CN106784760B - A kind of preparation method of nitrogen-doped graphene/zinc hydroxide/hollow sulphur composite material - Google Patents
A kind of preparation method of nitrogen-doped graphene/zinc hydroxide/hollow sulphur composite material Download PDFInfo
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- CN106784760B CN106784760B CN201710218778.3A CN201710218778A CN106784760B CN 106784760 B CN106784760 B CN 106784760B CN 201710218778 A CN201710218778 A CN 201710218778A CN 106784760 B CN106784760 B CN 106784760B
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Abstract
The present invention provides a kind of preparation method of nitrogen-doped graphene/zinc hydroxide/hollow sulphur composite material, comprises the following steps: sulphur powder is added to stirring and dissolving in carbon disulfide and forms uniform solution by step (1)；High-purity nickel powder is passed through high energy ball mill ball milling by step (2), is added in above-mentioned solution after ball milling, and stirring forms uniform suspension, and mechanical stirring forms the spheric granules of sulphur cladding after spray drying；Spheric granules is added in ferric chloride solution by step (3), is stirred to react, and is washed, is filtered；Filtered sediment is added in the solution of Containing Zinc Chloride, urea and surfactant by step (4), stirs into uniform suspension, heating stirring reaction, and centrifugation, washing obtain the sulfur granules of zinc hydroxide cladding.Hollow structure is designed as volume expansion reserved space of the sulfur materials in charge and discharge process in the composite material, can effectively improve chemical property.
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 nitrogen-doped graphene/zinc hydroxide/hollow sulphur composite material,
The composite material is made of the graphene network of the sulphur of hollow structure, the zinc hydroxide material of sulphur external sheath and N doping, is led
Electrically good to provide conductive network in outer layer graphene, the sulfenyl material of hollow structure provides the space of expansion, sulphur outer layer packet
The zinc hydroxide covered can adsorb the dissolution of discharging product polysulfide, improve the chemical property of material.
The preparation process flow that the present invention provides a kind of nitrogen-doped graphene/zinc hydroxide/hollow sulphur composite material is as follows:
(1) sulphur powder is added to stirring and dissolving in carbon disulfide and forms uniform solution；
(2) high-purity nickel powder is passed through into high energy ball mill ball milling, is added in above-mentioned solution after ball milling, stirring forms uniform
Suspension, mechanical stirring, after spray drying formed sulphur cladding spheric granules；
(3) spheric granules is added in ferric chloride solution, is stirred to react, washed, filter.
(4) filtered sediment is added in the solution of Containing Zinc Chloride, urea and surfactant, is stirred into uniform
Suspension, heating stirring reaction, centrifugation, washing obtain the sulfur granules of zinc hydroxide cladding；
(5) by nitrogen-doped graphene be added to the water ultrasonic disperse formed unit for uniform suspension, then by zinc hydroxide cladding
Sulfur granules are added, and stir, and filter, obtain composite material after washing.
The carbon disulfide solution concentration of sulphur is 1-5g/mL in step (1);
Nickel powder in step (2): the mass ratio of sulphur powder is 0.05-0.2:1, and Ball-milling Time is 0.5-2 hours, when mechanical stirring
Between be 0.5-1 hours;
The concentration of ferric chloride solution is 1-2mol/L in step (3), and being stirred to react the time is 1-5 hours；
Zinc chloride in step (4): urea: surfactant: the mass ratio of sulphur is 1-2:1-1.5:0.1-0.2:10, heating
The temperature of reaction are as follows: 60-90 DEG C, the reaction time is 30-60 minutes, and surfactant can be neopelex, two
One or more of octyl sodium sulfosuccinate, sodium stearyl sulfate;
In step (5) concentration of nitrogen-doped graphene suspension be 0.5-2g/L, nitrogen-doped graphene nitrogen-doped graphene:
The mass ratio of sulphur is 1-2:10, and the reaction time being stirred to react is 5-30 minutes.
The invention has the following beneficial effects: the conductivity that (1) nitrogen-doped graphene has superelevation, are prepared by this method
Nitrogen-doped graphene/zinc hydroxide out/hollow sulphur composite material can effectively improve the electronics of lithium sulfur battery anode material
Conductivity and ionic conductivity, while the nitrogen on graphene can carry out chemisorption to polysulfide, reduce sulphur when charge and discharge
Loss；(2) cladding of zinc hydroxide can carry out physical protection to sulfenyl material in the composite material, while zinc hydroxide also can be right
Polysulfide carries out chemisorption, reduces shuttle effect；(3) hollow structure is designed as sulfur materials in charge and discharge in the composite material
Volume expansion reserved space in electric process, can effectively improve chemical property.
Detailed description of the invention
Fig. 1 is process flow chart of the 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) 100g sulphur powder is added to the solution that stirring and dissolving in carbon disulfide forms 1g/mL；
(2) 5g high-purity nickel powder is passed through into high energy ball mill, ball milling 0.5 hour, is added in above-mentioned solution, stirs after ball milling
It mixes to form uniform suspension, mechanical stirring 0.5 hour, forms the spheric granules of sulphur cladding after spray drying；
(3) spheric granules is added in 1mol/L ferric chloride solution, is stirred to react 5 hours, washing, filtering.
(4) filtered sediment is added to the molten of zinc chloride containing 10g, 10g urea and 1g neopelex
In liquid, uniform suspension is stirred into, 60 DEG C is heated to and is stirred to react 60 minutes, centrifugation, washing obtain the sulphur of zinc hydroxide cladding
Particle；
(5) by 10g nitrogen-doped graphene be added to the water ultrasonic disperse formed uniform concentration be 0.5g/L suspension, then
The sulfur granules of zinc hydroxide cladding are added, are stirred, filters, obtains composite material after washing.
Embodiment 2
(1) 100g sulphur powder is added to the solution that stirring and dissolving in carbon disulfide forms 5g/mL；
(2) 20g high-purity nickel powder is passed through into high energy ball mill, ball milling 2 hours, is added in above-mentioned solution, stirs after ball milling
It mixes to form uniform suspension, mechanical stirring 1 hour, forms the spheric granules of sulphur cladding after spray drying；
(3) spheric granules is added in 2mol/L ferric chloride solution, is stirred to react 1 hour, washing, filtering.
(4) filtered sediment is added to zinc chloride containing 20g, 15g urea and 2g dioctyl succinate disulfonate acid
In solution, uniform suspension is stirred into, 90 DEG C is heated to and is stirred to react 30 minutes, centrifugation, washing obtain zinc hydroxide cladding
Sulfur granules；
(5) by 20g nitrogen-doped graphene be added to the water ultrasonic disperse formed uniform concentration be 2g/L suspension, then will
The sulfur granules of zinc hydroxide cladding are added, and stir, and filter, obtain composite material after washing.
Embodiment 3
(1) 100g sulphur powder is added to the solution that stirring and dissolving in carbon disulfide forms 2g/mL；
(2) 10g high-purity nickel powder is passed through into high energy ball mill, ball milling 1 hour, is added in above-mentioned solution, stirs after ball milling
It mixes to form uniform suspension, mechanical stirring 0.6 hour, forms the spheric granules of sulphur cladding after spray drying；
(3) spheric granules is added in 1.5mol/L ferric chloride solution, is stirred to react 3 hours, washing, filtering.
(4) filtered sediment is added to the molten of zinc chloride containing 15g, 12g urea and 1.5g sodium stearyl sulfate
In liquid, uniform suspension is stirred into, 70 DEG C is heated to and is stirred to react 45 minutes, centrifugation, washing obtain the sulphur of zinc hydroxide cladding
Particle；
(5) by 15g nitrogen-doped graphene be added to the water ultrasonic disperse formed uniform concentration be 1g/L suspension, then will
The sulfur granules of zinc hydroxide cladding are added, and stir, and filter, obtain composite material after washing.
Embodiment 4
(1) 100g sulphur powder is added to the solution that stirring and dissolving in carbon disulfide forms 3g/mL；
(2) 15g high-purity nickel powder is passed through into high energy ball mill, ball milling 1.5 hours, is added to after ball milling in above-mentioned solution,
Stirring forms uniform suspension, and mechanical stirring 0.7 hour, the spheric granules of sulphur cladding is formed after spray drying；
(3) spheric granules is added in 1.2mol/L ferric chloride solution, is stirred to react 4 hours, washing, filtering.
(4) that filtered sediment is added to zinc chloride containing 12g, 11g urea and 1.2g neopelex is molten
In liquid, uniform suspension is stirred into, 80 DEG C is heated to and is stirred to react 40 minutes, centrifugation, washing obtain the sulphur of zinc hydroxide cladding
Particle；
(5) by 12g nitrogen-doped graphene be added to the water ultrasonic disperse formed uniform concentration be 1.5g/L suspension, then
The sulfur granules of zinc hydroxide cladding are added, are stirred, filters, obtains composite material after washing.
Embodiment 5
(1) 100g sulphur powder is added to the solution that stirring and dissolving in carbon disulfide forms 4g/mL；
(2) 18g high-purity nickel powder is passed through into high energy ball mill, ball milling 1.6 hours, is added to after ball milling in above-mentioned solution,
Stirring forms uniform suspension, and mechanical stirring 0.8 hour, the spheric granules of sulphur cladding is formed after spray drying；
(3) spheric granules is added in 1.8mol/L ferric chloride solution, is stirred to react 2 hours, washing, filtering.
(4) filtered sediment is added to zinc chloride containing 18g, 14g urea and 1.8g dioctyl succinate disulfonate acid
Solution in, stir into uniform suspension, be heated to 75 DEG C and be stirred to react 55 minutes, centrifugation, washing obtain zinc hydroxide cladding
Sulfur granules；
(5) by 18g nitrogen-doped graphene be added to the water ultrasonic disperse formed uniform concentration be 1.8g/L suspension, then
The sulfur granules of zinc hydroxide cladding are added, are stirred, filters, obtains composite material after washing.
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) | 950 | 970 | 940 | 950 | 930 |
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 950 mAh/g, and efficiency for charge-discharge 81% fills for the second time
Discharge capacity is 1060 mAh/g, after 200 charge and discharge cycles, capacity relative to second of discharge capacity still possess 82% with
On, illustrate that the structure of the composite material can effectively inhibit shuttle effect, improves the service life of sulphur battery.
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, exist
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 (6)
1. a kind of nitrogen-doped graphene/zinc hydroxide/hollow sulphur composite material preparation process, which is characterized in that including as follows
Several steps:
Sulphur powder is added to stirring and dissolving in carbon disulfide and forms uniform solution by step (1)；
High-purity nickel powder is passed through high energy ball mill ball milling by step (2), is added in above-mentioned solution after ball milling, and stirring forms uniform
Suspension, mechanical stirring, after spray drying formed sulphur cladding spheric granules；
Spheric granules is added in ferric chloride solution by step (3), is stirred to react, and is washed, is filtered；
Filtered sediment is added in the solution of Containing Zinc Chloride, urea and surfactant by step (4), is stirred into uniform
Suspension, heating stirring reaction, centrifugation, washing obtain the sulfur granules of zinc hydroxide cladding；
Step (5) by nitrogen-doped graphene be added to the water ultrasonic disperse formed unit for uniform suspension, then by zinc hydroxide cladding
Sulfur granules are added, and stir, and filter, obtain composite material after washing.
2. preparation process as described in claim 1, which is characterized in that the carbon disulfide solution concentration of sulphur is 1- in step (1)
5g/mL。
3. preparation process as described in claim 1, which is characterized in that nickel powder in step (2): the mass ratio of sulphur powder is 0.05-
0.2:1, Ball-milling Time are 0.5-2 hours, and the mechanical stirring time is 0.5-1 hours.
4. preparation process as described in claim 1, which is characterized in that the concentration of ferric chloride solution is 1-2mol/ in step (3)
L, being stirred to react the time is 1-5 hours.
5. preparation process as described in claim 1, which is characterized in that zinc chloride in step (4): urea: surfactant: sulphur
Mass ratio be 1-2:1-1.5:0.1-0.2:10, heat the temperature of reaction are as follows: 60-90 DEG C, the reaction time be 30-60 minutes,
Surfactant can for one of neopelex, dioctyl succinate disulfonate acid, sodium stearyl sulfate or
Person is a variety of.
6. preparation process as described in claim 1, which is characterized in that the concentration of nitrogen-doped graphene suspension in step (5)
For 0.5-2g/L, nitrogen-doped graphene nitrogen-doped graphene: the mass ratio of sulphur is 1-2:10, and the reaction time being stirred to react is 5-
30 minutes.
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