CN109065867A - Molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material preparation method - Google Patents
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention discloses a kind of molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material preparation method, for solving the technical problem of the negative electrode material of existing method preparation forthright difference again.Technical solution is to be dissolved in molybdenum source in the deionized water containing concentrated nitric acid carrying out hydro-thermal reaction, obtains molybdenum trioxide nano-wire presoma.It disperses molybdenum trioxide in deionized water, acid for adjusting pH is added, add molybdenum trioxide/sulphur source/pyrrole monomer dissolution, hydro-thermal reaction obtains molybdenum disulfide/polypyrrole nano line.Molybdenum disulfide/polypyrrole nano line is laid in porcelain boat, and porcelain boat is placed in tube furnace, after heating up and keeping the temperature under an inert atmosphere, is cooled to room temperature, molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material is obtained.After tested, when current density is 4A g‑1When, specific capacity by background technique 350mAh g‑1It is increased to 506~600mAh g‑1, show the multiplying power property of superelevation.
Description
Technical field
The present invention relates to a kind of preparation method of negative electrode material, in particular to a kind of molybdenum disulfide/nitrogen-doped carbon nano wire
The preparation method of negative electrode material.
Background technique
With electric vehicle and can portable electronic device fast development, have that operating voltage is high, energy density is big, the circulation longevity
The lithium ion battery that life grows the advantages such as low with self-discharge rate is concerned.Negative electrode material is the important of decision performance of lithium ion battery
One of factor.The advantages that commercialized graphite material is although conductive good, platform point is low and stable circulation is good at present, but
Lower (the 372mAh g of its theoretical specific capacity-1), therefore, seeks and develop alternative high performance lithium ionic cell cathode material
As current research hotspot.
It is that sulphur atom and molybdenum atom pass through covalently as a kind of typical stratiform transient metal sulfide, in layer of molybdenum-disulfide
The sandwich structure that key is constituted, is combined by Van der Waals force between layers, and unique layer structure is conducive to the biography of ion
It is defeated.In addition, molybdenum disulfide reversible capacity can achieve 900mAh g-1, therefore be considered as a kind of negative electrode material of great potential.
But molybdenum disulfide, there are still electron conduction difference and volume expansion two large problems, which prevent it in lithium ion battery
Practical application.Currently, researcher mainly passes through molybdenum disulfide nano and by molybdenum disulfide and high conductivity material compound two
Kind approach solves problem above, and a lot of research work shows that the molybdenum disulfide negative electrode material for introducing high conductivity material can be greatly
It improves molybdenum disulfide and stores up lithium performance in ground.But under high current density, most of molybdenum disulfide negative electrode materials cannot be real well
Existing fast charging and discharging, leads to poor high rate performance.
Document " Chinese invention patent that application publication number is CN106229499A " discloses a kind of molybdenum disulfide/polyaniline
The preparation method of negative electrode material.The polyaniline for being dispersed with molybdenum salt and sulphur source hydro-thermal are obtained molybdenum disulfide/polyaniline and born by this method
Pole material, improves the ion and electron conduction of molybdenum disulfide, and performance of lithium ion battery increases.However, it was found that the polyphenyl
Amine is unsatisfactory to molybdenum disulfide electric conductivity and volume change improvement, when current density is 4A g-1When, specific capacity only has
350mAh g-1, show poor high rate performance.
Summary of the invention
Negative electrode material in order to overcome the shortcomings of existing method preparation is forthright poor again, the present invention provide a kind of molybdenum disulfide/
The preparation method of nitrogen-doped carbon nano wire negative electrode material.This method by molybdenum source be dissolved in the deionized water containing concentrated nitric acid carry out water
Thermal response obtains molybdenum trioxide nano-wire presoma.It disperses molybdenum trioxide in deionized water, addition acid for adjusting pH, then plus
Enter molybdenum trioxide/sulphur source/pyrrole monomer dissolution, hydro-thermal reaction obtains molybdenum disulfide/polypyrrole nano line.By molybdenum disulfide/poly-
Pyrroles's nano wire is laid in porcelain boat, and porcelain boat is placed in tube furnace, after heating up and keeping the temperature under an inert atmosphere, is cooled to
Room temperature obtains molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material.After tested, when current density is 4A g-1When, specific capacity
By the 350mAh g of background technique-1It is increased to 506~600mAh g-1, show the multiplying power property of superelevation.
A kind of the technical solution adopted by the present invention to solve the technical problems: molybdenum disulfide/nitrogen-doped carbon nano wire cathode
The preparation method of material, its main feature is that the following steps are included:
Step 1: molybdenum source is dissolved in the deionized water containing 0.1~3.0mol/L concentrated nitric acid, hydro-thermal at 160~240 DEG C
6~36h is reacted, molybdenum trioxide nano-wire presoma is obtained.
Step 2: dispersing molybdenum trioxide nano-wire presoma in deionized water, acid is added, adjusting pH is 0.1~5,
Adding molar ratio is 1:(4~6): the molybdenum trioxide/sulphur source/pyrrole monomer of (0.207~0.615) sufficiently dissolves, 160~
240 DEG C of 6~36h of hydro-thermal reaction obtain molybdenum disulfide/polypyrrole nano line.Step 3: molybdenum disulfide/polypyrrole nano line is put down
It is laid in porcelain boat, and porcelain boat is placed in tube furnace, rise to 600 under an inert atmosphere with 0.5~20 DEG C/min heating rate
~1000 DEG C, 0.5~10h is kept the temperature, is cooled to room temperature, obtains molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material.
The molybdenum source is any of ammonium molybdate or sodium molybdate.
The sulphur source is any of thiocarbamide, L-cysteine or thioacetamide.
The acid is any of sulfuric acid, hydrochloric acid, acetic acid or nitric acid.
The inert atmosphere selects any of nitrogen or argon gas.
The beneficial effects of the present invention are: this method by molybdenum source be dissolved in the deionized water containing concentrated nitric acid carry out hydro-thermal it is anti-
It answers, obtains molybdenum trioxide nano-wire presoma.It disperses molybdenum trioxide in deionized water, acid for adjusting pH is added, adds three
Molybdenum oxide/sulphur source/pyrrole monomer dissolution, hydro-thermal reaction obtain molybdenum disulfide/polypyrrole nano line.By molybdenum disulfide/polypyrrole
Nano wire is laid in porcelain boat, and porcelain boat is placed in tube furnace, after heating up and keeping the temperature under an inert atmosphere, is cooled to room
Temperature obtains molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material.After tested, when current density is 4A g-1When, specific capacity by
The 350mAh g of background technique-1It is increased to 506~600mAh g-1, show the multiplying power property of superelevation.
It elaborates with reference to the accompanying drawings and detailed description to the present invention.
Detailed description of the invention
Fig. 1 is molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material scanning electron prepared by embodiment of the present invention method 1
MIcrosope image.
Fig. 2 is that molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material high-resolution prepared by embodiment of the present invention method 1 is saturating
Penetrate electron microscope image.
Fig. 3 is that molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material X-ray prepared by embodiment of the present invention method 1 is spread out
Penetrate map.
Fig. 4 is molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material of the preparation of embodiment of the present invention method 1 in 100mAg-1
Under the conditions of cycle performance test chart.
Fig. 5 is molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material high rate performance prepared by embodiment of the present invention method 1
Test chart.
Specific embodiment
Following embodiment referring to Fig.1-5.
Embodiment 1:
Nitric acid and deionized water mixed solution is added in the ammonium molybdate for weighing 0.5g, and wherein the concentration of nitric acid is 2.6mol/L,
Sufficiently dissolution, is transferred in 50ml water heating kettle, is placed in convection oven hydro-thermal 20h at 200 DEG C.Cooled to room temperature to be reacted
Afterwards, obtained white precipitate filtered, washed, dried, obtain MoO3Nano wire.Weigh the MoO of 0.1g3Nano wire dispersion
In 30ml deionized water, appropriate hydrochloric acid is added, adjusts dispersion liquid pH to 0.23, adds 100 μ l pyrrole monomers and 200mg sulphur
Urea sufficiently dissolves, is transferred in 40ml autoclave and reacts 12h at 200 DEG C.After reacting cooled to room temperature, will
To black precipitate filtered, washed, dried, obtain molybdenum disulfide/polypyrrole nano line.Molybdenum disulfide/polypyrrole is received
Rice noodles are placed in porcelain boat, and porcelain boat is placed in position among tube furnace, are risen in a nitrogen atmosphere with the rate of 5 DEG C/min
800 DEG C, 2h is kept the temperature, black powder is obtained after being cooled to room temperature, i.e. molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material.
Gained molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material, conductive carbon black and PVDF is matched with mass ratio for 7:2:1
It is cathode that slurrying material, which is coated on copper foil as positive, lithium piece, ethylene carbonate/dimethyl carbonate/ethyl carbonate is electrolyte, poly-
Propylene is diaphragm, is assembled into half-cell.When current density is 4A g-1When, specific capacity is up to 600mAh g-1, work as current density
Rise to 10A g-1When, specific capacity is up to 453mAh g-1, the multiplying power property of superelevation is shown, and in 100mA g-1Current density
Under, its specific capacity is up to 821mAh g after 100 circle of circulation-1, show excellent cyclical stability.
It can be seen from figure 1, molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material pattern is uniform, and length is 10-15 μm,
Diameter is 300-500nm, and surface is uniformly distributed nanometer sheet.
The molybdenum disulfide number of plies is 1-5 layers as can be seen from Figure 2, and interlamellar spacing is greater than 0.9nm.
From figure 3, it can be seen that the diffraction maximum positioned at 33.2 ° and 56.7 ° can belong to MoS2(100) and (110) crystal face,
Interlamellar spacing, which is corresponded respectively to, positioned at the diffraction maximum of 8.6 ° (*) and 17.2 ° (* *) expands front and back MoS2(002) diffraction maximum of crystal face,
In addition, showing that the material is pure MoS without the appearance of other miscellaneous peaks2Phase.
From fig. 4, it can be seen that molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material 100mA g-1Under the conditions of, for the first time may be used
Inverse capacity can reach 744mAh g-1, after circulation 100 is enclosed, capacity is up to 821mAh g-1, show excellent stable circulation
Property.
From fig. 5, it can be seen that when current density is 4A g-1When, specific capacity is up to 600mAh g-1；10A g-1When,
Specific capacity is up to 453mAh g-1；Show the multiplying power property of superelevation.
Embodiment 2:
It weighs 0.5g ammonium molybdate and nitric acid and deionized water mixed solution is added, wherein the concentration of nitric acid is 0.1mol/L, is filled
Divide dissolution, is transferred in 50ml water heating kettle, is placed in convection oven hydro-thermal 36h at 160 DEG C.After reacting cooled to room temperature,
Obtained white precipitate is filtered, washed, is dried, MoO is obtained3Nano wire.Weigh the MoO of 0.1g3Nano wire is scattered in
In 30ml deionized water, moderate amount of sulfuric acid is added, adjusts dispersion liquid pH to 0.2, adds the L- of 100 μ l pyrrole monomers and 314mg
Cysteine sufficiently dissolves, is transferred in 40ml autoclave and reacts 6h at 240 DEG C.After reacting cooled to room temperature,
Obtained black precipitate is filtered, washed, is dried, molybdenum disulfide/polypyrrole nano line is obtained.By molybdenum disulfide/poly- pyrrole
It coughs up nano wire to be placed in porcelain boat, and porcelain boat is placed in position among tube furnace, in a nitrogen atmosphere with the rate liter of 0.5 DEG C/min
Temperature rise keeps the temperature 10h, black powder is obtained after being cooled to room temperature, i.e. molybdenum disulfide/nitrogen-doped carbon nano wire cathode material to 600 DEG C
Material.
Gained molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material, conductive carbon black and PVDF is matched with mass ratio for 7:2:1
It is cathode that slurrying material, which is coated on copper foil as positive, lithium piece, ethylene carbonate/dimethyl carbonate/ethyl carbonate is electrolyte, poly-
Propylene is diaphragm, is assembled into half-cell.When current density is 4A g-1When, specific capacity is 540mAh g-1, when current density liter
To 10A g-1When, specific capacity is 375mAh g-1, and in 100mA g-1Under current density, its specific capacity is after 100 circle of circulation
780mAh g-1。
Embodiment 3:
It weighs 0.5g sodium molybdate and nitric acid and deionized water mixed solution is added, wherein the concentration of nitric acid is 3.0mol/L, is filled
Divide dissolution, is transferred in 50ml water heating kettle, is placed in convection oven hydro-thermal 8h at 240 DEG C.It, will after reacting cooled to room temperature
Obtained white precipitate is filtered, is washed, is dried, and MoO is obtained3Nano wire.Weigh the MoO of 0.1g3Nano wire is scattered in 30ml
In deionized water, appropriate nitric acid is added, adjusts dispersion liquid pH to 5, adds the thioacetyl of 300 μ l pyrrole monomers and 197mg
Amine sufficiently dissolves, is transferred in 40ml autoclave and reacts 36h at 160 DEG C.After reacting cooled to room temperature, will
To black precipitate filtered, washed, dried, obtain molybdenum disulfide/polypyrrole nano line.Molybdenum disulfide/polypyrrole is received
Rice noodles are placed in porcelain boat, and porcelain boat is placed in position among tube furnace, are heated up rise with the rate of 20 DEG C/min under an argon atmosphere
To 1000 DEG C, 0.5h is kept the temperature, black powder is obtained after being cooled to room temperature, i.e. molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material.
Gained molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material, conductive carbon black and PVDF is matched with mass ratio for 7:2:1
It is cathode that slurrying material, which is coated on copper foil as positive, lithium piece, ethylene carbonate/dimethyl carbonate/ethyl carbonate is electrolyte, poly-
Propylene is diaphragm, is assembled into half-cell.When current density is 4A g-1When, specific capacity is 506mAh g-1, when current density liter
To 10A g-1When, reachable specific capacity is 386mAh g-1, and in 100mA g-1Under current density, its specific volume after 100 circle of circulation
Amount is 768mAh g-1。
Embodiment 4:
It weighs 0.5g Ammonium Molybdate Tetrahydrate and nitric acid and deionized water mixed solution is added, wherein the concentration of nitric acid is
2.6mol/L sufficiently dissolves, is transferred in 50ml water heating kettle, is placed in convection oven hydro-thermal 6h at 200 DEG C.Natural cooling to be reacted
To room temperature, obtained white precipitate is filtered, washed, is dried, MoO is obtained3Nano wire.Weigh the MoO of 0.1g3Nanometer
Line is scattered in 30ml deionized water, be added proper amount of acetic acid, adjust dispersion liquid pH to 0.1, add 100 μ l pyrrole monomers and
300mg thiocarbamide sufficiently dissolves, is transferred in 40ml autoclave and reacts 12h at 200 DEG C.Cooled to room temperature to be reacted
Afterwards, obtained black precipitate filtered, washed, dried, obtain molybdenum disulfide/polypyrrole nano line.By molybdenum disulfide/poly-
Pyrroles's nano wire is placed in porcelain boat, and porcelain boat is placed in position among tube furnace, under an argon atmosphere with the rate liter of 5 DEG C/min
Temperature rise keeps the temperature 2h, black powder is obtained after being cooled to room temperature, i.e. molybdenum disulfide/nitrogen-doped carbon nano wire cathode material to 600 DEG C
Material.
Gained molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material, conductive carbon black and PVDF is matched with mass ratio for 7:2:1
It is cathode that slurrying material, which is coated on copper foil as positive, lithium piece, ethylene carbonate/dimethyl carbonate/ethyl carbonate is electrolyte, poly-
Propylene is diaphragm, is assembled into half-cell.When current density is 4A g-1When, specific capacity is 522mAh g-1, when current density liter
To 10A g-1When, specific capacity is 392mAh g-1, and in 100mA g-1Under current density, its specific capacity is after 100 circle of circulation
774mAh g-1。
Claims (5)
1. a kind of molybdenum disulfide/nitrogen-doped carbon nano wire negative electrode material preparation method, it is characterised in that the following steps are included:
Step 1: molybdenum source is dissolved in the deionized water containing 0.1~3.0mol/L concentrated nitric acid, hydro-thermal reaction at 160~240 DEG C
6~36h obtains molybdenum trioxide nano-wire presoma；
Step 2: dispersing molybdenum trioxide nano-wire presoma in deionized water, acid is added, adjusting pH is 0.1~5, then plus
Entering molar ratio is 1:(4~6): the molybdenum trioxide/sulphur source/pyrrole monomer of (0.207~0.615) sufficiently dissolves, 160~240 DEG C
6~36h of hydro-thermal reaction obtains molybdenum disulfide/polypyrrole nano line；
Step 3: molybdenum disulfide/polypyrrole nano line is laid in porcelain boat, and porcelain boat is placed in tube furnace, in inertia
600~1000 DEG C are risen to 0.5~20 DEG C/min heating rate under atmosphere, 0.5~10h is kept the temperature, is cooled to room temperature, obtains two sulphur
Change molybdenum/nitrogen-doped carbon nano wire negative electrode material.
2. molybdenum disulfide according to claim 1/nitrogen-doped carbon nano wire negative electrode material preparation method, feature exist
In: the molybdenum source be any of ammonium molybdate or sodium molybdate.
3. molybdenum disulfide according to claim 1/nitrogen-doped carbon nano wire negative electrode material preparation method, feature exist
In: the sulphur source is any of thiocarbamide, L-cysteine or thioacetamide.
4. molybdenum disulfide according to claim 1/nitrogen-doped carbon nano wire negative electrode material preparation method, feature exist
In: the acid is any of sulfuric acid, hydrochloric acid, acetic acid or nitric acid.
5. molybdenum disulfide according to claim 1/nitrogen-doped carbon nano wire negative electrode material preparation method, feature exist
Any of nitrogen or argon gas is selected in: the inert atmosphere.
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| CN112063365A (en) * | 2020-09-04 | 2020-12-11 | 山东大学 | Molybdenum disulfide nitrogen composite porous carbon material and preparation method and application thereof |
| CN112063365B (en) * | 2020-09-04 | 2021-06-01 | 山东大学 | Molybdenum disulfide nitrogen composite porous carbon material and preparation method and application thereof |
| CN113816425A (en) * | 2021-09-16 | 2021-12-21 | 陕西科技大学 | MoS2Nitrogen-doped carbon/modified activated carbon sodium ion battery negative electrode material and preparation method thereof |
| CN113816425B (en) * | 2021-09-16 | 2022-08-09 | 陕西科技大学 | MoS 2 Nitrogen-doped carbon/modified activated carbon sodium ion battery negative electrode material and preparation method thereof |
| CN114050241A (en) * | 2021-11-10 | 2022-02-15 | 南京大学 | Molybdenum disulfide @ carbon-based nanocage composite material with threshold-limiting structure and preparation method and application thereof |
| CN114512665A (en) * | 2022-01-28 | 2022-05-17 | 上海华起睿智新能源科技有限公司 | Preparation method of metal ion doped sodium ion battery negative electrode material |
| CN114512665B (en) * | 2022-01-28 | 2024-02-27 | 上海华起睿智新能源科技有限公司 | Preparation method of metal ion doped sodium ion battery negative plate |
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