CN106876683B - A kind of Ti3C2Tx/ KIT-1 type is classified sulphur carbon composite - Google Patents
A kind of Ti3C2Tx/ KIT-1 type is classified sulphur carbon composite Download PDFInfo
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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
- H01M4/00—Electrodes
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- 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
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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
- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- 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
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of Ti3C2Tx/ KIT-1 type is classified sulphur carbon composite, by the carbon material of spherical hierarchical structure, the Ti being dispersed in hierarchical structure carbon material3C2TxIt is formed with elemental sulfur, is classified carbon material in outer layer to elemental sulfur and Ti3C2TxIt is coated, wherein Ti3C2Tx: carbon: the mass ratio of sulphur is 0.1-0.3:0.1-0.3:1, and classification carbon material micro-pore carbon material made of the organic carbon of meso-porous carbon material and external sheath forms.Ti in the composite material3C2TxOn T be-F group or-OH group, oxygen with surface of graphene oxide is highly polar group, strong chemisorption can be formed to the polysulfide formed in charge and discharge process, the micropore of porous carbon materials also can carry out physical absorption to polysulfide simultaneously, it is this while there is the ability of physics and chemisorption effectively polysulfide can be prevented to move, the generation for reducing shuttle effect, improves the service life of lithium-sulfur cell.
Description
Technical field
The present invention relates to nano material synthesis, in particular to a kind of preparation method of lithium sulfur battery anode material.
Background technique
Lithium-sulfur cell is using lithium metal as cathode, and elemental sulfur is the battery system of anode.There are two put the tool of lithium-sulfur cell
Level platform (about 2.4 V and 2.1 V), but its electrochemical reaction mechanism is more complicated.Lithium-sulfur cell has specific energy high
(2600 Wh/kg), specific capacity height (1675 mAh/g), it is at low cost the advantages that, it is considered to be very promising a new generation's electricity
Pond.But there is the problems such as active material utilization is low, cycle life is low and safety is poor at present, this seriously restricts lithium
The development of sulphur battery.The main reason for causing the above problem has the following aspects: (1) elemental sulfur is electronics and ion insulation
Body, room-temperature conductivity low (5 × 10-30S·cm-1), since the sulphur of not no ionic state exists, thus it is tired as positive electrode activation
It is difficult；(2) the poly- more lithium sulfide Li of state of height generated in electrode process2Sn(8 n >=4 >) are soluble in electrolyte, positive and negative
Concentration difference is formed between pole, cathode is moved under the action of concentration gradient, and the high poly- more lithium sulfides of state are reduced into low by lithium metal
The poly- more lithium sulfides of state.With the progress reacted above, the oligomeric more lithium sulfides of state are assembled in cathode, are finally formed between electrodes
Concentration difference, and move to anode and be oxidized to the high poly- more lithium sulfides of state.This phenomenon is referred to as shuttle effect, reduces sulphur activity
The utilization rate of substance.Insoluble Li simultaneously2S and Li2S2It is deposited on cathode of lithium surface, is further degrading lithium-sulfur cell
Performance；(3) final product Li is reacted2S is equally electronic body, can be deposited on sulfur electrode, and lithium ion vulcanizes in solid-state
Migration velocity is slow in lithium, keeps electrochemical reaction kinetic rate slack-off；(4) sulphur and final product Li2The density of S is different, works as sulphur
It is lithiated rear volume expansion about 79%, easily leads to Li2The dusting of S causes the safety problem of lithium-sulfur cell.Above-mentioned insufficient restriction
The development of lithium-sulfur cell, this is also the Important Problems that the research of current lithium-sulfur cell needs to solve.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of Ti3C2Tx/ KIT-1 type is classified sulphur carbon composite, this is multiple
Carbon material of the condensation material by spherical hierarchical structure, the Ti that is dispersed in hierarchical structure carbon material3C2TxIt is formed with elemental sulfur, classification
Carbon material is in outer layer to elemental sulfur and Ti3C2TxIt is coated, wherein Ti3C2Tx: carbon: the mass ratio of sulphur is 0.1-0.3:0.1-
0.3:1, classification carbon material micro-pore carbon material made of the organic carbon of meso-porous carbon material and external sheath form.
The present invention provides a kind of Ti3C2Tx/ KIT-1 type be classified sulphur carbon composite the preparation method is as follows:
(1) eight silsesquioxane of 1.5mmol octaphenyl is added to 70mL 1, in 2- dichloroethanes, is stirred in 60 DEG C of machinery
Dissolution is mixed, Ti is added3AlC2Ceramic powders and KIT-1 powder, stirring form suspension；
(2) 2mmol anhydrous aluminum chloride catalyst is added into suspension and 40 mL carbon tetrachloride crosslinking agents are added, stirring
After reaction ethanol/water solution is added, ethyl alcohol/dilute hydrochloric acid solution is washed, washes, is dried in vacuo, before obtaining in cross-linking reaction 10h
Drive body；
(3) presoma is placed in the Muffle furnace of nitrogen atmosphere protection, the reaction of 900 DEG C 3h2 °C/min high temperature cabonization；
(4) product after carbonization is placed in hydrofluoric acid and is performed etching, solution is added deionized water and is centrifuged after corrosion
Processing, then sediment is dried, obtain Ti3C2Tx/ spherical porous carbon material；
(5) by Ti3C2Tx/ spherical porous carbon material is uniformly mixed with elemental sulfur, is placed in 155- in the tube furnace of sealing
165 DEG C are reacted 12 hours, are heated to 200 DEG C and are passed through nitrogen reaction 30 minutes, after natural cooling, obtain Ti3C2Tx/ sulphur carbon is multiple
Condensation material.
Eight silsesquioxane of octaphenyl in step (1): the ratio of 1,2- dichloroethanes is 1g:50-100mL, is stirred to react
Temperature is 50-70 DEG C, eight silsesquioxane of octaphenyl and Ti3AlC2The mass ratio of ceramic powders is 1:0.05-0.5, octaphenyl eight
The mass ratio of silsesquioxane and KIT-1 are 1:0.05-0.5;
Catalyst is anhydrous aluminum chloride in step (2), and the quality of catalyst is the 5- of eight silsesquioxane quality of octaphenyl
10%, crosslinking agent is carbon tetrachloride, and crosslinking agent quality is eight 10-40 times of silsesquioxane quality of octaphenyl, is stirred to react the time and is
5-10 hours, ethyl alcohol in ethanol/water solution: the volume ratio of water was 2-4:1, and dilute hydrochloric acid is quality point in ethyl alcohol/dilute hydrochloric acid solution
The hydrochloric acid solution that number is 10%, ethyl alcohol and dilute hydrochloric acid volume ratio 2-4:1;
Reaction atmosphere in step (3) in Muffle furnace is nitrogen, 800-1200 DEG C of reaction temperature, reaction time 1-5 hour,
1-5 °C/minute of heating rate；
The concentration of hydrofluoric acid is 20%-50% in step (4), and the time of corrosion is 4-24 hours;
Ti in step (5)3C2TxThe mass ratio of/spherical porous carbon material and elemental sulfur is 0.1-0.3:1, in tube furnace just
Phase reaction temperature is 155-165 DEG C, and the reaction time is 10-20 hours, and the reaction temperature after being passed through nitrogen is 180-200 DEG C, instead
It is 10-30 minutes between seasonable.
The invention has the following beneficial effects: (1) Ti3C2Tx/ KIT-1 type, which is classified in sulphur carbon composite, has classification
Pore structure, by a large amount of micropore and it is mesoporous form, it is internal it is mesoporous surrounded by external micropore, the advantage of this structure is,
Sulphur can be injected into internal meso-hole structure, and external lesser micropore can as a physical barriers of limitation lithium polysulfide
To provide effective storage sulphur space；(2) carbon material of the composite material external sheath effectively limits the movement of sulfenyl material, makes
It is only in internal motion；(3) Ti in the composite material3C2TxOn T be-F group or-OH group, with surface of graphene oxide
Oxygen be highly polar group, strong chemisorption can be formed to the polysulfide formed in charge and discharge process, while porous
The micropore of carbon material can also carry out physical absorption to polysulfide, this while having the ability of physics and chemisorption effective
Prevention polysulfide movement, reduce shuttle effect generation, improve the service life of lithium-sulfur cell.
Detailed description of the invention
Fig. 1 is the preparation technology flow chart of composite material of the present invention.
Fig. 2 is the charge-discharge performance figure of composite material of the present invention.
Specific embodiment
With reference to the accompanying drawing, preferably embodiment of the invention is described in further detail:
Embodiment 1
(1) eight silsesquioxane of 1g octaphenyl is added to 50mL 1, it is molten in 50 DEG C of mechanical stirrings in 2- dichloroethanes
Solution, adds 0.05gTi3AlC2Ceramic powders and 0.05g KIT-1 powder, stirring form suspension；
(2) 0.05g anhydrous aluminum chloride catalyst is added into suspension and 10g carbon tetrachloride crosslinking agent is added, stirring is handed over
After reaction ethanol/water solution is added, ethyl alcohol/dilute hydrochloric acid solution is washed, washes, is dried in vacuo, before obtaining in connection reaction 5 hours
Drive body；
(3) presoma is placed in the Muffle furnace of nitrogen atmosphere protection, 800 DEG C of calcinings 5h, 1 °C/min of heating rate；
(4) by the product after carbonization be placed in concentration be 20% hydrofluoric acid in etch 24 hours, after corrosion solution be added go from
Sub- water carries out centrifugal treating, then dries sediment, obtains Ti3C2Tx/ spherical porous carbon material；
(5) by 0.1g Ti3C2Tx/ spherical porous carbon material is uniformly mixed with 1g elemental sulfur, is placed in the tube furnace of sealing
Interior 165 DEG C are reacted 10 hours, are heated to 200 DEG C and are passed through nitrogen reaction 10 minutes, after natural cooling, obtain Ti3C2Tx/ KIT-
1 type is classified sulphur carbon composite.
Embodiment 2
(1) eight silsesquioxane of 1g octaphenyl is added to 100mL 1, it is molten in 70 DEG C of mechanical stirrings in 2- dichloroethanes
Solution, adds 0. 5gTi3AlC2Ceramic powders and 0. 5g KIT-1 powder, stirring form suspension；
(2) 0.1g anhydrous aluminum chloride catalyst is added into suspension and 40g carbon tetrachloride crosslinking agent is added, stirring crosslinking
After reaction ethanol/water solution is added, ethyl alcohol/dilute hydrochloric acid solution is washed, washes, is dried in vacuo, before obtaining in reaction 10 hours
Drive body；
(3) presoma is placed in the Muffle furnace of nitrogen atmosphere protection, 1200 DEG C of calcinings 1h, 5 °C/min of heating rate；
(4) product after carbonization is placed in concentration is to etch 4 hours in 50% hydrofluoric acid, and deionization is added in solution after corrosion
Water carries out centrifugal treating, then dries sediment, obtains Ti3C2Tx/ spherical porous carbon material；
(5) by 0.3g Ti3C2Tx/ spherical porous carbon material is uniformly mixed with 1g elemental sulfur, is placed in the tube furnace of sealing
Interior 155 DEG C are reacted 20 hours, are heated to 180 DEG C and are passed through nitrogen reaction 30 minutes, after natural cooling, obtain Ti3C2Tx/ KIT-
1 type is classified sulphur carbon composite.
Embodiment 3
(1) eight silsesquioxane of 1g octaphenyl is added to 70mL 1, it is molten in 60 DEG C of mechanical stirrings in 2- dichloroethanes
Solution, adds 0.1gTi3AlC2Ceramic powders and 0.2g KIT-1 powder, stirring form suspension；
(2) 0.08g anhydrous aluminum chloride catalyst is added into suspension and 20g carbon tetrachloride crosslinking agent is added, stirring is handed over
After reaction ethanol/water solution is added, ethyl alcohol/dilute hydrochloric acid solution is washed, washes, is dried in vacuo, before obtaining in connection reaction 8 hours
Drive body；
(3) presoma is placed in the Muffle furnace of nitrogen atmosphere protection, 1000 DEG C of calcinings 3h, 3 °C/min of heating rate；
(4) product after carbonization is placed in concentration is to etch 16 hours in 30% hydrofluoric acid, and deionization is added in solution after corrosion
Water carries out centrifugal treating, then dries sediment, obtains Ti3C2Tx/ spherical porous carbon material；
(5) by 0.2g Ti3C2Tx/ spherical porous carbon material is uniformly mixed with 1g elemental sulfur, is placed in the tube furnace of sealing
Interior 160 DEG C are reacted 15 hours, are heated to 190 DEG C and are passed through nitrogen reaction 20 minutes, after natural cooling, obtain Ti3C2Tx/ KIT-
1 type is classified sulphur carbon composite.
Embodiment 4
(1) eight silsesquioxane of 1g octaphenyl is added to 80mL 1, it is molten in 65 DEG C of mechanical stirrings in 2- dichloroethanes
Solution, adds 0.2gTi3AlC2Ceramic powders and 0.4g KIT-1 powder, stirring form suspension；
(2) 0.07g anhydrous aluminum chloride catalyst is added into suspension and 30g carbon tetrachloride crosslinking agent is added, stirring is handed over
After reaction ethanol/water solution is added, ethyl alcohol/dilute hydrochloric acid solution is washed, washes, is dried in vacuo, before obtaining in connection reaction 6 hours
Drive body；
(3) presoma is placed in the Muffle furnace of nitrogen atmosphere protection, 900 DEG C of calcinings 4h, 2 °C/min of heating rate；
(4) product after carbonization is placed in concentration is to etch 10 hours in 40% hydrofluoric acid, and deionization is added in solution after corrosion
Water carries out centrifugal treating, then dries sediment, obtains Ti3C2Tx/ spherical porous carbon material；
(5) by 0.15g Ti3C2Tx/ spherical porous carbon material is uniformly mixed with 1g elemental sulfur, is placed in the tubular type of sealing
It is reacted 18 hours for 158 DEG C in furnace, is heated to 185 DEG C and is passed through nitrogen reaction 25 minutes, after natural cooling, obtain Ti3C2Tx/
KIT-1 type is classified sulphur carbon composite.
Embodiment 5
(1) eight silsesquioxane of 1g octaphenyl is added to 60mL 1, it is molten in 55 DEG C of mechanical stirrings in 2- dichloroethanes
Solution, adds 0.3gTi3AlC2Ceramic powders and 0.2g KIT-1 powder, stirring form suspension；
(2) 0.09g anhydrous aluminum chloride catalyst is added into suspension and 25g carbon tetrachloride crosslinking agent is added, stirring is handed over
After reaction ethanol/water solution is added, ethyl alcohol/dilute hydrochloric acid solution is washed, washes, is dried in vacuo, before obtaining in connection reaction 7 hours
Drive body；
(3) presoma is placed in the Muffle furnace of nitrogen atmosphere protection, 1100 DEG C of calcinings 2h, 4 °C/min of heating rate；
(4) product after carbonization is placed in concentration is to etch 12 hours in 35% hydrofluoric acid, and deionization is added in solution after corrosion
Water carries out centrifugal treating, then dries sediment, obtains Ti3C2Tx/ spherical porous carbon material；
(5) by 0.25g Ti3C2Tx/ spherical porous carbon material is uniformly mixed with 1g elemental sulfur, is placed in the tubular type of sealing
It is reacted 13 hours for 1625 DEG C in furnace, is heated to 195 DEG C and is passed through nitrogen reaction 20 minutes, after natural cooling, obtain Ti3C2Tx/
KIT-1 type is classified sulphur carbon composite.
The preparation and performance test of electrode；By composite material, acetylene black and PVDF 80:10:10 in mass ratio in NMP
Mixing, being coated in is electrode film on aluminium foil, and metal lithium sheet is to electrode, and CELGARD 2400 is diaphragm, the LiTFSI/ of 1mol/L
DOL-DME (volume ratio 1:1) is electrolyte, and the LiNO3 of 1mol/L is additive, electric full of button is assembled into Ar glove box
Pond carries out constant current charge-discharge test using Land battery test system.Charging/discharging voltage range is 1-3V, and current density is
0.5C, performance are as shown in table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| First discharge specific capacity (mAh/g) | 880 | 890 | 881 | 878 | 886 |
Fig. 2 is the charge-discharge performance figure that 1 composite material of the embodiment of the present invention is prepared into lithium-sulfur cell.As can be seen from the figure
Efficiency for charge-discharge can achieve 99% or more, and first charge-discharge capacity is 920 mAh/g, efficiency for charge-discharge 99.2%, fill for 500 times
After discharge cycles, capacity still possesses 73%, illustrates that the structure of the composite material can effectively inhibit shuttle effect, improves sulphur battery
Service life.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, In
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (3)
1. a kind of Ti3C2Tx/ KIT-1 type is classified sulphur carbon composite, which is characterized in that by the carbon material of spherical hierarchical structure,
Ti3C2Tx and the elemental sulfur composition being dispersed in hierarchical structure carbon material, are classified carbon material in outer layer to elemental sulfur and Ti3C2Tx
Coated, wherein Ti3C2Tx: carbon: the mass ratio of sulphur is 0.1-0.3:0.1-0.3:1, is classified carbon material by meso-porous carbon material
The composition of micro-pore carbon material made of organic carbon with external sheath；T on Ti3C2Tx is-F group or-OH group；It is described
The preparation method of composite material comprises the following steps:
Step (1): eight silsesquioxane of octaphenyl is added in 1,2- dichloroethanes, and mechanical stirring dissolution adds
Ti3AlC2 ceramic powders and KIT-1 powder, stirring form suspension；
Step (2): anhydrous aluminum chloride catalyst being added into suspension and carbon tetrachloride is added, and stirring crosslinking reacts 10h, reaction
After, ethanol/water solution is added, ethyl alcohol/dilute hydrochloric acid solution is washed, washes, is dried in vacuo, and presoma is obtained；
Presoma is placed in the Muffle furnace of nitrogen atmosphere protection by step (3), is increased to temperature with the heating rate of 2 °C/min
900 DEG C, then high temperature cabonization reacts 3h at a temperature of 900 DEG C；
Product after carbonization is placed in hydrofluoric acid by step (4) to be performed etching, and solution is added deionized water and is centrifuged after corrosion
Processing, then sediment is dried, obtain the spherical porous carbon material of Ti3C2Tx/；
The spherical porous carbon material of Ti3C2Tx/ is uniformly mixed by step (5) with elemental sulfur, is placed in 155- in the tube furnace of sealing
165 DEG C are reacted 12 hours, are heated to 200 DEG C and are passed through nitrogen reaction 30 minutes, after natural cooling, obtain Ti3C2Tx/ KIT-1
Type is classified sulphur carbon composite；Eight silsesquioxane of octaphenyl in the step (1): the ratio of 1,2- dichloroethanes is 1g:50-
100mL, being stirred to react temperature is 50-70 DEG C, and the mass ratio of eight silsesquioxane of octaphenyl and Ti3AlC2 ceramic powders is 1:
The mass ratio of 0.05-0.5, eight silsesquioxane of octaphenyl and KIT-1 are 1:0.05-0.5；Catalyst is in the step (2)
Anhydrous aluminum chloride, the quality of catalyst are the 5-10% of eight silsesquioxane quality of octaphenyl, and crosslinking agent is carbon tetrachloride, crosslinking
Agent quality is eight 10-40 times of silsesquioxane quality of octaphenyl, and being stirred to react the time is 5-10 hours, second in ethanol/water solution
Alcohol: the volume ratio of water is 2-4:1, and dilute hydrochloric acid is the hydrochloric acid solution that mass fraction is 10% in ethyl alcohol/dilute hydrochloric acid solution, ethyl alcohol with
Dilute hydrochloric acid volume ratio 2-4:1.
2. Ti3C2Tx/ KIT-1 type as described in claim 1 is classified sulphur carbon composite, which is characterized in that the step
(4) concentration of hydrofluoric acid is 20%-50% in, and the time of corrosion is 4-24 hours.
3. Ti3C2Tx/ KIT-1 type as described in claim 1 is classified sulphur carbon composite, which is characterized in that the step
(5) mass ratio of the spherical porous carbon material of Ti3C2Tx/ and elemental sulfur is 0.1-0.3:1 in.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105024054A (en) * | 2015-07-11 | 2015-11-04 | 中国计量学院 | Preparation method for polymer/hollow sulfur composite electrode material |
| CN105958031A (en) * | 2016-06-30 | 2016-09-21 | 湖南桑顿新能源有限公司 | Sulfur-based cathode composite material and preparation method thereof |
| CN106450205A (en) * | 2016-11-02 | 2017-02-22 | 南京工业大学 | Two-dimensional transition metal carbide (nitride) and nano sulfur particulate composite as well as preparation and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105024054A (en) * | 2015-07-11 | 2015-11-04 | 中国计量学院 | Preparation method for polymer/hollow sulfur composite electrode material |
| CN105958031A (en) * | 2016-06-30 | 2016-09-21 | 湖南桑顿新能源有限公司 | Sulfur-based cathode composite material and preparation method thereof |
| CN106450205A (en) * | 2016-11-02 | 2017-02-22 | 南京工业大学 | Two-dimensional transition metal carbide (nitride) and nano sulfur particulate composite as well as preparation and application thereof |
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