CN112909230A - Electrode for absorbing composite tin elementary substance by using dunaliella salina and preparation method thereof - Google Patents
Electrode for absorbing composite tin elementary substance by using dunaliella salina and preparation method thereof Download PDFInfo
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- CN112909230A CN112909230A CN202110066775.9A CN202110066775A CN112909230A CN 112909230 A CN112909230 A CN 112909230A CN 202110066775 A CN202110066775 A CN 202110066775A CN 112909230 A CN112909230 A CN 112909230A
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/387—Tin or alloys based on tin
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses an electrode for absorbing a composite tin simple substance by dunaliella and a preparation method thereof, wherein the electrode for absorbing the composite tin simple substance by the dunaliella comprises an active material, ketjen black and polyvinylidene fluoride; the electrode is of a core-shell structure, the active material comprises dunaliella salina and a tin simple substance, the basic carbon of the dunaliella salina is a core, and the tin simple substance on the outer layer is of a shell structure; in the electrode, the weight percentage of the active material is 65-75%, the weight percentage of the Ketjen black is 10-20%, the weight percentage of the polyvinylidene fluoride is 10-20%, the weight content of the organic carbon in the active material is 10-20%, and the weight content of the tin simple substance is 80-90%. The electrode for absorbing the composite tin simple substance by the dunaliella salina disclosed by the invention takes the dunaliella salina as a template, a large amount of tin simple substances can be compounded inside and outside the electrode, and the natural structure of the electrode ensures that the structure of the electrode is not easily damaged during charging and discharging.
Description
Technical Field
The invention relates to the technical field of lithium battery cathode materials, in particular to an electrode for absorbing a composite tin simple substance by dunaliella and a preparation method thereof.
Background
Energy sources such as coal and petroleum, which are consumed in a limited and rapid manner, cannot be continuously utilized, and development and utilization of such energy sources are accompanied by a series of problems such as a large amount of industrial pollution. New energy sources and energy storage devices need to be researched. In the energy storage materials, the most studied and applied at present are lithium ion batteries, and the successful research and development of positive and negative electrode battery materials are key elements for the successful research of the lithium ion batteries. Although the energy density of the lithium ion battery has been doubled compared to the commercial battery marketed by sony corporation in 1991, the lithium ion battery also faces a new problem in many details with the continuous expansion of the application field of the lithium ion battery, and research and solution are urgently needed. For example, the frequency and time of using electronic devices are getting higher and longer, the functions of the electronic devices are also getting more and more, the display size of the screen is also getting larger and the application field is more and more extensive, and the performance of the corresponding lithium ion battery needs to be correspondingly improved in all aspects. Therefore, the lithium ion battery has the advantages of high capacity, long service life, high stability, high rate performance, environmental friendliness and low cost, and is the trend of future lithium ion battery research. How to solve the problems is that researchers find lithium ion battery materials with better structures and more diversified forms to create better technologies, materials and solutions to solve the problems faced by the development of lithium ion batteries.
Disclosure of Invention
The invention aims to: the electrode and the preparation method thereof solve the problems in the prior art, and the electrode energy storage element is prepared from low-cost materials and a simple method, so that the cost is saved, and the structure is not easily damaged during charging and discharging.
The technical scheme of the invention is as follows:
an electrode for absorbing composite tin elementary substance by dunaliella salina is characterized in that: it comprises active material, Ketjen black, polyvinylidene fluoride;
the electrode is of a core-shell structure, the active material comprises dunaliella salina and a tin simple substance, the basic carbon of the dunaliella salina is a core, and the tin simple substance on the outer layer is of a shell structure; in the electrode, the weight percentage of the active material is 65-75%, the weight percentage of the Ketjen black is 10-20%, the weight percentage of the polyvinylidene fluoride is 10-20%,
the weight content of organic carbon in the active material is 10-20%, and the weight content of the simple substance tin is 80-90%.
As a further improvement of the scheme, the Ketjen black and the polyvinylidene fluoride are analytically pure, the tin simple substance particles are 5 nanometers to 1.5 micrometers, and the dunaliella salina has a basal carbon length of 3 to 40 micrometers and a width of 1 to 3 micrometers.
As a further improvement of the scheme, the dunaliella salina is hollow dunaliella salina, and the basal carbon of the hollow dunaliella salina is wrapped by multiple layers of tin simple substances.
A preparation method of an electrode for absorbing a composite tin simple substance by dunaliella is characterized by comprising the following steps: which comprises the following steps:
(1) culturing dunaliella salina;
(2) adding tin salt into Dunaliella salina;
(3) removing impurities in the culture solution of the dunaliella salina, and then carrying out suction filtration;
(4) performing ultrasonic treatment to obtain a concentrated solution, performing centrifugal treatment on the concentrated solution to obtain a precipitate, and freeze-drying the precipitate;
(5) annealing;
(6) and coating to form the electrode.
As a further improvement of the scheme, in the first step, the dunaliella salina is cultured in artificial seawater, the dunaliella salina is cultured in the artificial seawater for one week, the concentration of sodium salt is gradually increased to 200 g/L, and then the dunaliella salina is cultured in a light and dark field for 13 to 28 days alternately.
As a further improvement of the scheme, the salt algae culture solution is added with tin salt according to the proportion that 1 liter of culture solution is added with 1-10 grams of tin salt; adding tin salt into 3L of Dunaliella salina culture solution in batches to increase the concentration of the tin salt in the Dunaliella salina culture solution, slightly stirring during the addition of the tin salt until the tin salt is not dissolved, standing for 24-48 hr, and recording the amount of the added tin salt (6-24 g).
As a further improvement of this embodiment, the tin salt is tin tetrachloride or tin dichloride.
As a further improvement of the scheme, in the third step, concentrated hydrochloric acid is added into 3 liters of the dunaliella salina culture solution before suction filtration in a proportion of 10 drops of concentrated hydrochloric acid to remove impurities, then the dunaliella salina culture solution added with tin salt is subjected to vacuum suction filtration, then the suction filtration is subjected to ultrasonic treatment in 60-100 ml of deionized water for 3-15 minutes to obtain an impurity-free concentrated solution after absorbing the compound tin salt, a precipitate is obtained through centrifugal treatment, and the precipitate is freeze-dried for 10-24 hours.
As a further improvement of the scheme, in the fourth step, powder is obtained after freeze drying, the powder is annealed by argon protective gas, the heating rate is 3-8 ℃ per minute in the annealing process, the heat preservation time is 1-15 minutes after 800 ℃, and the annealed sample is naturally cooled after annealing to be used.
And as a further improvement of the scheme, coating the sample obtained in the fifth step into an electrode, drying and tabletting to prepare the half cell.
The invention has the advantages that:
1. the invention discloses an electrode for absorbing composite tin elementary substance by dunaliella and a preparation method thereof, wherein dunaliella is used as a template, a large amount of tin elementary substance can be compounded inside and outside, and the natural structure of the electrode ensures that the structure of the electrode is not easy to damage during charging and discharging.
2. The electrode for absorbing the composite tin simple substance by the brine alga and the preparation method thereof disclosed by the invention are used for preparing the electrode energy storage element by using low-cost materials and a simple method, so that the cost is saved, the environmental pollution is reduced, and the electrode is beneficial to environmental protection.
Drawings
The invention is further described with reference to the following figures and examples:
fig. 1 is a schematic TEM microstructure of the active material of the electrode of the invention, wherein dunaliella salina absorbs composite tin simple substance.
Fig. 2 is a schematic diagram of a TEM magnified microstructure of an active material of an electrode of the invention, wherein dunaliella salina absorbs composite tin simple substance.
Fig. 3 is a schematic diagram of a TEM high-resolution structural diagram of an active material of the electrode for absorbing the composite tin elementary substance by dunaliella salina.
FIG. 4 is a schematic TEM morphology of the active material of the electrode for absorbing composite tin elementary substance by dunaliella salina.
FIG. 5 is a schematic SEM image of the active material of the electrode of the invention with dunaliella salina absorbing composite tin simple substance.
FIG. 6 is a schematic SEM enlarged morphology of an active material of the electrode for absorbing the composite tin simple substance by the dunaliella salina.
FIG. 7 is a schematic diagram of the selected area of the SEM elemental spectrum of the active material of the electrode for absorbing the composite tin elementary substance by dunaliella salina.
Fig. 8 is a schematic diagram of an SEM tin element spectrum of an active material of the electrode for absorbing the composite tin simple substance by dunaliella salina.
Fig. 9 is a schematic diagram of an SEM carbon element spectrum of an active material of an electrode for absorbing a composite tin simple substance by dunaliella salina.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to the accompanying drawings and preferred embodiments.
The invention discloses an electrode for absorbing a composite tin simple substance by dunaliella salina, which comprises an active material, Keqin black and polyvinylidene fluoride; the electrode is of a core-shell structure, the active material comprises dunaliella salina and a tin simple substance, the tin simple substance is tin tetrachloride in the embodiment, the basic carbon of the dunaliella salina is a core, and the tin simple substance on the outer layer is of a shell structure; in the electrode, the weight percentage of the active material is 65-75%, the weight percentage of the Ketjen black is 10-20%, the weight percentage of the polyvinylidene fluoride is 10-20%, the weight content of the organic carbon in the active material is 10-20%, and the weight content of the tin simple substance is 80-90%. The electrode for absorbing the composite tin simple substance by the dunaliella salina disclosed by the invention takes the dunaliella salina as a template, a large amount of tin simple substances can be compounded inside and outside the electrode, and the natural structure of the electrode ensures that the structure of the electrode is not easily damaged during charging and discharging.
As a further improvement of the scheme, the Ketjen black and the polyvinylidene fluoride are analytically pure, the tin simple substance particles are about 5 nanometers to 1.5 micrometers, and the dunaliella salina has a basal carbon length of 3 to 40 micrometers and a width of 1 to 3 micrometers. The structure further ensures the charge and discharge functions and the service life of the electrode.
As a further improvement of the scheme, the dunaliella salina is hollow dunaliella salina, and the basal carbon of the hollow dunaliella salina is wrapped by multiple layers of tin simple substances. The material composition can ensure the cycle stability, the cycle life and the energy density of the lithium ion battery.
A preparation method of an electrode for absorbing a composite tin simple substance by dunaliella salina comprises the following steps:
(1) culturing dunaliella salina;
(2) adding tin salt into Dunaliella salina;
(3) removing impurities in the culture solution of the dunaliella salina, and then carrying out suction filtration;
(4) performing ultrasonic treatment to obtain a concentrated solution, performing centrifugal treatment on the concentrated solution to obtain a precipitate, and freeze-drying the precipitate;
(5) annealing;
(6) and coating to form the electrode.
The preparation method of the electrode for absorbing the composite tin simple substance by the brine alga disclosed by the invention prepares the electrode energy storage element by using low-cost materials and a simple method, saves the cost, reduces the environmental pollution and is beneficial to environmental protection. Dunaliella salina has a complete carbon structure and is suitable for being selected as a carrier for absorbing tin salt. In our living environment, the halophyte has very strong ability of adapting to the environment in a long evolution process and very strong reproductive capacity, so the cost is very low, and the method is suitable for mass production. The dunaliella salina can selectively or passively absorb and compound corresponding inorganic salt, so that a large amount of metal cations exist in and out of the dunaliella salina body. And due to the natural biological structure of the dunaliella salina, the dunaliella salina can absorb the composite tin simple substance to be used as an electrode material with good performance. Because the individual of the dunaliella salina is very small, and because of the natural biological structure of the dunaliella salina and the specific capacity of the lithium ion battery of the tin simple substance is high, the electrode material of the dunaliella salina absorbing the composite tin simple substance has good performance, so the electrode material is a good material for preparing the energy storage element in the invention.
As a further improvement of the scheme, in the first step, the dunaliella salina is cultured in artificial seawater, the dunaliella salina is cultured in the artificial seawater for one week, the concentration of sodium salt is gradually increased to 200 g/L, and then the dunaliella salina is cultured in a light and dark field for 13 to 28 days alternately. The dunaliella salina cultured in this way meets the requirements and can improve the performance of the lithium battery.
As a further improvement of this embodiment, the tin salt is tin tetrachloride or tin dichloride.
As a further improvement of the scheme, 1-10 g of stannic chloride is added into 1L of the culture solution of the dunaliella salina; taking 3 liters of the dunaliella salina culture solution, adding tin tetrachloride in batches to improve the concentration of the tin tetrachloride in the dunaliella salina culture solution, slightly stirring in the process of adding the tin tetrachloride until the tin tetrachloride is not dissolved any more, standing for 24-48 hours, and recording the amount of the added tin tetrachloride (6-24 grams). This allows the concentration of tin tetrachloride to be increased without wasting tin tetrachloride, and achieving maximum results at the lowest cost.
As a further improvement of the scheme, in the third step, concentrated hydrochloric acid is added into 3 liters of the dunaliella salina culture solution before suction filtration in a proportion of 10 drops of concentrated hydrochloric acid to remove impurities, then the dunaliella salina culture solution added with tin salt is subjected to vacuum suction filtration, then the suction filtration is subjected to ultrasonic treatment in 60-100 ml of deionized water for 3-15 minutes to obtain an impurity-free concentrated solution after absorbing the compound tin salt, a precipitate is obtained through centrifugal treatment, and the precipitate is freeze-dried for 10-24 hours. Therefore, the stability of the lithium ion battery can be ensured, and the service life of the lithium ion battery is prolonged.
As a further improvement of the scheme, in the fourth step, powder is obtained after freeze drying, the powder is annealed by argon protective gas, the heating rate is 3-8 ℃ per minute in the annealing process, the heat preservation time is 1-15 minutes after 800 ℃, and the annealed sample is naturally cooled after annealing to be used. The sample prepared in the way can further ensure the performance of the electrode and ensure the safe, stable and efficient use of the lithium battery.
And as a further improvement of the scheme, coating the sample obtained in the fifth step into an electrode, drying and tabletting to prepare the half cell. Simple operation, low cost and energy conservation.
N-methyl pyrrolidone can also be added as a solvent in the process of processing the electrode, and the N-methyl pyrrolidone is removed before the electrode is manufactured.
The existing carbon template is artificial carbon, and is easy to collapse after repeated charge and discharge, and finally, the battery is easy to collapse. In the embodiment of the invention, the basal carbon of the dunaliella salina is wrapped by multiple layers of tin simple substances. FIG. 1 is a schematic diagram of TEM microstructure of active material of an electrode for absorbing composite tin simple substance by dunaliella salina, wherein the surface of a Sn-carbon sample is provided with a large number of granular black spots, and the sizes of the granular black spots are different and most of the granular black spots are not more than 10 nanometers. Fig. 2 is a schematic view of the TEM magnified microstructure of the active material of the electrode for absorbing the composite tin simple substance by dunaliella salina, and a magnified TEM image of a side view of the surface of the Sn-carbon sample further shows the size of the particles, most of which are concentrated at about 5 nm, and at the same time, a large amount of spherical Sn particles in the sample can be seen. Fig. 3 is a schematic diagram of a TEM high-resolution structural diagram of an active material of the electrode for absorbing the composite tin simple substance by dunaliella salina, which shows that the Sn simple substance particles have good crystallinity and also shows that the basic carbon of the dunaliella salina is non-graphitized carbon. Fig. 4 is a schematic TEM image of the active material of the electrode for absorbing the composite tin simple substance by using dunaliella salina, and fig. 4 shows two shapes of dunaliella salina, one is a strip dunaliella salina with two ends being the same, the width is about 1.5 microns, the length is 4 microns, and the other shape is pear-shaped dunaliella salina, the width is about 1 micron, and the length is 2.5 microns. FIG. 5 is a schematic SEM image of the active material of the electrode of the invention with dunaliella salina absorbing composite tin simple substance. Fig. 5 shows that the Sn-carbon sample consists of many oval substances and a large number of small particles, which is a result of a large number of metallic Sn particles attached to the surface of dunaliella salina, and at the same time, shows that metallic Sn particles are present widely and uniformly distributed. Fig. 6 is a schematic diagram of an SEM magnified morphology of the active material of the electrode for absorbing composite tin element by dunaliella salina according to the present invention, wherein the metal Sn particles are spherical about 2.2 microns and have surface defects, and the diagram shows another shape of dunaliella salina, which is similar to pear-shaped, and has a length of about 2.3 microns and a width of about 1.3 microns. FIG. 7 is a schematic diagram of the selected area of the SEM elemental spectrum of the active material of the electrode for absorbing the composite tin elementary substance by dunaliella salina. Fig. 8 is a schematic diagram of an SEM tin element spectrum of an active material of the electrode for absorbing the composite tin simple substance by dunaliella salina, and it can be seen that Sn particles are mainly of a spherical structure. Fig. 9 is a schematic diagram of an SEM carbon element spectrum of an active material of an electrode for absorbing a composite tin simple substance by dunaliella salina. It can be seen that the dunaliella salina exhibits a pear-shaped structure. The dunaliella salina and the tin simple substance are not overlapped, and the existence of pear-shaped dunaliella salina in the material is proved. Such a structure can ensure the stability and life of the battery.
In a preferred embodiment, the dunaliella salina is cultured in artificial seawater for one week, then the salt concentration is increased until the concentration reaches two hundred thousand, then the dunaliella salina is cultured alternately in a bright and dark field for about half a month, after the dunaliella salina is cultured to a sufficient concentration, stannic chloride is added, 1-10 g of stannic chloride is added in each liter of solution, after 24-48 hours, hydrochloric acid is added, and the dunaliella salina is centrifuged in an acid environment (pH value is 2-6) to obtain a precipitate. The precipitate is then annealed under a protective gas and coated into an electrode. The method has the advantages that the electrode is obtained by a simple method with low cost, the lithium ion battery cathode is taken as a starting point, the cheap material selection and the environmental friendliness are taken as starting points, the dunaliella salina is selected and utilized as a carrier, and the composite tin simple substance is absorbed to prepare the high-performance cathode material with long range, high stability, good multiplying power, high energy density and high power density. After the dunaliella salina absorbs the composite tin simple substance, the dunaliella salina can effectively reduce the expansion and pulverization of tin ions in the process of charge-discharge cycle, so that the electrode material has good performance. In addition, the tin element is widely distributed on the earth and has good energy storage property.
The performance of the cathode material of the electrode prepared by the embodiment is stable, the electrode reaches 2000 cycles without attenuation basically, and the capacity of the cathode material is higher than that of the conventional cathode graphite or graphene by twice. The service life of the lithium ion battery power supply can be greatly prolonged. The cathode material can bear large-current charge and discharge and has good rate performance. Low cost and easy obtaining.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. The present invention is not to be limited by the specific embodiments disclosed herein, and other embodiments that fall within the scope of the claims of the present application are intended to be within the scope of the present invention. The invention has various embodiments, and all technical solutions formed by adopting equivalent transformation or equivalent transformation are within the protection scope of the invention.
Claims (10)
1. An electrode for absorbing composite tin elementary substance by dunaliella salina is characterized in that: it comprises active material, Ketjen black, polyvinylidene fluoride;
the electrode is of a core-shell structure, the active material comprises dunaliella salina and a tin simple substance, the basic carbon of the dunaliella salina is a core, and the tin simple substance on the outer layer is of a shell structure; in the electrode, the weight percentage of the active material is 65-75%, the weight percentage of the Ketjen black is 10-20%, the weight percentage of the polyvinylidene fluoride is 10-20%,
the weight content of organic carbon in the active material is 10-20%, and the weight content of the simple substance tin is 80-90%.
2. The electrode for absorbing composite tin elementary substance by dunaliella salina according to claim 1, wherein: the Ketjen black and the polyvinylidene fluoride are analytically pure, the tin simple substance particles are 5 nanometers to 1.5 micrometers, the length of the basic carbon of the dunaliella salina is 3 to 40 micrometers, and the width of the basic carbon is 1 to 3 micrometers.
3. The electrode for absorbing composite tin elementary substance by dunaliella salina according to claim 1, wherein: the dunaliella salina is hollow dunaliella salina, and the basal carbon of the hollow dunaliella salina is wrapped by multiple layers of tin simple substances.
4. A preparation method of an electrode for absorbing a composite tin simple substance by dunaliella is characterized by comprising the following steps: which comprises the following steps:
(1) culturing dunaliella salina;
(2) adding tin salt into Dunaliella salina;
(3) removing impurities in the culture solution of the dunaliella salina, and then carrying out suction filtration;
(4) performing ultrasonic treatment to obtain a concentrated solution, performing centrifugal treatment on the concentrated solution to obtain a precipitate, and freeze-drying the precipitate;
(5) annealing;
(6) and coating to form the electrode.
5. The method for preparing the electrode for absorbing the composite tin elementary substance by the dunaliella salina as claimed in claim 4, wherein: in the first step, the dunaliella salina is cultured in artificial seawater for one week, the concentration of sodium salt is gradually increased to 200 g/L, and then the dunaliella salina is cultured in a light and dark field for 13-28 days alternately.
6. The method for preparing the electrode for absorbing the composite tin elementary substance by the dunaliella salina as claimed in claim 4, wherein: adding 1-10 g of tin salt into 1L of the culture solution of the dunaliella salina; adding tin salt into 3L of Dunaliella salina culture solution in batches to increase the concentration of tin salt in the Dunaliella salina culture solution, slightly stirring during the process of adding tin salt until tin salt is no longer dissolved, and standing for 24-48 hr.
7. The method for preparing the electrode for absorbing the composite tin elementary substance by the dunaliella salina as claimed in claim 6, wherein: the tin salt is tin tetrachloride or tin dichloride.
8. The method for preparing the electrode for absorbing the composite tin elementary substance by the dunaliella salina as claimed in claim 4, wherein: in the third step, before pumping filtration, adding concentrated hydrochloric acid into 3 liters of dunaliella salina culture solution according to the proportion of adding 10 drops of concentrated hydrochloric acid, removing impurities, then carrying out vacuum filtration on the dunaliella salina culture solution added with tin salt, then carrying out ultrasonic treatment on the filtrate in 60-100 ml of deionized water for 3-15 minutes to obtain an impurity-free concentrated solution after absorbing the composite tin salt, carrying out centrifugal treatment to obtain a precipitate, and freeze-drying the precipitate for 10-24 hours.
9. The method for preparing the electrode for absorbing the composite tin elementary substance by the dunaliella salina as claimed in claim 4, wherein: and step four, obtaining powder after freeze drying, annealing the powder by using argon protective gas, wherein the heating rate is 3-8 ℃ per minute in the annealing process, the heat preservation time is 1-15 minutes after 800 ℃, and naturally cooling after annealing to obtain an annealed sample for later use.
10. The method for preparing the electrode for absorbing the composite tin elementary substance by the dunaliella salina as claimed in claim 4, wherein: and (4) coating the sample obtained in the fifth step into an electrode, drying and tabletting to prepare the half cell.
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