CN105990569A - Preparation method of sulfur-carbon composite powder material, powder material, and application of powder material - Google Patents
Preparation method of sulfur-carbon composite powder material, powder material, and application of powder material Download PDFInfo
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- CN105990569A CN105990569A CN201510080480.1A CN201510080480A CN105990569A CN 105990569 A CN105990569 A CN 105990569A CN 201510080480 A CN201510080480 A CN 201510080480A CN 105990569 A CN105990569 A CN 105990569A
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- 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
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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 invention provides a preparation method of a high-performance sulfur-carbon composite powder material. The method concretely comprises the following steps: 1, placing a carbon powder material in a fluidized bed, continuously introducing a gas from the bottom of the fluidized bed, and adjusting the flow velocity of the gas to make the carbon powder be in a fluidized state; and 2, processing elemental sulfur to prepare liquid sulfur, keeping the temperature of the liquid sulfur in a range of 113-440DEG C, atomizing the liquid sulfur, spraying the atomized liquid sulfur into the fluidized bed to make the atomized liquid sulfur be in contact with the fluidized carbon powder material, and cooling the contact mixture to prepare the sulfur-carbon composite powder material. The sulfur-carbon composite powder material prepared in the invention has the following advantages: the sulfur/carbon ratio and the particle size are adjustable and controllable, carbon and sulfur are uniformly distributed in the composite material, and the particle size of the material is uniform; sulfur and carbon are compactly combined in the composite material, and the electricity conductivity is high; carbon coated outside sulfur can effectively inhibit dissolving loss and shuttle effect of polysulfide; and the composite powder material has a spherical or spheroidic morphology and high tap density, and the processing performance of the material is improved.
Description
Technical field
The invention belongs to field of chemical power source, relate to the preparation of a kind of lithium sulfur battery anode material
Method, particularly to the preparation method of a kind of high-performance sulfur carbon composite powder material.
Background technology
Social development is growing to the demand of energy storage technology.Lithium-sulfur cell has high theory
Energy density 2600Wh/kg, battery raw material rich reserves, low cost and other advantages, have
Wide application potential, becomes the study hotspot of high specific energy secondary cell.
But there are some problems in lithium-sulfur cell.First, the ionic conductivity of elemental sulfur and electronics
Electric conductivity is extremely low；Secondly, the intermediate product polysulfide of discharge process is easily soluble in organic molten
Agent, occurs " effect of shuttling back and forth ", causes the loss of sulfur and the corrosion of lithium metal, ultimately cause electricity
Tankage decay and service life reduction.Additionally, electric discharge end-product Li2S or Li2S2Electric insulation
Property, insoluble, and elemental sulfur volumetric expansion before and after discharge and recharge also results in circulating battery
Degradation.
Preparing sulfur carbon composite is to improve lithium sulfur battery anode material electrical conductivity, suppression " effect of shuttling back and forth
Should " effective means.The method of preparation includes ball milling mixing method, sulfur sublimed method, sulfur dissolution method
Deng.Material sulfur, carbon distribution that ball-milling method prepares are uneven.Sulfur sublimed method prepares the sulfur of material
Actual loading on the low side.The majority of organic solvent used in sulfur dissolution method has toxicity,
To environment.
Therefore, need badly exploitation a kind of " sulfur/carbon " than and material granule size tunable, efficiently multiple
Close, sphericity is high and pollution-free, low cost, technique simple, the sulfur carbon of favorable reproducibility is multiple
Close the preparation method of powder body material, to improve chemical property and the cyclical stability of material；
And improve energy density and the cycle life of lithium-sulfur cell further.
Summary of the invention
It is an object of the invention to provide the preparation side of a kind of high-performance sulfur carbon composite powder material
Method.The sulfur carbon ratio of sulfur carbon composite powder material prepared by the method is controlled, the ball of powder body material
Shape degree is high, size tunable.Preparation technology is simple, low cost, homogeneity of product are high, environment
Close friend, is suitable for large-scale production.
The invention provides the preparation method of a kind of high-performance sulfur carbon composite powder material, it is special
Levy and be, first prepare liquid sulfur, at high temperature, liquid sulfur is atomized, with the powder of the carbon of fluidisation
Body material contacts with each other, and chilling prepares " sulfur/carbon " ratio and the adjustable controlled composite granule of particle diameter
Material；Specifically comprise the steps of
Step 1: the powder body material of carbon is placed in fluid bed, persistently leads to from fluidized-bed bottom
Entering gas, regulation gas flow rate makes carbon dust be in fluidized state；
Step 2: elemental sulfur is made liquid sulfur, keeps the temperature of liquid sulfur at 113-
440 DEG C, liquid sulfur is atomized, the liquid sulfur of atomization is sprayed into fluid bed, the liquid sulfur of atomization
Contact with each other with the powder body material of the carbon of fluidisation, prepare sulfur carbon composite powder material.
Spraying stops, and fluidized-bed bottom ventilation stops, and carries out discharging.
The elemental sulfur used is 1:9 9:1 with the mass ratio of the powder body material of carbon；The powder of carbon
The particle diameter D of body material50For 0.01-10 μm.
Described elemental sulfur is the one in refined sulfur, Sublimed Sulfur or sedimentation sulfur or two kinds or three
Kind；The powder body material of described carbon is hard carbon or soft carbon or the one of graphite or two kinds or three
Kind, the pattern of the powder body material of carbon be graininess, spherical, fibrous, tubulose, lamellar or
One or two or more kinds of cystose.
Using heat melting method that elemental sulfur is made liquid sulfur, the heating-up temperature of heat fusing is 113-
440 DEG C, carry out in nitrogen or argon gas atmosphere.
In step 1, gases used for one or both in nitrogen or argon, the temperature of gas
Degree is for-30-100 DEG C；Gas flow rate is 0.1m/s-120m/s.
In step 2, when using air-blast atomization, atomization needs use atomization gas, mist
Change gas is one or both in nitrogen or argon；The liquid sulfur of atomization and atomization gas
Between mass ratio be 1:20-100:1；The aerodynamic atomization pressure of atomization gas is 0.1-10MPa；
The nozzle of nebulizer and the distance of fluid bed are 1-20m, and the liquid sulfur of atomization is sprayed from nebulizer
The speed of mouth ejection is 0.1-120m/s, the particle diameter D of the liquid sulfur of atomization50For 0.01-
30μm。
The sulfur carbon composite powder material prepared according to the method described above, in carbon sulfur composite powder material
Sulfur is 1:9 9:1 with the mass ratio of carbon, the particle diameter D of solid sulfur in material50For 0.02-
30μm。
The sulfur carbon composite powder materials application prepared according to the method described above is in lithium-sulfur rechargeable battery
Positive electrode.
The present invention can use equipment as shown in Figure 1 to synthesize, and synthesis device includes liquid
State sulfur supply system, nebulizer, fluid bed, compressed gas supply system and fluidizing gas supply
Answer system.
The fluid reservoir in liquid sulfur supply system in synthesis, feed pump, nebulizer, heating
Device, heat indicator, and the pipeline sealing between it, and it is provided with attemperator.
Compressed gas supply system in synthesis device include gas compressor a, heater,
Effusion meter, Pressure gauge, heat indicator, pipeline, and good airproof performance.
Fluidizing gas supply system in synthesis device include gas compressor b, heater,
Effusion meter, Pressure gauge, heat indicator, pipeline, and good airproof performance.
Liquid sulfur fluid reservoir, feed pump, nebulizer and the pipeline sealing between it, and join
There are heater, heating-up temperature 110-440 DEG C；
The invention have the advantages that
(1) " sulfur/carbon " of the sulfur carbon composite that the present invention prepares is than adjustable controlled with particle diameter, multiple
Being evenly distributed of carbon and sulfur in condensation material, the uniform particle diameter of material.
(2) present invention prepares carbon sulfur composite sulfur and carbon combine densification, and electrical conductivity is high.
(3) the carbon sulfur composite that the present invention prepares, the carbon of sulfur external sheath can effectively suppress many sulfur
The loss by dissolution of compound and effect of shuttling back and forth.
(4) the sulfur carbon composite powder material that the present invention prepares has spherical or class spherical morphology, shakes
Real density is high, improves the processing characteristics of electrode plates.
(5) present invention uses total enclosing equipment, and preparation process whole process is pollution-free, environmental friendliness.
(6) adjustable controlled, the process of the technological parameter of the present invention is simple, processing ease, low cost,
Homogeneity of product is high, is suitable for large-scale production.
Therefore, technical scheme have that Parameter adjustable is controlled, technique and simple to operate,
Environmental friendliness, the advantage of low cost, the composition of obtained sulfur carbon composite is controlled, can
Adjusting, electrical conductivity is high, has spherical morphology, uniform particle diameter, and tap density is high, and pole piece is processed
Performance is good, it is adaptable to the high performance electrode material of lithium-sulfur cell sulfur positive pole.
The present invention is by atomized liquid sulfur, the powder body material of fluidisation carbon, by ejection atomized liquid
Sulfur, utilizes collision between the two, strong interaction, directly prepares sulfur carbon composite.
The size of atomized sulfur droplets, and then regulation and control composite can be regulated and controled by controlling atomization parameter
The size of middle sulfur；Again by controlling the particle diameter of toner body material, final sulfur carbon can be regulated and controled multiple
" sulfur/carbon " ratio of condensation material, and the particle diameter of composite powder material.Therefore, material have sulfur,
The advantage that carbon composition is evenly distributed and material particle size is homogeneous.Meanwhile, the composite prepared
In, sulfur and carbon combine densification, beneficially electric transmission, improve the electrical conductivity of composite and shake
Real density；Further, the carbon of sulfur external sheath also can effectively suppress the loss by dissolution of polysulfide
With effect of shuttling back and forth.Higher tap density and spherical morphology also improve the electrode plates of material
Processing characteristics.
Accompanying drawing explanation
The equipment of the preparation method of Fig. 1 sulfur carbon composite powder material and process schematic.
1 fluid reservoir, 2 feed pumps, 3 nebulizers, 4 fluid beds, 5 gas compressor a, 6
Heater, 7 effusion meters, 8 gas compressor b, 9 heaters, 10 effusion meters.
Detailed description of the invention
With embodiment, the detailed description of the invention of the present invention is carried out furtherly below in conjunction with the accompanying drawings
Bright, but it is not to be regarded as the restriction to protection scope of the present invention.
The following example is all carried out in Fig. 1 shown device, the liquid sulfur supply system in device
Fluid reservoir, feed pump, nebulizer, heater and the pipeline sealing between it in system,
And it being provided with attemperator, attemperator is set by the thermostat temperature in following example respectively
Put.
Embodiment 1:
Step 1: under room temperature, refines 30kg sulfur and joins the liquid sulfur supply system of synthesis device
In, be passed through nitrogen, 115 DEG C by sulfur heat fusing to liquid, and constant temperature 115 DEG C is stored in
In fluid reservoir；
Step 2: by 30kg particle diameter D50The graphene powder being about 2.6m joins fluid bed
In；
Step 3: start gas compressor, compressed nitrogen enters from fluidized-bed bottom, regulates gas
Flow velocity about 0.5m/s, makes graphene powder be in fluidized state, and the temperature of nitrogen is-30 DEG C；
Step 4: the liquid sulfur in fluid reservoir is delivered in atomization chamber and is passed through nitrogen, sulfur and nitrogen
The mass ratio of gas is 1:1, and the aerodynamic atomization pressure of nitrogen is 0.2MPa, by the liquid of atomization
Sulfur is with flow velocity in about 2m/s sprays into fluid bed；Atomizer nozzle to the distance of fluid bed is
10m, heating devices heat temperature is 115 DEG C；The atomizing particle size D of liquid sulfur50It is about
0.1μm；
Prepare " sulfur/Graphene " composite, the particle diameter D of sulfur ball in material50It is about
20m, " sulfur/carbon " mass ratio about 1:1.
Embodiment 2:
Step 1: under room temperature, settles 1kg sulfur and joins the liquid sulfur supply system of synthesis device
In.Be passed through nitrogen, 200 DEG C by sulfur heat fusing to liquid, and constant temperature 200 DEG C is stored in
In fluid reservoir；
Step 2: by 9kg particle diameter D50It is about 0.01m and there is the carbon black powders of meso-hole structure
Join in fluid bed；
Step 3: start gas compressor, compressed nitrogen enters from fluidized-bed bottom, regulates gas
Flow velocity is about 100m/s, makes carbon dust be in fluidized state, the temperature of nitrogen 100 DEG C；
Step 4: the liquid sulfur in fluid reservoir is delivered in atomization chamber and is passed through nitrogen, sulfur and nitrogen
The mass ratio of gas is 1:10, and the aerodynamic atomization pressure of nitrogen is 10MPa, by the liquid of atomization
Sulfur is with flow velocity about 120m/s, and the distance of atomizer nozzle to fluid bed is 2m；Heater
Heating-up temperature is 200 DEG C；The atomizing particle size D of liquid sulfur50It is about 0.005 μm；
Prepare " sulfur/carbon black " composite, the particle diameter D of sulfur in material50It is about 0.02m,
" sulfur/carbon " mass ratio about 1:9.
Embodiment 3:
Step 1: under room temperature, joins the liquid sulfur supply system of synthesis device by 81kg Sublimed Sulfur
In.Be passed through argon, 440 DEG C by sulfur heat fusing to liquid, and constant temperature 440 DEG C is stored in
In fluid reservoir；
Step 2: by 9kg particle diameter D50The CNT being about 0.5m joins synthesis device
In fluid bed；
Step 3: start gas compressor, compressed argon enters from fluidized-bed bottom, regulates gas
Flow velocity is about 0.1m/s, makes carbon nanotube dust be in fluidized state, and the temperature of argon is-
10℃；
Step 4: the liquid sulfur in fluid reservoir is delivered in atomization chamber and is passed through argon, sulfur and argon
The mass ratio 8:2 of gas, the aerodynamic atomization pressure of argon is 0.1MPa, by the liquid sulfur of atomization
With flow velocity in about 0.8m/s sprays into fluid bed, the distance of atomizer nozzle to fluid bed is
20m；Heater temperature is 440 DEG C；The atomizing particle size D of liquid sulfur50It is about 0.5 μm；
Prepare " sulfur/CNT " composite, the particle diameter D of sulfur ball in material50It is about
30m, " sulfur/carbon " mass ratio about 9:1.
Embodiment 4:
Step 1: under room temperature, joins the liquid sulfur supply system of synthesis device by 4kg Sublimed Sulfur
In.Be passed through argon, 180 DEG C by sulfur heat fusing to liquid, and constant temperature 180 DEG C is stored in
In fluid reservoir；
Step 2: by 16kg particle diameter D50The carbon fiber powder body being about 10m joins synthesis device
Fluid bed in；
Step 3: start gas compressor, compressed argon enters from fluidized-bed bottom, regulates gas
Flow velocity is about 0.5m/s, makes carbon fiber powder body be in fluidized state, and the temperature of argon is
0℃；
Step 4: the liquid sulfur in fluid reservoir is delivered in atomization chamber and is passed through argon, sulfur and argon
The mass ratio of gas is 4:6, and the aerodynamic atomization pressure of argon is 0.12MPa, by the liquid of atomization
Sulfur is with flow velocity in about 1m/s sprays into fluid bed；Heater temperature is 180 DEG C；Liquid sulfur
Atomizing particle size D50It is about 0.25 μm；
Preparing " sulfur/carbon fiber " composite, in material, the particle diameter of sulfur ball is about 28m, " sulfur
/ carbon " mass ratio about 1:4.
Embodiment 5:
Step 1: under room temperature, joins the liquid sulfur supply system of synthesis device by 9kg Sublimed Sulfur
In.Be passed through nitrogen, 150 DEG C by sulfur heat fusing to liquid, and constant temperature 150 DEG C is stored in
In fluid reservoir；
Step 2: by 6kg particle diameter D50The foamy carbon powder body of about 0.01m joins synthesis device
In fluid bed；
Step 3: start gas compressor, compressed nitrogen enters from fluidized-bed bottom, regulates gas
Flow velocity about 15m/s, makes foamy carbon powder body be in fluidized state, and the temperature of nitrogen is 25 DEG C；
Step 4: the liquid sulfur in fluid reservoir is delivered in atomization chamber and is passed through nitrogen, sulfur and nitrogen
The mass ratio of gas is 6:4, and the aerodynamic atomization pressure of nitrogen is 4MPa, by atomization liquid sulfur with
Flow velocity is in about 50m/s sprays into fluid bed, and the distance of atomizer nozzle to fluid bed is 5m；Add
Thermal temperature is 150 DEG C；The atomizing particle size D of liquid sulfur50It is about 0.03 μm；
Prepare " sulfur/foamy carbon " composite, the particle diameter D of sulfur ball in material50It is about
0.1m, " sulfur/carbon " mass ratio about 3:2.
Embodiment 6:
Step 1: under room temperature, settles 16kg sulfur and joins the liquid sulfur supply system of synthesis device
In.Be passed through argon, 300 DEG C by sulfur heat fusing to liquid, and constant temperature 300 DEG C is stored in
In fluid reservoir；
Step 2: by 24kg particle diameter D50The carbonaceous mesophase spherules powder body of about 2m joins synthesis
In the fluid bed of equipment；
Step 3: start gas compressor, compressed argon enters from fluidized-bed bottom, regulates gas
Flow velocity is about 2m/s, makes carbonaceous mesophase spherules powder body be in fluidized state, and the temperature of argon is
70℃；
Step 4: the liquid sulfur in fluid reservoir is delivered in atomization chamber and is passed through argon, uses gas
Streaming is atomized, and sulfur is 3:7 with the mass ratio of argon, and the aerodynamic atomization pressure of argon is
0.4MPa, by the liquid sulfur of atomization with flow velocity in about 5m/s sprays into fluid bed, atomizer nozzle
Distance to fluid bed is 10m；Heater temperature is 300 DEG C；The atomization grain of liquid sulfur
Footpath D50It is about 0.1 μm；
Prepare " sulfur/carbonaceous mesophase spherules " composite, the particle diameter D of sulfur ball in material50It is about
11m, " sulfur/carbon " mass ratio 2:3.
Embodiment 7:
Step 1: under room temperature, refines 8kg sulfur and joins the liquid sulfur supply system of synthesis device
In.Be passed through nitrogen, 160 DEG C by sulfur heat fusing to liquid, and constant temperature 160 DEG C is stored in
In fluid reservoir；
Step 2: by 2kg particle diameter D50The absorbent charcoal powder body of about 0.6m joins synthesis device
In fluid bed；
Step 3: start gas compressor, compressed nitrogen enters from fluidized-bed bottom, regulates gas
Flow velocity about 1m/s makes absorbent charcoal powder body be in fluidized state, and the temperature of nitrogen is 40 DEG C；
Step 4: the liquid sulfur in fluid reservoir is delivered in atomization chamber and is passed through nitrogen, sulfur and nitrogen
The mass ratio of gas is 8:2, and the aerodynamic atomization pressure of nitrogen is 0.3MPa, by the liquid sulfur of atomization
With flow velocity in about 4m/s sprays into fluid bed, the distance of atomizer nozzle to fluid bed is 10m；
Heater temperature is 160 DEG C；The atomizing particle size D of liquid sulfur50It is about 0.12 μm；
Prepare " sulfur/activated carbon " composite, the particle diameter D of sulfur ball in material50It is about
15m, " sulfur/carbon " mass ratio 4:1.
Although present disclosure is made by above-described embodiment and specifically being introduced, but above-described embodiment
Should not be considered as limitative to the invention.Therefore, protection scope of the present invention should be by institute
Attached claims limit.
Claims (8)
1. the preparation method of a sulfur carbon composite powder material, it is characterised in that: first make
Obtain liquid sulfur, liquid sulfur is atomized, contact with each other with the powder body material of the carbon of fluidisation, prepare
" sulfur/carbon " ratio and the regulatable composite powder material of particle diameter；Concretely comprise the following steps:
Step 1: the powder body material of carbon is placed in fluid bed, persistently leads to from fluidized-bed bottom
Entering gas, regulation gas flow rate makes carbon dust be in fluidized state；
Step 2: elemental sulfur is made liquid sulfur, keeps the temperature of liquid sulfur at 113-
440 DEG C, liquid sulfur is atomized, the liquid sulfur of atomization is sprayed into fluid bed, the liquid sulfur of atomization
Contact with each other with the powder body material of the carbon of fluidisation, prepare sulfur carbon composite powder material.
Preparation method the most according to claim 1, it is characterised in that: the list used
Matter sulfur is 1:9 9:1 with the mass ratio of the powder body material of carbon；The particle diameter D of the powder body material of carbon50
For 0.01-10 μm；.
Preparation method the most according to claim 1, it is characterised in that: described simple substance
Sulfur is the one in refined sulfur, Sublimed Sulfur or sedimentation sulfur or two kinds or three kinds；Described carbon
Powder body material is hard carbon or soft carbon or the one of graphite or two kinds or three kinds, the powder body material of carbon
Pattern be graininess, spherical, fibrous, tubulose, lamellar or the one of cystose or two
More than Zhong.
Preparation method the most according to claim 1, it is characterised in that: in step 1, institute
Being the one in nitrogen or argon or two kinds with gas, the temperature of gas is-30-100 DEG C；Gas
Rate of flow of fluid is 0.1m/s-120m/s.
Preparation method the most according to claim 1, it is characterised in that: use heat fusing
Elemental sulfur is made liquid sulfur by method, and the heating-up temperature of heat fusing is 113-440 DEG C, at nitrogen or
Argon gas atmosphere is carried out.
Preparation method the most according to claim 1 or 5, it is characterised in that: step 2
In, atomizing gas is one or both in nitrogen or argon；The liquid sulfur of atomization and mist
Mass ratio between activating QI body is 1:20-100:1；The aerodynamic atomization pressure of atomization gas is 0.1-
10MPa；The particle diameter D of the liquid sulfur of atomization50For 0.01-30 μm；The nozzle of nebulizer and stream
The distance changing bed is 1-20m, and the speed that the liquid sulfur of atomization sprays from atomizer nozzle is
0.1-120m/s。
7. the sulfur carbon composite powder material that the described method according to claim 1-6 prepares
Material, it is characterised in that: in carbon sulfur composite powder material, sulfur is 1:9 with the mass ratio of carbon
9:1, the particle diameter D of solid sulfur in material50For 0.02-30 μm.
8. lithium sulfur secondary electricity prepared by the sulfur carbon composite powder material described in a claim 7
Application in the positive electrode in pond.
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| CN106848252A (en) * | 2017-03-16 | 2017-06-13 | 成都新柯力化工科技有限公司 | One kind evaporation aluminum fluoride improves the durothermic method of ternary anode material of lithium battery |
| WO2021048815A1 (en) * | 2019-09-12 | 2021-03-18 | Fondazione Istituto Italiano Di Tecnologia | Process for the production of a sulfur-carbon composite material, composite material thus obtained and electrode for lithium-sulfur batteries produced with the material |
| CN114784261A (en) * | 2022-06-21 | 2022-07-22 | 宜宾锂宝新材料有限公司 | Lithium battery positive electrode material and preparation method thereof |
| EP4142928A4 (en) * | 2019-06-28 | 2023-05-24 | Ejoule, Inc. | System and process with assisted gas flow inside a reaction chamber |
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| US11376559B2 (en) * | 2019-06-28 | 2022-07-05 | eJoule, Inc. | Processing system and method for producing a particulate material |
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| CN105990569B (en) | 2018-10-30 |
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