CN109920657B - Novel lithium ion electrode material of super capacitor - Google Patents
Novel lithium ion electrode material of super capacitor Download PDFInfo
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- CN109920657B CN109920657B CN201910201128.7A CN201910201128A CN109920657B CN 109920657 B CN109920657 B CN 109920657B CN 201910201128 A CN201910201128 A CN 201910201128A CN 109920657 B CN109920657 B CN 109920657B
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 53
- 239000007772 electrode material Substances 0.000 title claims abstract description 46
- 239000003990 capacitor Substances 0.000 title claims abstract description 33
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 20
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 11
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 11
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 230000014759 maintenance of location Effects 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 abstract description 2
- 229910052719 titanium Inorganic materials 0.000 abstract description 2
- -1 titanium ions Chemical class 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 238000011161 development Methods 0.000 description 5
- 230000010287 polarization Effects 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 235000011837 pasties Nutrition 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to the technical field of novel functional materials, and discloses a novel lithium ion electrode material of a super capacitor, which is prepared by introducing titanium ions and silicon-oxygen bonds into lithium carbonate and utilizing the structure and the morphology of a nano material, so that the electronic conductivity of the lithium ion electrode material is improved, the novel lithium ion electrode material with a stable structure is prepared, the reaction activity is strong, the charge conduction and the material transportation of a lithium ion electrode are improved, the polarizability is reduced, the charge and discharge speed is high, more energy can be stored, the self-discharge can be prevented, the novel lithium ion electrode material is further applied to the super capacitor, and the novel lithium ion electrode material has the advantages of high specific capacitance, good conductivity, low cost, wide application range, long cycle service life and the like, and has the performances of quick charge and discharge, high capacitance retention rate and the like.
Description
Technical Field
The invention belongs to the technical field of novel functional materials, and particularly relates to a novel lithium ion electrode material of a super capacitor.
Background
A supercapacitor is a new type of energy storage device between a conventional capacitor and a rechargeable battery, and its capacity can reach several hundreds to thousands of methods. Compared with the traditional capacitor, the capacitor has larger capacity, specific energy or capacity density, wider working temperature range and extremely long service life; compared with accumulator, it has higher specific power and no environmental pollution. A supercapacitor is a novel component that stores energy through an interfacial double layer formed between electrodes and an electrolyte. When the electrode contacts with the electrolyte, the solid-liquid interface generates stable double-layer charges with opposite signs under the action of coulomb force, intermolecular force and interatomic force, and the double-layer charges are called as interface double layers. The electric double layer supercapacitor is considered to be 2 inactive porous plates suspended in an electrolyte, and a voltage is applied to the 2 plates. The potential applied to the positive plate attracts negative ions in the electrolyte and the negative plate attracts positive ions, thereby forming an electric double layer capacitor on the surfaces of the two electrodes. The electric double layer capacitor may be classified into a carbon electrode double layer supercapacitor, a metal oxide electrode supercapacitor, and an organic polymer electrode supercapacitor according to the difference in electrode materials.
With the change of electronic information technology, the update and update speed of digital electronic products is faster and faster, the production and sales volume of consumer electronic products mainly including flat panel televisions (LCDs and PDPs), notebook computers, digital cameras and other products is continuously increased, the capacitor industry is driven to increase, and more scale applications are developed to the fields of green energy, national defense, medical treatment, traffic equipment, wireless communication and the like to serve the society. The electrode performance of the capacitor is directly related to the capacitance of the capacitor and the service life. The lithium ion battery has the advantages of high energy density, long cycle service life and the like, but in the lithium ion super capacitor, the problems of low utilization rate, low diffusion speed, easy polarization and the like exist, and the development of the lithium ion super capacitor is restricted.
Disclosure of Invention
The invention aims to solve the existing problems, provides a novel lithium ion electrode material of a super capacitor, improves the charge conduction and the material transportation of a lithium ion electrode, reduces the polarizability, has high charge and discharge rate, can store more energy and can prevent self-discharge.
The invention is realized by the following technical scheme:
a novel lithium ion electrode material of a super capacitor is prepared from the following components in parts by weight: 9.5-9.8 parts of lithium carbonate, 5.1-5.4 parts of butyl titanate, 3.6-3.8 parts of ethyl orthosilicate, 0.25-0.30 part of aminopropyltriethoxysilane, 25-30 parts of dilute hydrochloric acid, 18-20 parts of absolute ethyl alcohol and 35-40 parts of ammonia water solution; the preparation method comprises the following steps:
(1) adding lithium carbonate and dilute hydrochloric acid into a four-neck flask, heating to 65-70 ℃ under stirring, slowly adding butyl titanate into absolute ethyl alcohol under stirring at 25-28 ℃ to prepare a solution A, dropwise adding the solution A into the four-neck flask, introducing nitrogen, continuously heating to 85-88 ℃, closing the nitrogen, carrying out heat preservation reflux reaction for 2.0-3.0 hours, cooling to 45-55 ℃ after the reaction is finished, adding a sodium carbonate solution to adjust the pH value to be within the range of 5.8-6.0, naturally cooling to room temperature under stirring, pouring out a supernatant liquid, carrying out centrifugal separation washing on the obtained precipitate, carrying out centrifugal washing for 3-5 times by using deionized water, and drying in an oven at 90-100 ℃ for 2-3 hours;
(2) and (2) placing the dried solid obtained in the step (1) in a crucible for grinding for 50-60 minutes, then placing the crucible in an ammonia water solution for soaking for 3-4 hours, adding tetraethoxysilane and aminopropyltriethoxysilane while stirring, heating to 30-34 ℃, keeping the temperature and continuously stirring for 2-3 hours, then carrying out ultrasonic treatment for 10-15 minutes to form a uniform state, transferring the uniform state to a muffle furnace for heating reaction, heating to 430-440 ℃ in the first stage, carrying out heat preservation and calcination for 1.5-2.0 hours, heating to 700-720 ℃ in the second stage, carrying out heat preservation and calcination for 70-80 minutes, and naturally cooling to room temperature along with the furnace to obtain the lithium ion electrode material.
As a further description of the scheme, the mass concentration of the sodium carbonate solution in the step (1) is 35-38%.
As a further description of the above scheme, the particle size of the lithium ion electrode material is between 70 and 80 nanometers.
As a further description of the above scheme, the mass concentration of the ammonia water solution is 60-65%.
As a further description of the above scheme, the dilute hydrochloric acid has a pH of between 3.0 and 3.3.
As a further description of the above scheme, the temperature rise rate in the muffle furnace in the step (2) is 1.6-1.8 ℃/min.
Compared with the prior art, the invention has the following advantages: in order to solve the problems of low utilization rate, low diffusion speed, easy polarization and the like in the existing lithium ion super capacitor, the invention provides a novel lithium ion electrode material of the super capacitor, the electronic conductivity of the lithium ion electrode material is improved by introducing titanium ions and silicon-oxygen bonds into lithium carbonate and utilizing the structure and the appearance of a nano material, so that the novel lithium ion electrode material with stable structure is prepared, the reaction activity is strong, the charge conduction and the material transportation of the lithium ion electrode are improved, the polarization rate is reduced, the charge and discharge speed is high, more energy can be stored, the self-discharge can be prevented, the novel lithium ion electrode material is further applied to the super capacitor, and the novel lithium ion electrode material has the advantages of high specific capacitance, good conductivity, low cost, wide application range, long cycle service life and the like, and has the performances of high charge and discharge speed, high retention rate and the like, the method has the advantages of greatly improving the performance of the lithium ion super capacitor, having strong adaptability to temperature, improving economic benefit, reducing cost, improving development and utilization of electrode materials of the super capacitor, realizing the practical significance of promoting the development of capacitor industry and improving application value in the fields of electronics, biology, medicine and the like, along with low utilization rate, low diffusion speed, easy polarization and the like, safety and no toxicity.
Detailed Description
In order to make the objects, technical solutions and effects of the present invention clearer and clearer, the present invention is further described with reference to specific embodiments, and it should be understood that the specific embodiments described herein are only used for explaining the present invention and are not used for limiting the technical solutions provided by the present invention.
Example 1
A novel lithium ion electrode material of a super capacitor is prepared from the following components in parts by weight: 9.5 parts of lithium carbonate, 5.1 parts of butyl titanate, 3.6 parts of ethyl orthosilicate, 0.25 part of aminopropyltriethoxysilane, 25 parts of dilute hydrochloric acid, 18 parts of absolute ethyl alcohol and 35 parts of ammonia water solution; the preparation method comprises the following steps:
(1) adding lithium carbonate and dilute hydrochloric acid into a four-neck flask, heating to 65 ℃ under stirring, slowly adding butyl titanate into absolute ethyl alcohol under stirring at 25 ℃ to prepare a solution A, dropwise adding the solution A into the four-neck flask, introducing nitrogen, continuously heating to 85 ℃, closing the nitrogen, carrying out heat preservation reflux reaction for 2.0 hours, cooling to 45 ℃ after the reaction is finished, adding a sodium carbonate solution to adjust the pH value to be within the range of 5.8-6.0, naturally cooling to room temperature under stirring, pouring out a clear liquid, carrying out centrifugal separation washing on the obtained precipitate, carrying out centrifugal washing for 3 times by using deionized water, and drying in an oven at 90 ℃ for 2 hours;
(2) and (2) placing the dried solid obtained in the step (1) in a crucible to grind for 50 minutes, then placing the crucible in an ammonia water solution to soak for 3 hours, adding tetraethoxysilane and aminopropyltriethoxysilane while stirring, heating to 30 ℃, keeping the temperature and continuously stirring for 2 hours, then carrying out ultrasonic treatment for 10 minutes to form a uniform state, transferring the uniform state to a muffle furnace to carry out heating reaction, heating to 430 ℃ in the first stage, keeping the temperature and calcining for 1.5 hours, heating to 700 ℃ in the second stage, keeping the temperature and calcining for 70 minutes, and naturally cooling to room temperature along with the furnace to obtain the lithium ion electrode material.
As a further description of the above scheme, the mass concentration of the sodium carbonate solution in the step (1) is 35%.
As a further description of the above scheme, the particle size of the lithium ion electrode material is between 70 and 80 nanometers.
As a further description of the above scheme, the mass concentration of the aqueous ammonia solution is 60%.
As a further description of the above scheme, the dilute hydrochloric acid has a pH of between 3.0 and 3.3.
As a further description of the above protocol, the muffle furnace temperature rise rate in step (2) was 1.6 deg.C/min.
Example 2
A novel lithium ion electrode material of a super capacitor is prepared from the following components in parts by weight: 9.6 parts of lithium carbonate, 5.2 parts of butyl titanate, 3.7 parts of ethyl orthosilicate, 0.28 part of aminopropyltriethoxysilane, 28 parts of dilute hydrochloric acid, 19 parts of absolute ethyl alcohol and 38 parts of ammonia water solution; the preparation method comprises the following steps:
(1) adding lithium carbonate and dilute hydrochloric acid into a four-neck flask, heating to 68 ℃ under stirring, slowly adding butyl titanate into absolute ethyl alcohol under stirring at 26 ℃ to prepare a solution A, dropwise adding the solution A into the four-neck flask, introducing nitrogen, continuously heating to 86 ℃, closing the nitrogen, carrying out heat preservation reflux reaction for 2.5 hours, cooling to 50 ℃ after the reaction is finished, adding a sodium carbonate solution to adjust the pH value to be within the range of 5.8-6.0, naturally cooling to room temperature under stirring, pouring out a clear liquid, carrying out centrifugal separation washing on the obtained precipitate, carrying out centrifugal washing for 4 times by using deionized water, and drying in an oven at 95 ℃ for 2.5 hours;
(2) and (2) placing the dried solid obtained in the step (1) in a crucible to grind for 55 minutes, then placing the crucible in an ammonia water solution to soak for 3.5 hours, adding tetraethoxysilane and aminopropyltriethoxysilane while stirring, heating to 32 ℃, keeping the temperature and continuously stirring for 2.5 hours, then carrying out ultrasonic treatment for 12 minutes to form a uniform state, transferring the uniform state to a muffle furnace to carry out heating reaction, heating to 435 ℃ in the first stage, keeping the temperature and calcining for 1.8 hours, heating to 710 ℃ in the second stage, keeping the temperature and calcining for 75 minutes, and naturally cooling to room temperature along with the furnace to obtain the lithium ion electrode material.
As a further description of the above scheme, the mass concentration of the sodium carbonate solution in the step (1) is 36%.
As a further description of the above scheme, the particle size of the lithium ion electrode material is between 70 and 80 nanometers.
As a further description of the above scheme, the mass concentration of the aqueous ammonia solution is 62%.
As a further description of the above scheme, the dilute hydrochloric acid has a pH of between 3.0 and 3.3.
As a further description of the above protocol, the muffle furnace temperature rise rate in step (2) was 1.7 ℃/min.
Example 3
A novel lithium ion electrode material of a super capacitor is prepared from the following components in parts by weight: 9.8 parts of lithium carbonate, 5.4 parts of butyl titanate, 3.8 parts of ethyl orthosilicate, 0.30 part of aminopropyltriethoxysilane, 30 parts of dilute hydrochloric acid, 20 parts of absolute ethyl alcohol and 40 parts of ammonia water solution; the preparation method comprises the following steps:
(1) adding lithium carbonate and dilute hydrochloric acid into a four-neck flask, heating to 70 ℃ under stirring, slowly adding butyl titanate into absolute ethyl alcohol under stirring at 28 ℃ to prepare a solution A, dropwise adding the solution A into the four-neck flask, introducing nitrogen, continuously heating to 88 ℃, closing the nitrogen, carrying out heat preservation reflux reaction for 3.0 hours, cooling to 55 ℃ after the reaction is finished, adding a sodium carbonate solution to adjust the pH value to be within the range of 5.8-6.0, naturally cooling to room temperature under stirring, pouring out a clear liquid, carrying out centrifugal separation washing on the obtained precipitate, carrying out centrifugal washing 5 times by using deionized water, and drying in an oven at 100 ℃ for 3 hours;
(2) and (2) placing the dried solid obtained in the step (1) in a crucible to grind for 60 minutes, then placing the crucible in an ammonia water solution to soak for 4 hours, adding tetraethoxysilane and aminopropyltriethoxysilane while stirring, heating to 34 ℃, keeping the temperature and continuously stirring for 3 hours, then carrying out ultrasonic treatment for 15 minutes to form a uniform state, transferring the uniform state to a muffle furnace to carry out heating reaction, heating to 440 ℃ in the first stage, keeping the temperature and calcining for 2.0 hours, heating to 720 ℃ in the second stage, keeping the temperature and calcining for 80 minutes, and naturally cooling to room temperature along with the furnace to obtain the lithium ion electrode material.
As a further description of the above scheme, the mass concentration of the sodium carbonate solution in the step (1) is 38%.
As a further description of the above scheme, the particle size of the lithium ion electrode material is between 70 and 80 nanometers.
As a further description of the above scheme, the ammonia solution has a mass concentration of 65%.
As a further description of the above scheme, the dilute hydrochloric acid has a pH of between 3.0 and 3.3.
As a further description of the above protocol, the muffle furnace temperature rise rate in step (2) was 1.8 ℃/min.
Comparative example 1
The only difference from example 1 is that in the preparation of the lithium ion electrode material, the addition of the butyl titanate is omitted, and the rest is kept the same.
Comparative example 2
The difference from example 2 is only that in the preparation of the lithium ion electrode material, the addition of the tetraethoxysilane is omitted, and the rest is kept consistent.
Comparative example 3
The difference from example 3 is only that in the preparation of the lithium ion electrode material, the heat-preservation reflux reaction time in step (1) was 1.5 hours, and the rest remained the same.
Comparative example 4
The difference from the example 3 is only that in the preparation of the lithium ion electrode material, the temperature rise reaction is carried out in the muffle furnace in the step (2), the temperature is raised to 400 ℃ in the first stage, the temperature is kept for 1.0 hour for calcination, and the rest is kept consistent.
Comparative example 5
The difference from the example 3 is only that in the preparation of the lithium ion electrode material, the temperature rise reaction is carried out in the muffle furnace in the step (2), the temperature rise is carried out to 780 ℃ in the second stage, the heat preservation and calcination are carried out for 100 minutes, and the rest is kept consistent.
Comparative experiment
Lithium ion electrode materials were prepared using the methods of examples 1 to 3 and comparative examples 1 to 5, taking a method of taking lithium titanate as a lithium ion electrode material as a control group, mixing the electrode materials of all groups with acetylene black and polyvinylidene fluoride according to the mass ratio of 7.8:1.0:1.0, grinding uniformly, then a small amount of absolute ethyl alcohol is dripped until the mixture is ground into pasty sticky substance, the pasty sticky substance is evenly coated on a flattened aluminum foil, drying at 95 deg.C for 10 hr, cutting to obtain electrode plate as working electrode and metal lithium plate as reference electrode, electrochemical performance tests are carried out on all groups of samples under the same test conditions, and when the data are stable, representative data are collected, the obtained experimental data are the average values of 5 groups of samples, the independent variables in the test are kept consistent, effective average values are counted, and the results are shown in the following table:
the novel lithium ion electrode material of the super capacitor solves the problems of low utilization rate, low diffusion speed, easy polarization and the like in the conventional lithium ion super capacitor, greatly improves the performance of the lithium ion super capacitor, has strong temperature adaptability, improves economic benefits, is safe and nontoxic, improves the functional effect and the service life of the electrode of the lithium ion super capacitor, reduces the cost, improves the development and utilization of the electrode material of the super capacitor, can realize the practical significance of promoting the development of the capacitor industry and improving the application value in the fields of electronics, biology, medicine and the like, and is a technical scheme which is extremely worthy of popularization and use.
Claims (6)
1. The novel lithium ion electrode material of the super capacitor is characterized by being prepared from the following components in parts by weight: 9.5-9.8 parts of lithium carbonate, 5.1-5.4 parts of butyl titanate, 3.6-3.8 parts of ethyl orthosilicate, 0.25-0.30 part of aminopropyltriethoxysilane, 25-30 parts of dilute hydrochloric acid, 18-20 parts of absolute ethyl alcohol and 35-40 parts of ammonia water solution; the preparation method comprises the following steps:
(1) adding lithium carbonate and dilute hydrochloric acid into a four-neck flask, heating to 65-70 ℃ under stirring, slowly adding butyl titanate into absolute ethyl alcohol under stirring at 25-28 ℃ to prepare a solution A, dropwise adding the solution A into the four-neck flask, introducing nitrogen, continuously heating to 85-88 ℃, closing the nitrogen, carrying out heat preservation reflux reaction for 2.0-3.0 hours, cooling to 45-55 ℃ after the reaction is finished, adding a sodium carbonate solution to adjust the pH value to be within the range of 5.8-6.0, naturally cooling to room temperature under stirring, pouring out a supernatant liquid, carrying out centrifugal separation washing on the obtained precipitate, carrying out centrifugal washing for 3-5 times by using deionized water, and drying in an oven at 90-100 ℃ for 2-3 hours;
(2) and (2) placing the dried solid obtained in the step (1) in a crucible for grinding for 50-60 minutes, then placing the crucible in an ammonia water solution for soaking for 3-4 hours, adding tetraethoxysilane and aminopropyltriethoxysilane while stirring, heating to 30-34 ℃, keeping the temperature and continuously stirring for 2-3 hours, then carrying out ultrasonic treatment for 10-15 minutes to form a uniform state, transferring the uniform state to a muffle furnace for heating reaction, heating to 430-440 ℃ in the first stage, carrying out heat preservation and calcination for 1.5-2.0 hours, heating to 700-720 ℃ in the second stage, carrying out heat preservation and calcination for 70-80 minutes, and naturally cooling to room temperature along with the furnace to obtain the lithium ion electrode material.
2. The novel lithium ion electrode material for the supercapacitor, according to claim 1, wherein the mass concentration of the sodium carbonate solution in the step (1) is 35-38%.
3. The novel lithium ion electrode material of the supercapacitor according to claim 1, wherein the particle size of the lithium ion electrode material is between 70 and 80 nanometers.
4. The novel lithium ion electrode material of the supercapacitor according to claim 1, wherein the mass concentration of the ammonia water solution is 60-65%.
5. The novel lithium ion electrode material for the supercapacitor according to claim 1, wherein the pH value of the dilute hydrochloric acid is between 3.0 and 3.3.
6. The novel lithium ion electrode material for the supercapacitor according to claim 1, wherein the temperature rise rate in the muffle furnace in the step (2) is 1.6-1.8 ℃/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106340637A (en) * | 2015-07-07 | 2017-01-18 | 中国科学院成都有机化学有限公司 | Polysilicate/NCM three-component composite positive electrode material for lithium ion battery and preparation method thereof |
| CN108777299A (en) * | 2018-06-11 | 2018-11-09 | 佛山腾鲤新能源科技有限公司 | A kind of lithium ion battery anode glue size |
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