CN110429250A - A kind of height ratio capacity positive electrode of sodium-sulfur cell material and preparation method thereof - Google Patents

A kind of height ratio capacity positive electrode of sodium-sulfur cell material and preparation method thereof Download PDF

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CN110429250A
CN110429250A CN201910648004.3A CN201910648004A CN110429250A CN 110429250 A CN110429250 A CN 110429250A CN 201910648004 A CN201910648004 A CN 201910648004A CN 110429250 A CN110429250 A CN 110429250A
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titanium dioxide
doped titanium
cobalt doped
sulphur
dioxide nanoplate
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CN110429250B (en
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张永光
王加义
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Zhaoqing South China Normal University Optoelectronics Industry Research Institute
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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
    • H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
    • H01M10/39—Accumulators not provided for in groups H01M10/05-H01M10/34 working at high temperature
    • H01M10/3909—Sodium-sulfur cells
    • 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
    • H01M4/362—Composites
    • 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
    • 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
    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • Y02E60/10—Energy storage using batteries

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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The present invention relates to a kind of height ratio capacity positive electrode of sodium-sulfur cell materials and preparation method thereof.The positive electrode is sulphur-cobalt doped titanium dioxide/carbon nano tube compound material, its preparation process includes, cobalt doped titanium dioxide nanoplate is prepared by hydro-thermal method first, carbon nanotube is grown on its surface by vapour deposition process again, finally sulphur is mixed using ball milling and hot fusion method and prepares sulphur-cobalt doped titanium dioxide/carbon nano tube compound material.The present invention introduces cobalt doped titanium dioxide nanoplate into positive electrode, provides more active sites for electrochemical reaction, promotes the progress of reaction, improves the chemical property of sodium-sulphur battery entirety.

Description

A kind of height ratio capacity positive electrode of sodium-sulfur cell material and preparation method thereof
Technical field
The present invention relates to a kind of height ratio capacity positive electrode of sodium-sulfur cell materials and preparation method thereof, belong to technical field of material chemistry.
Background technique
The energy resource structure of the world today mainly by 37% petroleum, 25% natural gas, 21% coal, 9% nuclear energy with And 3% renewable energy forms.Wherein renewable energy includes geothermal energy, solar energy, wind energy, biomass energy, hydroelectric generation Deng.Demand with people to the energy is continuously increased, and is exploited environmental problem caused by the energy and is also got worse, therefore developing can be again Raw production of energy, transport, conversion and storage problem, are a global problems in the urgent need to address.Improve new energy storage Technology, mainly applies to store renewable energy, such as wind energy, tide energy etc., applied to supporting electric vehicle and electric car Traveling, supports the use of portable electronic product, such as mobile phone, camera, laptop.
It is well known that the most extensive battery of current application is no more than lithium ion battery.Conventional lithium ion battery is due to its reason It is about 387Wh kg by energy density-1, and scarcity of the elemental lithium in the earth's crust, about 0.0065% is only accounted for, expensive, this limitation Its extensive use in the fields such as powered vehicle and the pure electric vehicle vehicles.And in lithium-sulfur cell, because of the theoretical ratio of sulphur Capacity is up to 1675mAh g, and lithium-sulfur cell theoretical energy density is up to 2500Wh kg-1, and sulphur has at low cost, nontoxic, peace The advantages that good perfection.The electrode potential of sodium is the -3.02V that -2.71V is slightly above lithium, and safety is much better.And at sodium and lithium In same main group, electrochemical properties are similar, and sodium element content in the earth's crust accounts for about 2.64%, so our trials are replaced with sodium Lithium constructs sodium-sulphur battery.
However, since metallic sodium is more active than lithium, so Na-S battery facing challenges ratio Li-S battery is more, especially It is in terms of the utilization rate of sulphur active material and circulation volume conservation rate.Similar with lithium-sulfur cell, room temperature sodium-sulphur batter is using When liquid electrolyte, because of the insulating properties of sulphur, polysulfide is soluble in electrolyte and leads to shuttle effect, the originals such as volume expansion Cause leads to low, poor circulation of the utilization rate of sulphur etc., so that the chemical property of sodium-sulphur battery is received and seriously affected.
Summary of the invention
The present invention is low for the existing load sulfur content of existing positive electrode of sodium-sulfur cell material, and shuttle effect is obvious, cyclical stability The problems such as poor, provides a kind of height ratio capacity positive electrode of sodium-sulfur cell material and preparation method thereof.The material is sulphur-cobalt doped titanium dioxide The preparation process of titanium/carbon nano tube compound material, material include cobalt doped titanium dioxide nanoplate is prepared by hydro-thermal method, then Carbon nanotube is grown on its surface by vapour deposition process, finally sulphur is mixed using ball milling and hot fusion method and prepares sulphur-cobalt doped dioxy Change the compound positive electrode of sodium-sulfur cell material of titanium/carbon nanotube.
The preparation method of the height ratio capacity positive electrode of sodium-sulfur cell material, specifically includes the following steps::
(1) cobalt doped titanium dioxide nanoplate is prepared:
Glucose, cabaltous nitrate hexahydrate, titanium sulfate are dissolved in deionized water, it is anti-to be placed in progress hydro-thermal in reaction kettle It answers, it is cooling with room temperature after the reaction was completed, product is collected by centrifugation in gained suspension, after being washed with deionized three times, at 60 DEG C It is spare to be dried to obtain powder；Products therefrom is placed in tube furnace, is heated up under air conditions, with room temperature after heat preservation 1~2 hour Cooling obtains cobalt doped titanium dioxide nanoplate powder；
(2) cobalt doped titanium dioxide nanoplate/carbon nano tube compound material is prepared:
The cobalt doped titanium dioxide nanoplate powder being prepared in step (1) is placed in tube furnace, in argon atmosphere Under with heating, close hydrogen and acetylene after being passed through acetylene and hydrogen gas mixture simultaneously after temperature is constant, under an argon atmosphere Natural cooling obtains cobalt doped titanium dioxide nanoplate/carbon mano-tube composite；
(3) sulphur-cobalt doped titanium dioxide nanoplate/carbon nano tube compound material is prepared:
By cobalt doped titanium dioxide nanoplate/carbon nano tube compound material obtained in step (2) and pure phase nanometer sulphur powder It is put into ball grinder, using planetary ball mill mixed processing, obtained mixture is put into the tube furnace under nitrogen protection Heat treatment, obtains sulphur-cobalt doped titanium dioxide nanoplate/carbon nano tube compound material.
Wherein, it is 10~20g that glucose quality is added in step (1), and cabaltous nitrate hexahydrate quality is 0.1~1g, sulfuric acid Titanium quality is 3~5g, and deionized water volume is 100~200mL, and hydrothermal temperature is 180~200 DEG C, the reaction time 2~4 Hour.
In the step (1), the reaction heating rate in tube furnace is 1~2 DEG C/min, and reaction temperature is 400~600 ℃。
The cobalt doped titanium dioxide nanoplate powder quality being added in the step (2) is 0.1~0.5g, in tube furnace Reaction heating rate be 0.5~1 DEG C/min, reaction temperature be 500~700 DEG C, be passed through hydrogen flow rate be 100~300mL/ Min, acetylene flow velocity are 10~50mL/min, and being continually fed into the time is 10~30min.
Cobalt doped titanium dioxide nanoplate/carbon nano tube compound material for being added in step (3) and pure phase nanometer sulphur powder Mass ratio is 1:2~5.
The revolving speed of planetary ball mill is 500~800r/min in step (3), and incorporation time is 3~5h.
Heat treatment temperature in step (3) tube furnace is 100~200 DEG C, the processing time is 8~for 24 hours.
Beneficial effects of the present invention are as follows:
The present invention introduces cobalt doped titanium dioxide nanoplate/carbon nano tube compound material, cobalt doped two during the preparation process TiOx nano piece provides more active sites for electrochemical reaction, promotes the progress of reaction, improves sodium-sulphur battery Whole chemical property.In addition we introduce carbon nanotube by vapour deposition process, the conductive material outstanding as one kind, The overall electrode material conductivity that exists for of carbon nanotube provides guarantee, and the tubular structure of carbon nanotube carries sulfur content to promotion Also have great importance.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples:
Fig. 1 is cobalt doped titanium dioxide nanoplate transmission electron microscope picture obtained by embodiment 1
Fig. 2 is sulphur-cobalt doped titanium dioxide nanoplate/carbon nano tube compound material electric discharge ratio obtained by embodiment 1 Capacity circulating figure.
Specific embodiment
Embodiment 1:
(1) cobalt doped titanium dioxide nanoplate is prepared:
By 15g glucose, 0.5g cabaltous nitrate hexahydrate, 4g titanium sulfate is dissolved in 150mL deionized water, is placed in 200mL In reaction kettle, hydro-thermal reaction should be descended 3 hours 190, it is cooling with room temperature after the reaction was completed.Production is collected by centrifugation in gained suspension Object, after being washed with deionized three times, 60, under to be dried to obtain powder spare.Then products therefrom is placed in tube furnace, in sky The heating rate for being dried to obtain powder under the conditions of gas with 1 is warming up to 500 temperature, obtains cobalt doped two with room temperature cooling after heat preservation 2 hours TiOx nano piece powder.
(2) cobalt doped titanium dioxide nanoplate/carbon nano tube compound material is prepared:
The cobalt doped titanium dioxide nanoplate powder being prepared in 0.3g step (1) is placed in tube furnace, in argon gas 600 temperature are warming up to the heating rate of 0.5 atmosphere min under atmosphere, are passed through acetylene and hydrogen mixed gas simultaneously after temperature is constant Body, wherein hydrogen flow rate 200mL/min, acetylene flow velocity be 30mL/min, be continually fed into 20min, after the completion close hydrogen and Acetylene, natural cooling, obtains cobalt doped titanium dioxide nanoplate/carbon mano-tube composite under an argon atmosphere.
(3) sulphur-cobalt doped titanium dioxide nanoplate/carbon nano tube compound material is prepared:
By cobalt doped titanium dioxide nanoplate/carbon nano tube compound material obtained in step (2) and pure phase nanometer sulphur powder According to mass ratio be 1:3 be put into ball grinder, using planetary ball mill revolving speed be 600r/min under the conditions of mixed processing 4h, The mixture obtained after ball milling is put into the tube furnace under nitrogen protection, is heat-treated 12h at 150 DEG C, obtains sulphur-cobalt doped Titanium dioxide nanoplate/carbon nano tube compound material is used as positive electrode of sodium-sulfur cell material.
Embodiment 2:
(1) cobalt doped titanium dioxide nanoplate is prepared:
By 10g glucose, 0.1g cabaltous nitrate hexahydrate, 3g titanium sulfate is dissolved in 100mL deionized water, is placed in 200mL It is cooling with room temperature after the reaction was completed lower hydro-thermal reaction 2 hours in 180 in reaction kettle.Production is collected by centrifugation in gained suspension Object, after being washed with deionized three times, 60, under to be dried to obtain powder spare.Then products therefrom is placed in tube furnace, in sky The heating rate for being dried to obtain powder under the conditions of gas with 1 is warming up to 400~600 speed, obtains cobalt with room temperature cooling after heat preservation 1 hour and mixes Miscellaneous titanium dioxide nanoplate powder.
(2) cobalt doped titanium dioxide nanoplate/carbon nano tube compound material is prepared:
The cobalt doped titanium dioxide nanoplate powder being prepared in 0.1g step (1) is placed in tube furnace, in argon gas 500 speed are warming up to the heating rate of 0.5 atmosphere min under atmosphere, are passed through acetylene and hydrogen mixed gas simultaneously after temperature is constant Body, wherein hydrogen flow rate 100mL/min, acetylene flow velocity be 10mL/min, be continually fed into 10min, after the completion close hydrogen and Acetylene, natural cooling, obtains cobalt doped titanium dioxide nanoplate/carbon mano-tube composite under an argon atmosphere.
(3) sulphur-cobalt doped titanium dioxide nanoplate/carbon nano tube compound material is prepared:
By cobalt doped titanium dioxide nanoplate/carbon nano tube compound material obtained in step (2) and pure phase nanometer sulphur powder According to mass ratio be 1:2 be put into ball grinder, using planetary ball mill revolving speed be 500r/min under the conditions of mixed processing 3h, The mixture obtained after ball milling is put into the tube furnace under nitrogen protection, is heat-treated 8h at 100 DEG C, obtains sulphur-cobalt doped Titanium dioxide nanoplate/carbon nano tube compound material is used as positive electrode of sodium-sulfur cell material.
Embodiment 3:
(1) cobalt doped titanium dioxide nanoplate is prepared:
By 20g glucose, 1g cabaltous nitrate hexahydrate, 5g titanium sulfate is dissolved in 200mL deionized water, it is anti-to be placed in 200mL It answers in kettle, it is cooling with room temperature after the reaction was completed lower hydro-thermal reaction 4 hours in 200.Product is collected by centrifugation in gained suspension, After being washed with deionized three times, 60, under to be dried to obtain powder spare.Then products therefrom is placed in tube furnace, in air Under the conditions of with 2 be dried to obtain powder heating rate heating 600 speed, heat preservation 2 hours after with room temperature cooling obtain cobalt doped titanium dioxide Titanium nanometer sheet powder.
(2) cobalt doped titanium dioxide nanoplate/carbon nano tube compound material is prepared:
The cobalt doped titanium dioxide nanoplate powder being prepared in 0.5g step (1) is placed in tube furnace, in argon gas 700 speed are warming up to the heating rate of 1 argon gas min under atmosphere, are passed through acetylene and hydrogen gas mixture simultaneously after temperature is constant, Wherein, hydrogen flow rate 300mL/min, acetylene flow velocity are 50mL/min, are continually fed into 30min, close hydrogen and second after the completion Alkynes, natural cooling, obtains cobalt doped titanium dioxide nanoplate/carbon mano-tube composite under an argon atmosphere.
(3) sulphur-cobalt doped titanium dioxide nanoplate/carbon nano tube compound material is prepared:
By cobalt doped titanium dioxide nanoplate/carbon nano tube compound material obtained in step (2) and pure phase nanometer sulphur powder According to mass ratio be 1:5 be put into ball grinder, using planetary ball mill revolving speed be 800r/min under the conditions of mixed processing 5h, The mixture obtained after ball milling is put into the tube furnace under nitrogen protection, is heat-treated at 200 DEG C for 24 hours, sulphur-cobalt doped is obtained Titanium dioxide nanoplate/carbon nano tube compound material is used as positive electrode of sodium-sulfur cell material.

Claims (8)

1. a kind of height ratio capacity positive electrode of sodium-sulfur cell material, the positive electrode is that sulphur-cobalt doped titanium dioxide/carbon nanotube is multiple Condensation material, which is characterized in that the sulphur-cobalt doped titanium dioxide/carbon nano tube compound material preparation process is to pass through first Hydro-thermal method prepares cobalt doped titanium dioxide nanoplate, then passes through vapour deposition process cobalt doped titanium dioxide nanoplate table made from Long carbon nanotube of looking unfamiliar obtains cobalt doped titanium dioxide nanoplate/carbon nano tube compound material, finally melts work using ball milling and heat Skill mixes sulphur in cobalt doped titanium dioxide nanoplate/carbon nano tube compound material, and sulphur-cobalt doped titanium dioxide/carbon nanometer is made Pipe composite material.
2. the preparation method of the material of height ratio capacity positive electrode of sodium-sulfur cell described according to claim 1, which is characterized in that specific packet Include following steps:
(1) cobalt doped titanium dioxide nanoplate is prepared:
Glucose, cabaltous nitrate hexahydrate, titanium sulfate are dissolved in deionized water, is placed in reaction kettle and carries out hydro-thermal reaction, instead It is cooling with room temperature after the completion of answering, product is collected by centrifugation in gained suspension, it is dry at 60 DEG C after being washed with deionized three times It is spare to powder；Products therefrom is placed in tube furnace, is heated up under air conditions, it is cooling with room temperature after heat preservation 1~2 hour To cobalt doped titanium dioxide nanoplate powder；
(2) cobalt doped titanium dioxide nanoplate/carbon nano tube compound material is prepared:
The cobalt doped titanium dioxide nanoplate powder being prepared in step (1) is placed in tube furnace, under an argon atmosphere with Heating closes hydrogen and acetylene after being passed through acetylene and hydrogen gas mixture simultaneously after temperature is constant, natural under an argon atmosphere It is cooling, obtain cobalt doped titanium dioxide nanoplate/carbon mano-tube composite；
(3) sulphur-cobalt doped titanium dioxide nanoplate/carbon nano tube compound material is prepared:
Cobalt doped titanium dioxide nanoplate/carbon nano tube compound material obtained in step (2) and pure phase nanometer sulphur powder are put into In ball grinder, using planetary ball mill mixed processing, obtained mixture is put into the tube furnace under nitrogen protection at heat Reason, obtains sulphur-cobalt doped titanium dioxide nanoplate/carbon nano tube compound material.
3. preparation method according to claim 2, it is characterised in that: be added in step (1) glucose quality be 10~ 20g, cabaltous nitrate hexahydrate quality are 0.1~1g, and titanium sulfate quality is 3~5g, and deionized water volume is 100~200mL, hydro-thermal Reaction temperature is 180~200 DEG C, the reaction time 2~4 hours.
4. preparation method according to claim 2 or 3, it is characterised in that the reaction heating in step (1), in tube furnace Speed is 1~2 DEG C/min, and reaction temperature is 400~600 DEG C.
5. preparation method according to claim 2, it is characterised in that: the cobalt doped titanium dioxide being added in step (2) is received Rice piece powder quality is 0.1~0.5g, and the reaction heating rate in tube furnace is 0.5~1 DEG C/min, reaction temperature 500 ~700 DEG C, being passed through hydrogen flow rate is 100~300mL/min, and acetylene flow velocity is 10~50mL/min, and being continually fed into the time is 10 ~30min.
6. preparation method according to claim 2, it is characterised in that: the cobalt doped titanium dioxide being added in step (3) is received Rice piece/carbon nano tube compound material and the mass ratio of pure phase nanometer sulphur powder are 1:2~5.
7. the preparation method according to claim 2 or 6, it is characterised in that: the revolving speed of planetary ball mill is in step (3) 500~800r/min, incorporation time are 3~5h.
8. the preparation method according to claim 2 or 6, it is characterised in that: the heat treatment temperature in step (3) tube furnace is 100~200 DEG C, processing the time be 8~for 24 hours.
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