CN109286009A - A kind of preparation method of nanometer sheet self assembled three-dimensional nano flower artificial gold/graphitization carbonitride lithium ion battery negative material - Google Patents
A kind of preparation method of nanometer sheet self assembled three-dimensional nano flower artificial gold/graphitization carbonitride lithium ion battery negative material Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of nanometer sheet self assembled three-dimensional nano flower artificial gold/graphitization carbonitride lithium ion battery negative material, melamine is kept the temperature into 2~6h under the conditions of 450-650 DEG C, when it naturally cools to room temperature, it grinds spare, it is then dispersed in ethyl alcohol and obtains suspension, suspension is centrifuged and is washed several times with deionized water and dehydrated alcohol, then vacuum drying obtains product g-C3N4, by product g-C3N4It is dissolved in deionized water, ultrasonic disperse after stirring, forms suspending liquid A, PVP is added into suspending liquid A, stirring is until be completely dissolved to form solution B, by TAA and SnCl4·2H2O is added in solution B, stirs evenly to form solution C, and solution C is carried out microwave hydrothermal reaction, after reaction, presoma is obtained, presoma is distinguished into centrifuge washing several times through deionized water and dehydrated alcohol, then vacuum drying obtains nanometer sheet self assembled three-dimensional nano flower SnS2/g‑C3N4Battery material.
Description
Technical field
The present invention relates to a kind of preparation methods of lithium ion battery negative material, and in particular to a kind of nanometer sheet self assembly three
Wiener popped rice artificial gold/graphitization carbonitride lithium ion battery negative material preparation method.
Background technique
Lithium ion battery relies primarily on the deintercalation of lithium ion between a positive electrode and a negative electrode as a kind of rechargeable secondary cell
To work.In addition, it has, operating voltage is high, have extended cycle life, specific capacity is big, have a safety feature, self discharge is small, without note
Recall the advantages such as effect.This advantage makes it be widely used in the portable devices such as mobile phone, camera, laptop.Closely
Several years by lithium ion battery charge/discharge capacity, multiplying power property, in terms of continuous development and improvement, new
The use in the fields such as energy automobile, electric tool, aerospace and energy storage is gradually expanded.It can be seen that lithium ion battery can
Main way as the development of the following secondary cell.And lithium ion battery negative material is the important composition portion of lithium ion battery
Point, the Nomenclature Composition and Structure of Complexes of negative electrode material has decisive impact the chemical property of lithium ion battery.Therefore, this makes me
To research and develop suitable battery material as emphasis.
SnS2It is the binary compound for belonging to IV:VI main group, by hexagonal phase basic unit CdI2Layered crystal structure (structure cell
Parameter: a=0.3648nm, c=0.5899nm) composition, this structural unit among the sulphion of two layers of hexagonal closs packing by adding
Enter sandwich structure (S-Sn-S) composition of tin ion.Every six sulphions are inserted into a tin ion formation regular octahedron and match
Position, and there is weak Van der Waals force between layers and pass through Covalent bonding together.In addition, there are many crystalline substances for this layer structure
Body vacancy can be used as the host lattice of intercalation.This unique layer structure makes it have excellent photoelectric characteristic.Currently, grinding
The persons of studying carefully prepare the SnS of different structure or size by different methods2, main structure have stannic disulfide nanoparticle,
The zero dimensions such as nanosphere, nanometer sheet, nanotube, nano-plates, one-dimensional and two-dimentional or 3-D nano, structure, or even there are also more multiple
Miscellaneous multistage micro nano structure.People prepare semiconductor material, light using the special performance that these different structures possess
Catalysis material, solar cell material, photo-translating system material and lithium ion battery material etc..Unique performance and extensively
Application so that SnS2Material becomes one of the material for most having application prospect.Moreover, SnS2Due to its high theoretical capacity
(690mAh·g-1), natural resources abundant, nontoxicity and low cost, it is considered to be the promising time of negative electrode material of new generation
Select object, but it is also the same with most of negative electrode materials, it is big there are volume expansion in poorly conductive, charge and discharge process the disadvantages of, limit
Its development as lithium ion battery negative material is made.For its major defect, we answer the material of itself and high conductivity
It closes or electrode design improves their electrochemistry cycle performance.
g-C3N4It is a kind of carbon material of two-dimentional (2D) graphene-structured, it is that a nitrogen heteroatom replaces graphite skeleton,
By the monatomic carry out sp of carbon and nitrogen2Hydridization is formed, and has unique planar structure, due to its relatively rich pore structure, Gao Han
Nitrogen quantity, high surface area, high cost-benefit availability and significant physics and chemical characteristic and cause sizable concern.And
Preparation process is simple, cost is relatively low.Therefore this project is by by the g-C of good conductivity3N4As the fid in charge and discharge process
Material, with SnS2Compound its electric conductivity of raising and structural stability, further increase its electricity as lithium ion battery negative material
Chemical property.Currently, many scholars by with g-C3The compound preparation novel composite electrode material of N, to improve the electrochemistry of battery
Performance.
Currently, Li et al. people [Li X, Feng Y, Li M, et al.Smart Hybrids of
Zn2GeO4Nanoparticles and Ultrathin g-C3N4Layers:Synergistic Lithium Storage
and Excellent Electrochemical Performance[J].Advanced Functional Materials,
2016,25 (44): 6858-6866.] preparation Zn2GeO4/g-C3N4Compound is in 200mAg-1140 are recycled under current density
Capacity is up to 1370mAhg after secondary-1, in high current density 2000mAg-1There is down excellent high rate performance, capacity is reachable
To 950mAhg-1；Senthil et al. [Chenrayan, K.S.Chandra, S.Manickam, Ultrathin
MoS2sheets supported on N-rich carbon nitride nanospheres with enhanced
Lithium storage properties, Applied Surface Science, 410 (2017) 215-224.] it is prepared for
MoS2/g-C3N4Nanosphere is as negative electrode material, and composite material has excellent chemical property, in 100mAg-1Electric current
Reversible capacity is 857mAhg after lower 50 circulations of density-1；The method prepared at present mainly has solvent-thermal method [Enzhou
Liu,Jibing Chen a,Yongning Ma.,et al.Fabrication of 2D SnS2/g-
C3N4heterojunction with enhanced H2evolution during photocatalytic water
splitting,Journal of Colloid and Interface Science[J].524(2018)313–324Journal
Of Catalysis, 352 (2017) 532-541.] ion-exchange [Liu Y, Chen P, Chen Y, et al.In situ
ion-exchange synthesis of SnS2/g-C3N4nanosheets heterojunction for enhancing
photocatalytic activity[J].Rsc Advances,2016,6(13).].Solvent thermal reaction method is a kind of improved
Hydro-thermal reaction method replaces traditional water to make solvent with organic solvent, but reaction process needs the condition of strict control solvent heat；From
Sub- exchange process can generate excessive regeneration liquid waste, and the period is longer, and consumption salt amount is big, and the presence of organic matter can contaminated ion exchange tree
Rouge.
Summary of the invention
The purpose of the present invention is to provide a kind of nanometer sheet self assembled three-dimensional nano flower artificial gold/graphitization carbonitride lithium from
The preparation method of sub- cell negative electrode material, to overcome the problems of the above-mentioned prior art, preparation cost of the present invention is low, operation is simple
Single, short preparation period, prepared nanometer SnS2/g-C3N4The size of cell negative electrode material reaches 50 rans, purity
Height, crystallinity is strong, pattern is uniform, is applied to negative electrode of lithium ion battery with excellent charge-discharge magnification performance.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation of nanometer sheet self assembled three-dimensional nano flower artificial gold/graphitization carbonitride lithium ion battery negative material
Method, comprising the following steps:
1) melamine is kept the temperature to 2~6h under the conditions of 450-650 DEG C, when it naturally cools to room temperature, is ground spare；
2) dispersion of step 1) products therefrom is obtained into suspension in ethanol, suspension is centrifuged and uses deionized water and nothing
Water-ethanol washs several times, and then vacuum drying obtains product g-C3N4；
3) by product g-C3N4It is dissolved in deionized water, ultrasonic disperse after stirring, forms suspending liquid A；
4) PVP is added into suspending liquid A, stirs up to being completely dissolved to form solution B, wherein product g-C3N4With the matter of PVP
Amount is than being (30mg~50mg): (0.4g~0.6g)；
5) elemental mole ratios n is pressedS: nSn=2:(0.5~2) by TAA and SnCl4·5H2O is added in solution B, is stirred evenly
Form solution C；
6) solution C progress microwave hydrothermal reaction is obtained into presoma after reaction；
7) presoma is distinguished into centrifuge washing several times through deionized water and dehydrated alcohol, then vacuum drying is received
Rice piece self assembled three-dimensional nano flower SnS2/g-C3N4Battery material.
Further, disperse 30~50mg step 1) products therefrom in step 2) in every 40~60mL ethyl alcohol.
Further, vacuum drying temperature is 60~100 DEG C in step 2), and the time is 8~14h.
Further, 30~50mg product g-C is dissolved in step 3) in every 40~60mL deionized water3N4。
Further, 1~2.85g SnCl is added in step 5) in every 40~60mL solution B4·5H2O。
Further, microwave hydrothermal reacts in step 6) specifically: solution C is put into microwave hydrothermal reaction kettle sealing, is filled out
It fills than control 40~60%, is put into microwave hydrothermal reaction, at 160~200 DEG C, reaction time control exists for reaction temperature control
1~5h.
Further, vacuum drying temperature is 80 DEG C in step 7), time 12h.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention is due to the full and uniform mixing of the auxiliary and hydro-thermal method of microwave, and, reaction very fast with reaction rate is sufficiently
Thoroughly, grain growth is controllable and the advantages such as even size distribution, and the energy consumption that it avoids conventional method is high, reaction is difficult to control, produces
The disadvantages of object is impure, nanometer sheet self assembled three-dimensional nano flower SnS prepared by the present invention2/g-C3N4Lithium ion battery negative material,
Particle size is about several nanometers, and preparation cost is low, controllable degree is high, low energy consumption, high production efficiency, yield are high, is coated on
The g-C on stannous sulfide surface3N4SnS can be alleviated2Volume change, charge-discharge performance in charge and discharge process is excellent, in 100mA/
Under the current density of g, discharge capacity can reach 640.2mAh/g or so for the first time, and after recycling 40 times, capacity is maintained at
440.6mAh/g or so, the stability with higher under high current density.
Detailed description of the invention
Fig. 1 is SnS prepared by example 2 of the present invention2/g-C3N4The SEM of cell negative electrode material schemes；
Fig. 2 is SnS prepared by example 2 of the present invention2/g-C3N4The TEM of cell negative electrode material schemes；
Fig. 3 is the made nanometer sheet self assembled three-dimensional nano flower-like structure SnS of example 3 of the present invention2/g-C3N4Lithium ion battery is negative
The high rate performance figure of pole composite material.
Specific embodiment
Embodiments of the present invention are described in further detail below:
A kind of preparation of nanometer sheet self assembled three-dimensional nano flower artificial gold/graphitization carbonitride lithium ion battery negative material
Method, comprising the following steps:
1) 5~15g melamine is placed in crucible with cover, is placed in Muffle furnace under the conditions of 450-650 DEG C
2~6h is kept the temperature, heating rate is maintained at 2 DEG C/min, when it naturally cools to room temperature, by the product of yellow as grinding in mortar
Carefully；
2) it is then dispersed in ethyl alcohol with vigorous stirring 2 hours, 30~50mg is dispersed in every 40~60mL ethyl alcohol
Step 1) products therefrom.Then, suspension is centrifuged and is washed several times with deionized water and dehydrated alcohol, then 60~100
8~14h is dried in vacuo at DEG C.It is final to obtain yellow product g-C3N4。
3) by 30~50mg g-C3N4It is dissolved in 40~60ml deionized water, strong stirring 5h, ultrasonic disperse 3h.It is formed outstanding
Supernatant liquid A；
4) 0.4~0.6g PVP (polyvinylpyrrolidone), magnetic agitation 10 are then slowly added in above-mentioned suspending liquid A
Minute is until be completely dissolved to form solution B；
5) elemental mole ratios n is pressedS: nSn=2:(0.5~2) by TAA (thioacetamide) and SnCl4·5H2O is added to
It states in solution B, 1~2.85g SnCl is added in every 40~60mL solution B4·5H2After O, magnetic agitation 30min, solution C is formed；
6) solution C is put into microwave hydrothermal reaction kettle sealing, packing ratio control is put into microwave hydrothermal reaction 40~60%
Instrument, at 160~200 DEG C, the reaction time is controlled in 1~5h for reaction temperature control；
7) to after reaction, take out presoma, at distinguishing centrifuge washing 3 times, 80 DEG C through deionized water and dehydrated alcohol
Vacuum drying 12h obtains SnS2/g-C3N4Presoma.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
1) 5g melamine is placed in crucible with cover, is placed in Muffle furnace and keeps the temperature 2h under the conditions of 450 DEG C, risen
Warm rate is maintained at 2 DEG C/min, when it naturally cools to room temperature, by the product of yellow as levigate in mortar；
2) it is then dispersed in ethyl alcohol with vigorous stirring 2 hours, 30mg step 1) institute is dispersed in every 40mL ethyl alcohol
Obtain product.Then, suspension is centrifuged and is washed several times with deionized water and dehydrated alcohol, is then dried in vacuo at 60 DEG C
8h.It is final to obtain yellow product g-C3N4。
3) by 30mg g-C3N4It is dissolved in 40ml deionized water, strong stirring 5h, ultrasonic disperse 3h.Form suspending liquid A；
4) it is then slowly added in above-mentioned suspending liquid A 0.4g PVP (polyvinylpyrrolidone), magnetic agitation 10 minutes
Until being completely dissolved to form solution B；
5) elemental mole ratios n is pressedS: nSn=2:0.5 is by TAA (thioacetamide) and SnCl4·2H2O is added to above-mentioned solution
In B, 1g SnCl is added in every 40mL solution B4·5H2After O, magnetic agitation 30min, solution C is formed；
6) solution C being put into microwave hydrothermal reaction kettle sealing, packing ratio is controlled 40%, it is put into microwave hydrothermal reaction,
At 160 DEG C, the reaction time is controlled in 1h for reaction temperature control；
7) to after reaction, take out presoma, at distinguishing centrifuge washing 3 times, 80 DEG C through deionized water and dehydrated alcohol
Vacuum drying 12h obtains SnS2/g-C3N4Presoma.
Embodiment 2
1) 10g melamine is placed in crucible with cover, is placed in Muffle furnace and keeps the temperature 4h under the conditions of 550 DEG C,
Heating rate is maintained at 2 DEG C/min, when it naturally cools to room temperature, by the product of yellow as levigate in mortar；
2) it is then dispersed in ethyl alcohol with vigorous stirring 2 hours, 40mg step 1) institute is dispersed in every 50mL ethyl alcohol
Obtain product.Then, suspension is centrifuged and is washed several times with deionized water and dehydrated alcohol, is then dried in vacuo at 80 DEG C
12h.It is final to obtain yellow product g-C3N4。
3) by 40mg g-C3N4It is dissolved in 50ml deionized water, strong stirring 5h, ultrasonic disperse 3h.Form suspending liquid A；
4) it is then slowly added in above-mentioned suspending liquid A 0.5g PVP (polyvinylpyrrolidone), magnetic agitation 10 minutes
Until being completely dissolved to form solution B；
5) elemental mole ratios n is pressedS: nSn=2:1 is by TAA (thioacetamide) and SnCl4·2H2O is added to above-mentioned solution B
In, 2.85g SnCl is added in every 60mL solution B4·5H2After O, magnetic agitation 30min, solution C is formed；
6) solution C being put into microwave hydrothermal reaction kettle sealing, packing ratio is controlled 50%, it is put into microwave hydrothermal reaction,
At 180 DEG C, the reaction time is controlled in 3h for reaction temperature control；
7) to after reaction, take out presoma, at distinguishing centrifuge washing 3 times, 80 DEG C through deionized water and dehydrated alcohol
Vacuum drying 12h obtains SnS2/g-C3N4Presoma.
As can be seen from Figure 1 prepared SnS2/g-C3N4Cell negative electrode material is nanometer sheet self assembled three-dimensional nano flower,
The thickness of nanometer sheet is about 50nm, and the size of nanometer sheet self assembled three-dimensional nano flower is about 500nm, is as can be seen from Figure 2 tied
Fruit is consistent with SEM, as can be seen from Figure 3 prepared nanometer sheet self assembled three-dimensional nano flower-like structure SnS2/g-C3N4Lithium ion
Battery cathode composite material under different current densities the capacity attenuation of battery it is very slow, and there is certain cyclical stability.
Embodiment 3
1) 15g melamine is placed in crucible with cover, is placed in Muffle furnace and keeps the temperature 6h under the conditions of 650 DEG C,
Heating rate is maintained at 2 DEG C/min, when it naturally cools to room temperature, by the product of yellow as levigate in mortar；
2) it is then dispersed in ethyl alcohol with vigorous stirring 2 hours, 50mg step 1) institute is dispersed in every 60mL ethyl alcohol
Obtain product.Then, suspension is centrifuged and is washed several times with deionized water and dehydrated alcohol, is then dried in vacuo at 100 DEG C
14h.It is final to obtain yellow product g-C3N4。
3) by 50mg g-C3N4It is dissolved in 60ml deionized water, strong stirring 5h, ultrasonic disperse 3h.Form suspending liquid A；
4) it is then slowly added in above-mentioned suspending liquid A 0.6g PVP (polyvinylpyrrolidone), magnetic agitation 10 minutes
Until being completely dissolved to form solution B；
5) elemental mole ratios n is pressedS: nSn=2:2 is by TAA (thioacetamide) and SnCl4·2H2O is added to above-mentioned solution B
In, 2g SnCl is added in every 50mL solution B4·5H2After O, magnetic agitation 30min, solution C is formed；
6) solution C being put into microwave hydrothermal reaction kettle sealing, packing ratio is controlled 60%, it is put into microwave hydrothermal reaction,
At 200 DEG C, the reaction time is controlled in 5h for reaction temperature control；
7) to after reaction, take out presoma, at distinguishing centrifuge washing 3 times, 80 DEG C through deionized water and dehydrated alcohol
Vacuum drying 12h obtains SnS2/g-C3N4Presoma.
Claims (7)
1. a kind of preparation side of nanometer sheet self assembled three-dimensional nano flower artificial gold/graphitization carbonitride lithium ion battery negative material
Method, which comprises the following steps:
1) melamine is kept the temperature to 2~6h under the conditions of 450-650 DEG C, when it naturally cools to room temperature, is ground spare；
2) dispersion of step 1) products therefrom is obtained into suspension in ethanol, suspension is centrifuged to and is used deionized water and anhydrous second
Alcohol washs several times, and then vacuum drying obtains product g-C3N4；
3) by product g-C3N4It is dissolved in deionized water, ultrasonic disperse after stirring, forms suspending liquid A；
4) PVP is added into suspending liquid A, stirs up to being completely dissolved to form solution B, wherein product g-C3N4With the amount ratio of PVP
For (30mg~50mg): (0.4g~0.6g)；
5) elemental mole ratios n is pressedS: nSn=2:(0.5~2) by TAA and SnCl4·5H2O is added in solution B, stirs evenly to be formed
Solution C；
6) solution C progress microwave hydrothermal reaction is obtained into presoma after reaction；
7) presoma is distinguished into centrifuge washing several times through deionized water and dehydrated alcohol, then vacuum drying obtains nanometer sheet
Self assembled three-dimensional nano flower SnS2/g-C3N4Battery material.
2. a kind of nanometer sheet self assembled three-dimensional nano flower artificial gold according to claim 1/graphitization nitrogenizes carbon lithium ion
The preparation method of cell negative electrode material, which is characterized in that disperse 30~50mg step 1) in step 2) in every 40~60mL ethyl alcohol
Products therefrom.
3. a kind of nanometer sheet self assembled three-dimensional nano flower artificial gold according to claim 1/graphitization nitrogenizes carbon lithium ion
The preparation method of cell negative electrode material, which is characterized in that in step 2) vacuum drying temperature be 60~100 DEG C, the time be 8~
14h。
4. a kind of nanometer sheet self assembled three-dimensional nano flower artificial gold according to claim 1/graphitization nitrogenizes carbon lithium ion
The preparation method of cell negative electrode material, which is characterized in that dissolve in 30~50mg production in step 3) in every 40~60mL deionized water
Object g-C3N4。
5. a kind of nanometer sheet self assembled three-dimensional nano flower artificial gold according to claim 1/graphitization nitrogenizes carbon lithium ion
The preparation method of cell negative electrode material, which is characterized in that 1~2.85g is added in step 5) in every 40~60mL solution B
SnCl4·5H2O。
6. a kind of nanometer sheet self assembled three-dimensional nano flower artificial gold according to claim 1/graphitization nitrogenizes carbon lithium ion
The preparation method of cell negative electrode material, which is characterized in that microwave hydrothermal reacts in step 6) specifically: solution C is put into microwave
Hydrothermal reaction kettle sealing, packing ratio control are put into microwave hydrothermal reaction 40~60%, and reaction temperature is controlled 160~200
DEG C, the reaction time controls in 1~5h.
7. a kind of nanometer sheet self assembled three-dimensional nano flower artificial gold according to claim 1/graphitization nitrogenizes carbon lithium ion
The preparation method of cell negative electrode material, which is characterized in that vacuum drying temperature is 80 DEG C in step 7), time 12h.
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| CN110148723A (en) * | 2019-05-18 | 2019-08-20 | 福建师范大学 | A kind of SnS with high performance2The preparation method and application of@nitrogen-doped carbon compound kalium ion battery negative electrode material |
| WO2021004150A1 (en) * | 2019-07-10 | 2021-01-14 | 陕西科技大学 | Preparation method for negative electrode material sns/nd-cn of lithium-ion battery |
| CN112717973A (en) * | 2020-11-16 | 2021-04-30 | 中北大学 | Preparation of rod-like g-C by microwave hydrothermal method3N4Method and application of nanosheet |
| CN113471421A (en) * | 2021-07-23 | 2021-10-01 | 山东理工大学 | Preparation method of composite positive electrode material of lithium-sulfur battery |
| CN113611835A (en) * | 2021-07-31 | 2021-11-05 | 青岛科技大学 | g-C3N4@WS2Electroactive material, method for the production thereof and use thereof |
| CN113745474A (en) * | 2021-08-13 | 2021-12-03 | 湖南理工学院 | PANI @ CN/SnS lithium ion battery anode material and preparation method thereof |
| CN114300657A (en) * | 2021-12-03 | 2022-04-08 | 荆门市格林美新材料有限公司 | Coating method of Prussian blue compound sodium ion battery positive electrode material |
| CN114653382A (en) * | 2022-03-25 | 2022-06-24 | 桂林电子科技大学 | P-n type stannous sulfide-zinc stannate semiconductor material and preparation method and application thereof |
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