall within the scope of the present invention as defined in the appended claims
Example 1
(taking rose sodium erythronate as an example)
1. Preparation of the Positive electrode
1.1 preparation of the rose sodium positive electrode:
taking 70 wt% of prepared rose sodium oxide as an active substance, 10 wt% of PVDF as an adhesive, 20 wt% of Super P as a conductive agent and a small amount of N-methylpyrrolidone, placing the mixture in an agate mortar, carefully grinding the mixture until the slurry is uniform, coating the obtained slurry on an Al foil, and drying the Al foil in vacuum at the temperature of 80 ℃ for 12 hours to obtain the positive pole piece to be tested.
1.2 activated carbon and sodium rose bengal Anode (AC/Na)2C6O6) The preparation of (1):
this method is similar to the above-described method for preparing the positive electrode: except that the total amount of the activated carbon and the sodium rhodizonate accounts for 80 wt% on the basis of 10 wt% of PVDF as a binder and 10 wt% of Super P as a conductive agent, and the corresponding mass ratios of the activated carbon and the sodium rhodizonate are 5:3, 4:4 and 3: 5.
2. Preparation of the negative electrode
The method of preparing the negative electrode is similar to the method of preparing the positive electrode described above: except that the slurry was mixed by grinding 70 wt% of the active material, 15 wt% of the CMCC binder, 15 wt% of the Super P conductive carbon and a little distilled water, and then coated on the Cu foil.
The negative active materials used were respectively commercialized anatase TiO2And a porous carbon material (NHPC-800) which was self-made in the laboratory. Preparation of NHPC-800 sample: calcining ethylenediaminetetraacetic acid tetrasodium salt for 2 hours at 800 ℃ in a protective atmosphere, adding acid for washing, and drying in vacuum to obtain the product.
3. Electrochemical testing:
for testing of half-cell, the cut organic sodium salt positive electrode was used as working electrode, the metallic Na plate was used as counter electrode and reference electrode, 1mol L-1NaClO4The volume ratio of the electrolyte to the membrane is 1:1:1, the electrolyte is ethylene carbonate, methyl ethyl carbonate and dimethyl carbonate, Whatman GF/C glass fiber membrane is used as a diaphragm, and a CR2016 battery shell is selected for assembly in a glove box.
And constructing the cut negative electrode, the organic sodium salt and the active carbon positive electrode into a sodium ion capacitor according to a certain mass ratio. The constructed sodium ion capacitor adopts a Cyclic Voltammetry (CV) test method, and the scanning speed is 5mVs-1In the voltage range of 0-4V (for carbon material) or 2-4.5V (for TiO)2) Scan 5 passes. After the scanning is finished and the standing is carried out for 12 hours, the in-situ pre-sodium treatment process can be realized.
In the invention, sodium rose oxide is selected as the positive electrode additive, and the electrochemical performance of the half cell is firstly carried out. As can be seen from FIG. 1a, relative to Na+In terms of the/Na potential, sodium rose bengal shows two anodic peaks at the 3.60V and 3.98V positions in the CV diagram of the first cycle, respectively, which may correspond to two sodium ion-depleted peaks in sodium rose bengal, respectively. The corresponding two peaks of the first cycle are not obvious in the subsequent second and third cycles, which shows that the sodium removing reaction of the sodium rose bengal is irreversible, and the removed sodium ions can not return to the original substance under high pressure. On the other hand, the product obtained after removing two sodium ions from the sodium rose oxide is cyclohexadenone, and the cyclohexadenone can be dissolved in the organic electrolyte, so that the forward progress of the reaction is promoted. At the same time, as can be seen from fig. 1b, the specific charge capacity of the first turn is about 309.8mAh g-1And the discharge specific capacity of the first ring is rapidly reduced to 24.9mAh g-1. This phenomenon further indicates that the sodium-removing reaction of sodium rosette under high pressure is irreversible, and the sodium-removing reaction has very high capacity, and is a novel and considerable pre-sodium treatment additive.
To demonstrate that the sodium rose bengal de-sodication reaction at high pressure is irreversible. We performed characterization analysis by ex situ X-ray powder diffraction testing. As can be seen from fig. 2, the intensity of the sodium rose bengal acid pole piece at the three peaks at about 26.6 °, 29.45 ° and 38.9 ° decreases significantly with increasing charging voltage during the first cycle of charging, indicating that the sodium rose bengal acid undergoes a sodium elimination reaction during charging, while the intensity of the corresponding three peaks does not increase significantly after subsequent first cycle discharge, indicating that the reaction is irreversible. After cycling, the intensity of the three XRD peaks of the pole piece at 26.6 deg., 29.45 deg. and 38.9 deg. was very small, more than sufficient to indicate that the reaction was irreversible, and the sodium removal process occurred mainly in the first cycle.
To verify that sodium rose bengal is an applicable additive in sodium ion capacitors. Adding sodium rosmarinate to the slurry at a ratio of 30%, 40% and 50% by weight of the slurryAnd (3) assembling the carbon with a negative electrode of NHPC-800 prepared in a laboratory to obtain the corresponding sodium ion capacitor. The open circuit voltage of the freshly assembled sodium ion capacitor is about-0.05V because the pre-sodium process cannot spontaneously occur. In order to achieve pre-sodium treatment of sodium ion capacitors, an in-situ one-step electrochemical treatment is necessary. The method selects a Cyclic Voltammetry (CV) test method, and the scanning speed is 5mV s-1Scanning 5 turns in the corresponding voltage interval. After scanning, the mixture was left standing for 12 hours. And fig. 3 is a corresponding CV diagram, and it can be seen from the diagram that the area of the first-ring CV is much larger than the CV areas of the second ring and the third ring, and the first-ring CV diagram has an obvious oxidation peak around 3V, which indicates that the assembled sodium ion capacitor has an irreversible sodium removal reaction in the first-ring CV cycle, and a sodium ion capacitor with normal electrochemical behavior is obtained after the sodium removal reaction. After the circular standing, the open-circuit voltage of the sodium ion capacitor is about 1.3V, which shows that the previous electrochemical treatment proves that the sodium ions of the sodium rosette in the anode move to the cathode NHPC-800 material, so that the effective pre-sodium treatment process is realized, and the usable sodium ion capacitor is obtained.
The mass ratio of the pre-sodium agent is very important in a positive electrode system, and is one of important indexes for measuring commercial sodium ion capacitors. Three of the components are 30% of rose bengal acid sodium and 50% of active carbon; 40% of rose bengal acid sodium and 40% of active carbon; the coating ratio of 50% sodium rose bengal and 30% activated carbon was used as a positive electrode, and the mass ratio of the additives was investigated to find the most excellent mass ratio of the additives. Fig. 4a and 4b are cyclic voltammetry and constant current charge-discharge graphs of a sodium ion capacitor assembled by 40% of sodium rose oxide and 40% of activated carbon in mass ratio as a positive electrode and a negative electrode of NHPC-800, and as can be seen from the graphs, the graphs are corresponding slightly deformed quasi-rectangular CV curves and non-completely linear constant current charge-discharge curves, and the phenomenon indicates that two energy storage mechanisms of Faraday behavior and non-Faraday behavior exist in the sodium ion capacitor system. As can be seen from FIG. 4c, the assembled in-situ pre-sodium-treated sodium ion capacitor is more suitable for the corresponding sodium ion battery than the negative electrode after the half-cell cyclic pre-sodium treatmentThis indicates that the pre-sodium treatment method provided by the invention is feasible, and the sodium ion capacitor after in-situ pre-sodium treatment is successful has excellent performance. In order to expand the adaptability of the method, the invention also selects the commercialized anatase TiO2The material serves as the negative electrode of the sodium ion capacitor. As can be seen in FIG. 5a, the assembled TiO2The sodium ion capacitor system as the cathode also successfully generates an in-situ pre-sodium treatment process, and realizes the TiO pre-sodium treatment2Pre-sodium treatment of the material. At the same time, in TiO2In-situ pre-sodium ion capacitor (TiO) assembled as negative electrode in sodium ion capacitor system2//AC/Na2C6O6SIC) is slightly poorer than the performance of a corresponding sodium ion capacitor assembled by a negative electrode subjected to half-cell circulating pre-sodium treatment, which shows that the pre-sodium treatment method provided by the invention has adaptability and can be applied to carbon and TiO2And the like, and the sodium ion capacitor after in-situ pre-sodium treatment is successful has excellent performance.
Claims (7)
1. A pre-sodium treatment method for efficiently constructing a sodium ion capacitor is characterized by comprising the following steps: the method comprises the following steps:
1) coating organic sodium salt and activated carbon as active substances, a binder and a conductive agent on a metal current collector by a coating method to prepare a composite positive electrode;
2) with anatase TiO2Or a porous carbon material is used as an active substance, a binder and a conductive agent and is coated on a metal current collector by a coating method to prepare a negative electrode;
3) after the composite positive electrode and the negative electrode are assembled into a sodium ion capacitor, charge and discharge circulation is carried out through a cyclic voltammetry method, and pre-sodium treatment of the negative electrode is realized.
2. The method of claim 1, wherein the pre-sodium treatment is carried out by: the organic sodium salt comprises at least one of rose bengal sodium, disodium crotonate, 1, 2-dicarbonyl-3, 4-dihydroxy-3-cyclobutene disodium salt, tetrahydroxybenzoquinone disodium salt and tetrahydroxybenzoquinone tetrasodium salt.
3. The method of claim 1, wherein the pre-sodium treatment is carried out by: the composite positive electrode comprises the following active substances in percentage by mass: 30-70% of organic sodium salt and 70-30% of active carbon.
4. The method for pre-sodium treatment for efficiently constructing a sodium ion capacitor as claimed in any one of claims 1 to 3, wherein:
the negative electrode comprises the following active materials in percentage by mass: 65-75% of active substance, 15-25% of conductive agent and 5-15% of binder;
the composite positive electrode comprises the following active substances, a binder and a conductive agent in percentage by mass: 70-90% of active substance, 5-15% of conductive agent and 5-15% of binder.
5. The method of claim 4, wherein the pre-sodium treatment is carried out by:
the conductive agent in the composite positive electrode and the composite negative electrode is conductive carbon black;
the binder in the negative electrode is CMCC;
and the binder in the composite positive electrode is PVDF.
6. The method of claim 1, wherein the pre-sodium treatment is carried out by: the porous carbon material is prepared by the following method: passing ethylenediaminetetraacetic acid tetrasodium salt through a reactor under a protective atmosphere of 700-900 DEG CoAnd C, calcining and pickling to obtain the catalyst.
7. The method of claim 1, wherein the pre-sodium treatment is carried out by:
the charge-discharge cycle is carried out by cyclic voltammetry, and the conditions for realizing the pre-sodium treatment of the cathode are as follows: adopting cyclic voltammetry with a scanning speed of 5mV s-1Scanning for 5 circles in a voltage interval, and after scanningStanding for 10-15 hours; wherein, when the negative active material is anatase TiO2When the negative active material is a porous carbon material, the voltage range is 2-4.5V, and when the negative active material is a porous carbon material, the voltage range is 0-4V.
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