CN108448165A - A kind of Dual-ion cell and preparation method thereof for making cathode using trielement composite material - Google Patents
A kind of Dual-ion cell and preparation method thereof for making cathode using trielement composite material Download PDFInfo
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- CN108448165A CN108448165A CN201810214676.9A CN201810214676A CN108448165A CN 108448165 A CN108448165 A CN 108448165A CN 201810214676 A CN201810214676 A CN 201810214676A CN 108448165 A CN108448165 A CN 108448165A
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
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- H—ELECTRICITY
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
The present invention relates to a kind of Dual-ion cells and preparation method thereof for making cathode using trielement composite material, metal/carbon/graphene trielement composite material is prepared using a step high temperature carbothermic method, make cathode with metal/carbon/graphene trielement composite material, graphite type material makees anode and metal salt electrolyte is assembled into Dual-ion cell.The preparation method of the present invention is simple, and environmentally protective, raw material are simple and easy to get, good cycle under high current, and coulombic efficiency is high.
Description
Technical field
The invention belongs to electrochemical energy storage fields, and in particular to a kind of double ion electricity for making cathode using trielement composite material
Pond and preparation method thereof, and more particularly to a kind of double ion electricity for making cathode using metal/carbon/graphene trielement composite material
Pond and preparation method thereof.
Background technology
Lithium ion battery has specific energy density high, has extended cycle life, and environmental pollution is small and memory-less effect etc. is prominent
Go out advantage, huge success is achieved in electronic field.But lithium metal reserves in the earth's crust are relatively low and are unevenly distributed so that lithium
The cost of manufacture of ion battery is high, so, urgent need exploitation is had excellent performance and resourceful, cheap energy storage technology.Wherein,
Recent years, emerging Dual-ion cell was exactly one of them.
Dual-ion cell, because it is with higher operating voltage, excellent specific energy density and low cost of manufacture etc. are excellent
Point becomes high-performance power battery of new generation, is expected to break through new-energy automobile, including electric vehicle (EV), oil electric mixed dynamic
The bottleneck of electric vehicle (HEV) and plug-in hybrid electric automobile (PHEV) development.There was only Li with lithium ion battery+It participates in
Reaction between positive and negative anodes is different, and Dual-ion cell participates in the reaction between positive and negative anodes there are two types of different ions.When charging, electricity
Solve metal salt in liquid（Such as LiPF6, NaClO4Deng）Anion shift to anode, embedded or adsorption reaction occurs in anode, meanwhile,
The cation of metal salt shifts to cathode, embedded or adsorption reaction occurs in cathode, correspondingly extraneous electric current flows to anode from cathode；
When electric discharge, anion and cation return in electrolyte, corresponding earth-current is from just respectively from anode and cathode abjection or desorption
Pole flows to cathode through external world's load, is a kind of energy storage based on double ion simultaneously, therefore is named as Dual-ion cell.
Currently, it is metal_based material that the most negative material of usage amount, which has two classes, one kind, in Dual-ion cell, such as aluminium foil,
Tinfoil paper etc..When wherein charging, alloy-type insertion reaction can occur with metal salt cation, theoretical specific capacity is high, but is closing
Huge volume change can occur for metal in aurification and removal alloying cyclic process, can bring electrode material structural instability, powder
The problems such as change is serious, failure and poor circulation.Another kind of is pure carbon-based material, such as graphite, expanded graphite, graphene and soft carbon
Plug-in type insertion mechanism or absorbent-type reaction can occur in these carbon materials Deng, metal cation.Carbon material has good
Electron conduction, volume change is small when deintercalation metal ion, is a kind of ideal stable carrier, while having cheap and green
The advantages that colour circle is protected, still, theoretical specific capacity is relatively low, and high rate performance is poor.In conclusion finding a kind of with high theoretical specific volume
Cathode of the composite material for the advantages that amount, is pressed in high electric discharge, and volume change is small when deintercalation metal ion as Dual-ion cell
Material is necessary.
Invention content
In view of the above-mentioned problems, the object of the present invention is to provide a kind of Dual-ion cells for making cathode using trielement composite material
And preparation method thereof, specifically a kind of Dual-ion cell and its system for making cathode using metal/carbon/graphene trielement composite material
Preparation Method, it is above-mentioned existing to solve the problems, such as, obtain with high-energy-density density, long circulation life, excellent high rate performance and
The Dual-ion cell of the advantages that outstanding security performance.
To achieve the above object, the technical solution adopted in the present invention is：It is a kind of that cathode is made using trielement composite material
Metal/carbon/graphene trielement composite material is prepared using a step high temperature carbothermic method in Dual-ion cell, with metal/
Carbon graphite alkene trielement composite material makees cathode, and graphite type material makees anode and metal salt electrolyte is assembled into Dual-ion cell.
The present invention also protects a kind of preparation method of Dual-ion cell that making cathode using trielement composite material, including as follows
Step：
（1）Metal salt, reproducibility organic acid and a variety of nitrogen sources are dissolved into the aaerosol solution of graphene oxide, carried out at dehydration
Obtained presoma is managed, the presoma is subjected to high temperature cabonization processing, obtains metallic particles insertion nitrogen-doped carbon matrix
Metal/carbon/graphene trielement composite material；
（2）By metal/carbon/graphene trielement composite material cathode, graphite type material anode, metal salt electrolyte be assembled into it is double from
Sub- battery.
In the above method, the metal salt be metal zinc salt, metal antimonic salt, metal lead salt and one kind in metal pink salt or
It is several；The metal zinc salt is one or more of zinc chloride, zinc nitrate, zinc acetate and zinc sulfate；The metal antimonic salt is
One or more of antimony trichloride, bromination antimony, Antimony pentachloride and antimony sulfate；The metal lead salt is in plumbi nitras and lead acetate
One or more；The metal pink salt is stannous chloride, nitric acid stannous, butter of tin and one kind or several in stannous oxalate
Kind；The reproducibility organic acid is one or more of tartaric acid, citric acid and grape acid；The nitrogen source be melamine,
One or more of cyanamide, urea and ammonium sulfate.
In the above method, the molar ratio of the metal salt and reproducibility organic acid is (5-90)：100, preferably (10-
70)：100；The molar ratio of reproducibility organic acid and nitrogen source is (10-90)：100, preferably (15-70)：100；Graphene oxide
With the mass ratio 1 of metal salt：(3-10).
In the above method, the high temperature cabonization processing is under argon atmosphere, under 400-1200 DEG C of high temperature, preferably
500-1000 DEG C, carbonization treatment 15-180min, preferably 20-120min are carried out to presoma.
In the above method, the metal salt electrolyte be selected from lithium perchlorate, sodium perchlorate, potassium hyperchlorate, lithium hexafluoro phosphate,
Sodium hexafluoro phosphate, one or more of Potassium Hexafluorophosphate.
In the above method, the voltage of the Dual-ion cell is 1.0 ~ 5.5V.
Compared with prior art, excellent effect of the invention is：
First, it is raw material to select metal salt, reproducibility organic acid, a variety of nitrogen sources and graphene oxide, under the same test conditions
Metal (zinc, antimony, lead or tin etc.)/carbon graphite alkene trielement composite material can be made.So the selection space of raw material is compared
Greatly, and simple and easy to get, coulombic efficiency is high.Entire synthesis technology is very simple, time saving, and safety is at low cost, environmentally protective, is suitble to
Large batch of industrialized production；Second is that prepare metallic particles insertion nitrogen-doped carbon matrix trielement composite material metal (zinc,
Antimony, lead or tin etc.)/carbon graphite alkene makees the synergistic effect that Dual-ion cell negative material is utilized between component, reach difference
The purpose having complementary advantages between component.The current potential of metal ion in metallic particles (zinc, antimony, lead or tin etc.) deintercalation electrolyte
Height can effectively avoid the generation of negative metal dendrite, substantially increase the security performance of Dual-ion cell.Carbon matrix is as gold
The carrier of metal particles, stereomutation that can be with buffer metal particle during repeated charge improve Dual-ion cell and exist
Stable circulation performance under high current.The theoretical specific capacity of metal (zinc, antimony, lead or tin etc.) is generally relatively high, while carbon matrix
The interface contact resistance between metallic particles can be reduced, to effectively increase the high rate performance of Dual-ion cell.
Description of the drawings
It is described further below in conjunction with the accompanying drawings：
Fig. 1 is metallic antimony/carbon graphite alkene trielement composite material cathode X-ray powder diffraction figure that embodiment 1 provides：
Fig. 2 is metallic antimony/carbon graphite alkene trielement composite material cathode TEM Electronic Speculum detection figures that embodiment 1 provides：
Fig. 3 is metallic antimony/carbon graphite alkene trielement composite material cathode HRTEM Electronic Speculum detection figures that embodiment 1 provides：
Fig. 4 is long-term charge and discharge cycles curve graph of the sodium Dual-ion cell that provides of embodiment 1 under 1A/g current densities：
Fig. 5 is high rate performance curve graph of the sodium Dual-ion cell that provides of embodiment 1 under different current densities.
Specific implementation mode
The method of the present invention is illustrated below by specific embodiment, but the present invention is not limited thereto.
Experimental method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
Embodiment 1：Sodium Dual-ion cell preparation method
Antimony trichloride, citric acid and cyanamide are dissolved into successively in a certain amount of graphene oxide aaerosol solution, then carried out
Dehydration obtains the presoma of high temperature cabonization, finally, the carbonization treatment under 700 DEG C of high temperature in the tube furnace of argon gas atmosphere protection
40min obtains metallic antimony/carbon graphite alkene trielement composite material cathode.
Sodium Dual-ion cell is made in glove box, wherein just extremely business expanded graphite, cathode are metallic antimony/carbon/stone
Black alkene trielement composite material cathode, electrolyte are 1M sodium perchlorates（NaClO4）, diaphragm is commercially available diaphragm.Dual-ion cell
Voltage is 2V-4.7V.
Metallic antimony/carbon graphite alkene trielement composite material cathode identifies that it is by simple metal antimony by x-ray powder diffraction instrument
It is formed with agraphitic carbon and without any other dephasign（As shown in Figure 1）.Use TEM（As shown in Figure 2）Its pattern is characterized, it can
To find out that metallic antimony particle is embedded into carbon matrix.Further HRTEM characterizations（As shown in Figure 3）, can be clearly seen that gold
The lattice fringe for belonging to antimony is 0.31nm by measuring lattice fringe spacing, just corresponds to metallic antimony（012）Interplanar distance, card
Bright metallic antimony is come out by success carbon thermal reduction.
As shown in Fig. 4-5, the electrochemistry of sodium Dual-ion cell is had studied using stable circulation performance and high rate performance etc.
Energy.Fig. 4 is long-term cycle stability energy of the sodium Dual-ion cell under 1 A/g high current densities, by 1400 circle charge and discharge
Still possess the high specific discharge capacity of 73 mA h/g after cycle and coulombic efficiency 32 circle after continually and steadily maintain 98% with
On.Fig. 5 is high rate performance of the sodium Dual-ion cell under different current densities, it can be seen from the figure that under low current density
（200 mA/g）, the specific discharge capacity of battery can reach 178 mA h/g.Even if under the high current density of 2 A/g, battery
Still there are 62 mA h/g high specific discharge capacities.Therefore using metallic antimony/carbon graphite alkene trielement composite material as negative material
Preparing sodium Dual-ion cell has excellent specific discharge capacity and super good long-term cycle stability energy.
Embodiment 2：Potassium Dual-ion cell preparation method
Butter of tin, tartaric acid and melamine are dissolved into successively in a certain amount of graphene oxide aaerosol solution, then into
Row dehydration obtains the presoma of high temperature cabonization, finally, in the tube furnace of argon gas atmosphere protection under 900 DEG C of high temperature at carbonization
50min is managed, metallic tin/carbon graphite alkene trielement composite material cathode is obtained.
Potassium Dual-ion cell is made in glove box, wherein just extremely business expanded graphite, cathode are metallic tin/carbon/stone
Black alkene trielement composite material cathode, electrolyte are 1M potassium hyperchlorates（KClO4）, diaphragm is commercially available diaphragm.The electricity of Dual-ion cell
Pressure is 2V-5V.
Embodiment 3：Lithium Dual-ion cell preparation method
Zinc chloride, grape acid and cyanamide are dissolved into successively in a certain amount of graphene oxide aaerosol solution, then taken off
Water process obtains the presoma of high temperature cabonization, finally, the carbonization treatment under 600 DEG C of high temperature in the tube furnace of argon gas atmosphere protection
20min obtains metallic zinc/carbon graphite alkene trielement composite material cathode.
Lithium Dual-ion cell is made in glove box, wherein just extremely business expanded graphite, cathode are metallic zinc/carbon/stone
Black alkene trielement composite material cathode, electrolyte are 1M lithium perchlorates（LiClO4）, diaphragm is commercially available diaphragm.Dual-ion cell
Voltage is 3V-5V.
Embodiment 4：Lithium Dual-ion cell preparation method
Antimony trichloride, tartaric acid and urea are dissolved into successively in a certain amount of graphene oxide aaerosol solution, then taken off
Water process obtains the presoma of high temperature cabonization, finally, the carbonization treatment under 700 DEG C of high temperature in the tube furnace of argon gas atmosphere protection
30min obtains metallic antimony/carbon graphite alkene trielement composite material cathode.
Lithium Dual-ion cell is made in glove box, wherein just extremely business expanded graphite, cathode are metallic antimony/carbon/stone
Black alkene trielement composite material cathode, electrolyte are 1M lithium hexafluoro phosphates（LiPF6）, diaphragm is commercially available diaphragm.Dual-ion cell
Voltage is 3V-5V.
Embodiment 5：Sodium Dual-ion cell preparation method
Lead acetate, tartaric acid and melamine are dissolved into successively in a certain amount of graphene oxide aaerosol solution, then carried out
Dehydration obtains the presoma of high temperature cabonization, finally, the carbonization treatment under 800 DEG C of high temperature in the tube furnace of argon gas atmosphere protection
50min obtains metallic lead/carbon graphite alkene trielement composite material cathode.
Sodium Dual-ion cell is made in glove box, wherein just extremely business expanded graphite, cathode are metallic lead/carbon/stone
Black alkene trielement composite material cathode, electrolyte are 1M sodium hexafluoro phosphates（NaPF6）, diaphragm is commercially available diaphragm.Dual-ion cell
Voltage is 1.5V-5V.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (8)
1. a kind of Dual-ion cell for making cathode using trielement composite material, which is characterized in that use a step high temperature carbon thermal reduction
Metal/carbon/graphene trielement composite material is prepared in method, makees cathode, graphite with metal/carbon/graphene trielement composite material
Class material makees anode and metal salt electrolyte is assembled into Dual-ion cell.
2. the preparation method of Dual-ion cell according to claim 1, which is characterized in that include the following steps：
（1）Metal salt, reproducibility organic acid and a variety of nitrogen sources are dissolved into the aaerosol solution of graphene oxide, carried out at dehydration
Obtained presoma is managed, the presoma is subjected to high temperature cabonization processing, obtains metallic particles insertion nitrogen-doped carbon matrix
Metal/carbon/graphene trielement composite material；
（2）By metal/carbon/graphene trielement composite material cathode, graphite type material anode, metal salt electrolyte be assembled into it is double from
Sub- battery.
3. preparation method according to claim 2, it is characterised in that：The metal salt is metal zinc salt, metal antimonic salt, gold
Belong to one or more of lead salt and metal pink salt；The metal zinc salt is in zinc chloride, zinc nitrate, zinc acetate and zinc sulfate
It is one or more of；The metal antimonic salt is one or more of antimony trichloride, bromination antimony, Antimony pentachloride and antimony sulfate；It is described
Metal lead salt is one or more of plumbi nitras and lead acetate；The metal pink salt is stannous chloride, nitric acid stannous, four chlorinations
One or more of tin and stannous oxalate.
4. preparation method according to claim 2, it is characterised in that：The reproducibility organic acid is tartaric acid, citric acid
One or more of with grape acid；The nitrogen source is one or more of melamine, cyanamide, urea and ammonium sulfate.
5. preparation method according to claim 2, it is characterised in that：The molar ratio of the metal salt and reproducibility organic acid
For (5-90)：100, preferably (10-70)：100；The molar ratio of reproducibility organic acid and nitrogen source is (10-90)：100, preferably
(15-70)：100；The mass ratio 1 of graphene oxide and metal salt：(3-10).
6. preparation method according to claim 2, it is characterised in that：The high temperature cabonization processing is in argon atmosphere
Under, at a high temperature of 400-1200 DEG C, carbonization treatment 15-180min is carried out to presoma；More preferably at 500-1000 DEG C
Under high temperature, carbonization treatment 20-120min is carried out to presoma.
7. preparation method according to claim 2, it is characterised in that：The metal salt electrolyte is selected from lithium perchlorate, high
Sodium chlorate, potassium hyperchlorate, lithium hexafluoro phosphate, sodium hexafluoro phosphate, one or more of Potassium Hexafluorophosphate.
8. preparation method according to claim 2, it is characterised in that：The voltage of the Dual-ion cell is 1.0 ~ 5.5V.
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Cited By (1)
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| CN114927668A (en) * | 2022-06-13 | 2022-08-19 | 海城申合科技有限公司 | Preparation method of nitrogen-doped antimony phosphate/carbon composite material for negative electrode of sodium ion battery |
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