CN109775675A - A kind of Re6P13, preparation method and its preparation method with the composite negative pole material of carbon material - Google Patents
A kind of Re6P13, preparation method and its preparation method with the composite negative pole material of carbon material Download PDFInfo
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- CN109775675A CN109775675A CN201811607897.9A CN201811607897A CN109775675A CN 109775675 A CN109775675 A CN 109775675A CN 201811607897 A CN201811607897 A CN 201811607897A CN 109775675 A CN109775675 A CN 109775675A
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- rhenium
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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 discloses a kind of Re6P13, preparation method and its preparation method with the composite negative pole material of carbon material, phosphatization rhenium material has been prepared by a step gas transport technology, to prepare safer negative electrode material；Phosphatization rhenium material has club shaped structure, has high specific surface area, is conducive to come into full contact with electrolyte, so that the diffusion path of lithium ion is shorter, substantially increases the high rate performance of its specific discharge capacity and battery, promote the performance of its fast charging and discharging；By compound with carbon material, electrode conductivuty is improved, and microscopic appearance can be protected not to be destroyed by the effect of the physically encapsulation or chemical bonding that are formed between the two, battery high rate performance is significantly improved；The vapor transportation technology of rheium oxide is made, production process is simple, is easy to batch and prepares, has broad application prospects.
Description
Technical field
The invention belongs to battery material technical field, especially a kind of Re6P13, preparation method and its compound with carbon material
The preparation method of negative electrode material.
Background technique
In numerous power energy storage technologies, lithium ion battery is with operating voltage is high, small in size, energy density is high, nothing
Memory effect, the advantages that having a safety feature, are widely applied in fields such as electric car, consumer electronics.In recent years, with
The driving of small-size portable device (such as: smart phone, tablet computer) and high-power electric automobile industry demand, exploitation
Lithium ion battery with fast charging and discharging ability and higher energy density is the target of currently related research.Current commodity
Lithium ion battery generally use carbon based negative electrodes material, such as graphite, although this material high stability, theoretical capacity only have
372mAh/g, therefore it is imperative to research and develop new cell negative electrode material system.It is elemental phosphorous to possess height compared to graphite cathode
Up to the theoretical capacity of 2596mAh/g, therefore phosphorous-based materials are by it is believed that be the splendid selection of commercial Li-ion battery cathode.
In general, reversible reaction can occur with lithium metal for phosphorus contained by transition metal phosphide, provide reversible capacity, for the first time
Process of intercalation are as follows:
M'xPy+3yLi++3ye-—xM+yLi3P。
The reaction lithiumation/de- lithium plateau potential is about 1V or so, much higher than the electro-deposition potential of lithium metal, therefore is conducive to
Inhibit the formation of Li dendrite, therefore there is the security performance higher than graphite electrode.At the same time, due to its low discharge platform,
The battery that transition metal phosphide and positive electrode are assembled into has considerable potential difference, this is also beneficial to the reality of high-energy density
It is existing.However, transition metal phosphide still has following problem using upper in ion cathode material lithium.On the one hand, phosphorous-based materials
Electric conductivity it is not high so that its active material utilization in sodium-ion battery is low, the capacity shown will be far below its reason
By capacity；On the other hand, although phosphorus lithiation can provide higher capacity, but volume change is larger during removal lithium embedded, especially
It is to destroy the microscopic appearance of electrode material during big circulation, causes the rapid decaying of capacity.In addition, not
Phosphide with metal has different crystal structure and activity, corresponds to different charge and discharge behavior and multiplying power stability.Mesh
Before, development of metallic phosphide is still a challenge for li-ion electrode negative electrode material.
Summary of the invention
It is an object of the invention to overcome the above-mentioned prior art, a kind of Re is provided6P13, preparation method and its and carbon
The preparation method of the composite negative pole material of material.
In order to achieve the above objectives, the present invention is achieved by the following scheme:
A kind of Re6P13Preparation method, comprising the following steps:
1) rhenium powder and red phosphorus are mixed under the atmosphere of inert gas, obtains two-phase mixture；Wherein, rhenium powder with it is red
The mass ratio of phosphorus is 6:(3.5~4.5)；
2) transfer agent is added in two-phase mixture, obtains three-phase mixture, the pressure in space where making three-phase mixture
For vacuum pressure；Wherein, the quality of transfer agent and rhenium powder and the mass ratio of red phosphorus gross mass are 1%~5%；
3) chemical vapor transport method is used, three-phase mixture is warming up to 850~900 DEG C, heat preservation cools down after 3-12 days,
Obtain include phosphatization rhenium mixture；
4) after taking out cleaned mixture, centrifugation and drying, phosphatization rhenium powder is obtained.
Further, the inert gas in step 1) is argon gas or nitrogen.
Further, the transfer agent in step 2) includes I2Or Br2。
Further, the vacuum pressure in step 2) is 10-2~10-6Pa。
Further, heating rate is 3~10 DEG C/min in step 3), and rate of temperature fall is 3~10 DEG C/min.
Further, in step 4), specific step is as follows for cleaning:
1) mixture is impregnated 3~6 hours in carbon disulfide；
2) mixture is impregnated in acetone 3~6 hours again；
3) last to be cleaned by ultrasonic 1~4 hour in ethanol.
A kind of claval Re of layer structure6P13。
A kind of Re6P13With the preparation method of the composite negative pole material of carbon material, comprising:
By Re6P13It is mixed with carbon material, carries out ball milling mixing after mixing, obtain the composite negative pole material of phosphatization rhenium and carbon material
Material；Wherein, the mass ratio of phosphatization rhenium and carbon material is (4~8): 1.
Further, carbon material is acetylene black, carbon nanotube, graphene or super P.
Further, rotational speed of ball-mill is 300~900r/min, and Ball-milling Time is 3~1 hours.Compared with prior art, originally
Invention has the advantages that
A kind of Re of the invention6P13, preparation method and its preparation method with the composite negative pole material of carbon material, pass through one
Step gas transport technology has prepared phosphatization rhenium material, and the product purity of chemical vapor transport method preparation is higher, to prepare
Safer negative electrode material；Stratiform phosphatization rhenium has club shaped structure, has high specific surface area, is conducive to abundant with electrolyte
Contact, so that the diffusion path of lithium ion is shorter, substantially increases the high rate performance of its specific discharge capacity and battery, and it is fast to promote it
Fill the performance put fastly；By compound with carbon material, improve electrode conductivuty, and can by the physically encapsulation that is formed between the two or
The effect of chemical bonding protects microscopic appearance not to be destroyed, and battery high rate performance is significantly improved；Make the gas of rheium oxide
Phase transport technique, production process is simple, is easy to batch and prepares, has broad application prospects.
Detailed description of the invention
Fig. 1 is the XRD diagram of phosphatization rhenium prepared by the embodiment of the present invention 1；
Fig. 2 is the crystal structure of phosphatization rhenium prepared by the embodiment of the present invention 1；
Fig. 3 is the scanning electron microscope (SEM) photograph of phosphatization rhenium prepared by the embodiment of the present invention 1；
Fig. 4 is the transmission electron microscope picture of phosphatization rhenium prepared by the embodiment of the present invention 1；
Fig. 5 is under the 0.1A/g of the composite negative pole material of the phosphatization rhenium and carbon material that are prepared using the embodiment of the present invention 1
The charging and discharging curve of first three circle；
Fig. 6 is the high rate performance curve of the phosphatization rhenium and carbon compound cathode materials that are prepared using the embodiment of the present invention 1.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, below in conjunction in the embodiment of the present invention
Attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only
The embodiment of a part of the invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people
The model that the present invention protects all should belong in member's every other embodiment obtained without making creative work
It encloses.
It should be noted that description and claims of this specification and term " first " in above-mentioned attached drawing, "
Two " etc. be to be used to distinguish similar objects, without being used to describe a particular order or precedence order.It should be understood that using in this way
Data be interchangeable under appropriate circumstances, so as to the embodiment of the present invention described herein can in addition to illustrating herein or
Sequence other than those of description is implemented.In addition, term " includes " and " having " and their any deformation, it is intended that cover
Cover it is non-exclusive include, for example, the process, method, system, product or equipment for containing a series of steps or units are not necessarily limited to
Step or unit those of is clearly listed, but may include be not clearly listed or for these process, methods, product
Or other step or units that equipment is intrinsic.
The invention will be described in further detail with reference to the accompanying drawing:
Chemical vapor transportation method is the important method of crystal growth, the synthesis of noval chemical compound and purification of substance etc..We
In method, Re and P can carry out dependent interaction with the transfer agent of gasification and generate volatile intermediate product in vacuum high-temperature environment,
And then can interact, generate Re6P13And it deposits, bulk chemical reaction equation are as follows:
6Re+13P→Re6P13
The product purity of chemical vapor transport method preparation is higher, can obtain high-purity by the method for controlling temperature gradient
Non-volatile reactant or product.
Embodiment 1
1) rhenium powder and red phosphorus are weighed according to the ratio that mass ratio is 6:3.5, is mixed under the protection of Ar gas, is placed in one end
In the quartz ampoule of sealing；
2) I is added into quartz ampoule2, it is evacuated to 10-6Pa, by another end closure of quartz ampoule；Wherein, the quality of iodine is compared
In the ratio of rhenium and red phosphorus gross mass be 1%；
3) I is used2As transfer agent, by chemical vapor transport method, quartz ampoule is placed in heating furnace with 5 DEG C/min liter
Temperature after heat preservation 3 days, is slowly cooled to room temperature with 5 DEG C/min to 900 DEG C, grows phosphatization rhenium powder；
4) mixture in quartz ampoule is taken out, is impregnated 3 hours first in carbon disulfide, then immersion 3 is small in acetone
When, finally it is cleaned by ultrasonic in ethanol 1 hour, is then placed in a vacuum drying oven drying by centrifugation, obtains phosphatization rhenium powder；
5) phosphatization rhenium powder and graphene that mass ratio is 8:1 are mixed, and is placed in high energy ball mill and carries out ball milling
Mixing, revolving speed 300r/min, Ball-milling Time are 3 hours, obtain the composite negative pole material of phosphatization rhenium and carbon material.
It is the XRD diagram of phosphatization rhenium prepared by the embodiment of the present invention 1 referring to Fig. 1, Fig. 1；XRD diagram is by manufactured in the present embodiment
Phosphatization rhenium carries out obtained by X-ray diffraction analysis, and by comparing with standard JCPDS card, phosphatization rhenium prepared by the present embodiment is
The Re of rhombohedral structure6P13Phase, crystal structure are as shown in Figure 2；
Referring to Fig. 3, Fig. 3 a and 3b are scanning electron microscope of the phosphatization rhenium for preparing of the embodiment of the present invention 1 in different amplification
Figure has high specific surface area from the figure 3, it may be seen that the phosphatization rhenium material prepared through this embodiment is the clava of layer structure,
Be conducive to come into full contact with electrolyte, so that the diffusion path of lithium ion is shorter, substantially increase its specific discharge capacity and electricity
The high rate performance in pond promotes the performance of its fast charging and discharging.
Referring to fig. 4, Fig. 4 is transmission electron microscope (TEM) figure of phosphatization rhenium prepared by the embodiment of the present invention 1, as shown in Figure 4,
The phosphatization rhenium material prepared through this embodiment is club shaped structure, average diameter 300nm.
By lithium ion battery negative material manufactured in the present embodiment and conductive black, Kynoar with mass ratio 8:1:1
Ground and mixed is uniform, and appropriate N-Methyl pyrrolidone (NMP) is added and is tuned into pulpous state, is coated on copper foil in 120 DEG C of drying
Dry 6h, is then cut into piece, anode plate for lithium ionic cell is made in case.Lithium ion battery negative electrode is assembled into button electricity
Its performance is tested in pond.
Referring to Fig. 5, Fig. 5 is the composite negative pole material of the phosphatization rhenium and carbon material that are prepared using the embodiment of the present invention 1
The charging and discharging curve that first three is enclosed under 0.1A/g；Figure 4, it is seen that battery initial charge specific capacity reaches 1249.1mAh/g.
Referring to Fig. 6, Fig. 6 is the forthright again of the phosphatization rhenium prepared using the embodiment of the present invention 1 and carbon compound cathode materials
It can curve.As can be known from Fig. 6, material has excellent high rate performance, under the high current density of 20A/g, cyclic specific capacity
Still reach 575.9mAh/g, illustrates that battery has the performance of preferable fast charging and discharging.
Embodiment 2
1) rhenium powder and red phosphorus are weighed according to the ratio of mass ratio 6:4, in N2Mechanical mixture under gas atmosphere is placed in an end seal
In the quartz ampoule of mouth；
2) Br is added into quartz ampoule2, Br2Quality compared to the ratio of rhenium and red phosphorus gross mass be 3%, be evacuated to
10-2Pa, by another end closure of quartz ampoule；
3) quartz ampoule, which is placed in heating furnace, is warming up to 850 DEG C with 3 DEG C/min, after keeping the temperature 12 days, with 3 DEG C/min Slow cooling
To room temperature, phosphatization rhenium powder is grown；
4) it by the product cleaning in quartz ampoule, is successively impregnated respectively 3 hours using carbon disulfide, acetone, then in ethanol
Ultrasonic cleaning 3 hours, centrifugation postposition in a vacuum drying oven, obtain phosphatization rhenium powder；
5) it is that 6:1 phosphatization rhenium powder and super P are mixed by mass ratio, is placed in high energy ball mill and carries out ball milling mixing,
Revolving speed is 600r/min, and Ball-milling Time is 1.5 hours, obtains the composite negative pole material of phosphatization rhenium and carbon material.
By lithium ion battery negative material manufactured in the present embodiment and conductive black, Kynoar with mass ratio 8:1:1
Ground and mixed is uniform, and appropriate N-Methyl pyrrolidone (NMP) is added and is tuned into pulpous state, is coated on copper foil in 120 DEG C of drying
Dry 6h, is then cut into piece, anode plate for lithium ionic cell is made in case.
Lithium ion battery negative electrode is assembled into button cell and tests its performance.Battery initial charge specific capacity reaches
1131.2mAh/g, under the high current density of 20A/g, cyclic specific capacity still reaches 515.3mAh/g, illustrate battery have compared with
The performance of good fast charging and discharging.
Embodiment 3
1) the rhenium powder and red phosphorus of mass ratio 6:4.5 are weighed, the mechanical mixture under Ar gas atmosphere is placed in the stone of an end closure
Ying Guanzhong；
2) I is added into quartz ampoule2, I2Quality compared to the ratio of rhenium and red phosphorus gross mass be 5%, be evacuated to 10-4Pa, by another end closure of quartz ampoule；
3) make iodine I2As transfer agent, by chemical vapor transport method, quartz ampoule is warming up to 860 with 10 DEG C/min
DEG C, 5 days are kept the temperature, is slowly cooled to room temperature with 10 DEG C/min, grows phosphatization rhenium；
4) product in quartz ampoule is taken out, is successively impregnated 6 hours in carbon disulfide, acetone, then is ultrasonic in ethanol
Cleaning 4 hours, centrifugation postposition in a vacuum drying oven, obtain phosphatization rhenium powder；
5) phosphatization rhenium powder and carbon nanotube are mixed with the mass ratio of 4:1, it is mixed is placed in progress ball milling in high energy ball mill
It closes, revolving speed 900r/min, Ball-milling Time is 1 hour, obtains the composite negative pole material of phosphatization rhenium and carbon material.
By lithium ion battery negative material manufactured in the present embodiment and conductive black, Kynoar with mass ratio 8:1:1
Ground and mixed is uniform, and appropriate N-Methyl pyrrolidone (NMP) is added and is tuned into pulpous state, is coated on copper foil in 120 DEG C of drying
Dry 6h, is then cut into piece, anode plate for lithium ionic cell is made in case.
Lithium ion battery negative electrode is assembled into button cell and tests its performance.Battery initial charge specific capacity reaches
1210.2mAh/g, under the high current density of 20A/g, cyclic specific capacity still reaches 523.7mAh/g, illustrate battery have compared with
The performance of good fast charging and discharging.
Embodiment 4
1) the rhenium powder and red phosphorus of mass ratio 6:4.5 are weighed, the mechanical mixture under Ar gas atmosphere is placed in the stone of an end closure
Ying Guanzhong；
2) I is added into quartz ampoule2, I2Quality compared to the ratio of rhenium and red phosphorus gross mass be 4%, be evacuated to 10-5Pa, by another end closure of quartz ampoule；
3)I2As transfer agent, by chemical vapor transport method, quartz ampoule is warming up to 900 DEG C with 8 DEG C/min, heat preservation
It 8 days, is slowly cooled to room temperature with 8 DEG C/min, grows phosphatization rhenium；
4) product in quartz ampoule is taken out, is successively impregnated 5 hours in carbon disulfide, acetone, then is ultrasonic in ethanol
Cleaning 4 hours, centrifugation postposition in a vacuum drying oven, obtain phosphatization rhenium powder；
5) phosphatization rhenium powder and acetylene black are mixed with the mass ratio of 5:1, it is mixed is placed in the progress ball milling in high energy ball mill
It closes, revolving speed 1000r/min, Ball-milling Time is 1 hour, obtains the composite negative pole material of phosphatization rhenium and carbon material.
By lithium ion battery negative material manufactured in the present embodiment and conductive black, Kynoar with mass ratio 8:1:1
Ground and mixed is uniform, and appropriate N-Methyl pyrrolidone (NMP) is added and is tuned into pulpous state, is coated on copper foil in 120 DEG C of drying
Dry 6h, is then cut into piece, anode plate for lithium ionic cell is made in case.
Lithium ion battery negative electrode is assembled into button cell and tests its performance.Battery initial charge specific capacity reaches
1007.2mAh/g, under the high current density of 20A/g, cyclic specific capacity still reaches 493.7mAh/g, illustrate battery have compared with
The performance of good fast charging and discharging.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press
According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention
Protection scope within.
Claims (10)
1. a kind of Re6P13Preparation method, which comprises the following steps:
1) rhenium powder and red phosphorus are mixed under the atmosphere of inert gas, obtains two-phase mixture；Wherein, rhenium powder and red phosphorus
Mass ratio is 6:(3.5~4.5)；
2) transfer agent is added in two-phase mixture, obtains three-phase mixture, the pressure in space is true where making three-phase mixture
Pneumatics power；Wherein, the quality of transfer agent and rhenium powder and the mass ratio of red phosphorus gross mass are 1%~5%；
3) chemical vapor transport method is used, three-phase mixture is warming up to 850~900 DEG C, heat preservation cools down after 3-12 days, obtains
It include the mixture of phosphatization rhenium；
4) after taking out cleaned mixture, centrifugation and drying, phosphatization rhenium powder is obtained.
2. Re according to claim 16P13Preparation method, which is characterized in that inert gas in step 1) is argon gas
Or nitrogen.
3. Re according to claim 16P13Preparation method, which is characterized in that the transfer agent in step 2) includes I2Or
Br2。
4. Re according to claim 16P13Preparation method, which is characterized in that vacuum pressure in step 2) is 10-2~
10-6Pa。
5. Re according to claim 16P13Preparation method, which is characterized in that in step 3) heating rate be 3~10
DEG C/min, rate of temperature fall is 3~10 DEG C/min.
6. Re according to claim 16P13Preparation method, which is characterized in that in step 4), the specific steps of cleaning are such as
Under:
1) mixture is impregnated 3~6 hours in carbon disulfide；
2) mixture is impregnated in acetone 3~6 hours again；
3) last to be cleaned by ultrasonic 1~4 hour in ethanol.
7. a kind of Re according to claim 1-66P13The obtained Re of preparation method6P13, which is characterized in that
Re6P13For the clava of layer structure.
8. a kind of Re according to claim 76P13With the preparation method of the composite negative pole material of carbon material, feature exists
In, comprising:
By Re6P13It is mixed with carbon material, carries out ball milling mixing after mixing, obtain the composite negative pole material of phosphatization rhenium and carbon material；
Wherein, the mass ratio of phosphatization rhenium and carbon material is (4~8): 1.
9. Re according to claim 86P13With the preparation method of the composite negative pole material of carbon material, which is characterized in that carbon
Material is acetylene black, carbon nanotube, graphene or super P.
10. Re according to claim 86P13With the preparation method of the composite negative pole material of carbon material, which is characterized in that ball
Mill revolving speed is 300~900r/min, and Ball-milling Time is 3~1 hours.
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