CN107768660A - A kind of lithium ion battery negative material and preparation method thereof - Google Patents
A kind of lithium ion battery negative material and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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Abstract
A kind of lithium ion battery negative material and preparation method thereof.The preparation method is that prepared by molybdenum precursor solution and template aqueous solution hybrid reaction into hybrid, and Mo is obtained through calcining after hybrid dinectly bruning or hybrid tablettingyOzLithium ion battery negative material.The preparation method of the present invention is simple, and equipment requirement is low, is easy to large-scale production.Molybdenum oxide prepared by the present invention has special pattern, good crystallinity, and initial discharge specific capacity is 710mAhg‑1More than, it is optimal up to 953mAhg‑1, can be most preferably more than 99.5% through 50 circulation specific discharge capacity conservation rates, be had a good application prospect in lithium ion battery negative material field.
Description
Technical field
The present invention relates to lithium ion battery negative material and preparation method thereof, more particularly to a kind of negative electrode of lithium ion battery material
Expect molybdenum oxide and preparation method thereof, belong to technical field of lithium ion.
Background technology
With the fast development of global economy, energy and environment, which have become, has a strong impact on the human society survival and development
Two big key issues.The world utilizes the 85% of the energy from conventional fossil fuels such as coal, oil, natural gases at present, and this
A little energy just gradually using up it is totally non-renewable, and environmental pollution caused by combustion of fossil fuels with climate change
The common difficulty faced as countries in the world.The exploitation of environment-friendly new energy technology increasingly becomes the world today with application
One of strategy of sustainable development of various countries.In numerous new energy technologies, lithium ion battery is as a kind of height that can be recycled
Effect green novel energy source, it is a kind of comprehensive important technology approach for alleviating the energy, resource and environmental problem.Especially base in the last few years
Numerous application fields such as the portable electric appts that are developed rapidly in lithium battery, electric vehicle, space flight and aviation, show
Lithium ion battery plays an important role in today's society.
Lithium ion battery negative material is the important component of lithium battery.At present, commercialized negative electrode of lithium ion battery
Material uses graphite material more, and its theoretical capacity is only 372mAhg-1, restricted because its specific capacity is low, the problem of poor safety performance
The further exploitation and application of power lithium-ion battery.Therefore, the lithium-ion electric that a kind of specific capacity is high, has a safety feature is developed
Pond negative material turns into the emphasis studied now and difficult point.In the last few years, the molybdenum oxide in transition metal oxide was due to it
Variable valency scope is big, specific capacity is high has been a great concern in lithium cell cathode material research field.
M.F.Hassan et al. is with (NH4)6Mo7O24·4H2O and HNO3For raw material, MoO is prepared for using hydro-thermal method3Nanometer
Band, first discharge specific capacity are about 1200mAhg-1, it is about 320mAhg to circulate its specific discharge capacity by 50 times-1, capacity declines
Subtract quite serious.C.Q.Feng et al. is with (NH4)2MoO4, PNA and DMF be raw material, it is different using method of electrostatic spinning and later stage
The calcining of atmosphere is prepared for MoO respectively3And MoO3/ C nano fiber.Current density is 100mAg-1When, MoO3Discharge specific volume first
Amount is about 720mAhg-1, it is about 200mAhg to circulate its specific discharge capacity by 30 times-1, the MoO of this method preparation3Stable circulation
Can be poor；MoO3/ C nano fiber first discharge specific capacity is about 1200mAhg-1, it is serious to circulate its capacitance loss for the second time, puts
Electric specific capacity is about 700mAhg-1, it is about 600mAhg to circulate its specific discharge capacity by 100 times-1Although later cycles are steady
It is qualitative relatively preferable, but its specific discharge capacity is relatively low, and also technological process is complicated.
The content of the invention
For insufficient existing for existing cathode of lithium battery molybdenum oxide material, an object of the present invention is to provide one kind
The preparation method of lithium ion battery negative material, the molybdenum oxide have excellent electrochemistry circulation as lithium cell cathode material
Stability.
The present invention adopts the following technical scheme that：
A kind of preparation method of lithium ion battery negative material, comprises the following steps：
(1) by molybdenum precursor solution and template solution hybrid reaction, the sediment of generation can filtered, washing, drying
Hydridization powder is made；
(2) by calcination processing after the hydridization powder dinectly bruning obtained by step (1) or hydridization powder tabletting, molybdenum is obtained
Oxide cathode material.
Preferably, template described in step (1) is the week reduction material with oh group, preferably polyethylene
One or more kinds of mixing in pyrrolidones, polyethylene glycol, PEG-PPO-PEG.With with oh group it is weak also
Immunogenic substance prepares the hybrid of different-shape and valence state as the structure directing agent and reducing agent of hybrid.
Preferably, the weight average molecular weight of the template is 1000~30000Da, for example, 2000Da, 3500Da,
5000Da, 8000Da, 15000Da, 22000Da, 25000Da, 28500Da, 29600Da etc., preferably 6000~20000Da.
Preferably, molybdenum precursor solution described in step (1) is made by the way that molybdenum powder is dissolved in hydrogen peroxide.
In order that molybdenum powder complete oxidation, it is preferable that the mol ratio of the molybdenum powder and hydrogen peroxide is 1:3.92~1:10, example
Such as it is 1:4、1:4.3、1:4.8、1:5.2、1:6、1:7.5、1:8.3、1:9、1:9.7 etc., preferably 1:5~1:8.
Preferably, template solution described in step (1) is made by adding to dissolve template in deionized water.
Preferably, the addition mole of the template is 1/4000~1/13, for example, 1/3500, the 1/ of molybdenum powder
2000th, 1/1000,1/500,1/330,1/100,1/85,1/60,1/50,1/35,1/20,1/15 etc., preferably 1/3000~
1/300.By the regulation to template addition, realize regulation and control to hybrid pattern and molybdenum oxide it is different degrees of also
Original, and different degrees of high conductivity carbon is formd in later stage high-temperature calcination, so as to improve the electron conduction of material and
Cyclical stability.
Preferably, the volume ratio of the hydrogen peroxide and deionized water is 1:1~1:5, for example, 1:1.2、1:1.6、1:
2.2、1:2.8、1:3.3、1:3.9、1:4.3、1:4.8 etc., preferably 1:1~1:3.
Preferably, the temperature reacted described in step (2) be 60~200 DEG C, for example, 63 DEG C, 69 DEG C, 80 DEG C, 95
DEG C, 120 DEG C, 145 DEG C, 160 DEG C, 175 DEG C, preferably 186 DEG C, 197 DEG C etc., 70~180 DEG C.
Preferably, the time of the reaction is 12~30h, for example, 13h, 16h, 19h, 22h, 26h, 29h etc., is preferably
16~28h.
Preferably, the molecular formula of the hybrid is H2MoOx, wherein 3≤x≤5, or be unformed.
Preferably, the pattern of the hybrid is one or more kinds of combinations in banding, spherical, cube.
Preferably, the pressure in step (3) during tabletting is 5~25MPa, for example, 7MPa, 9MPa, 12MPa, 16MPa,
21MPa, 24MPa etc., preferably 8~20MPa.
Preferably, the atmosphere during calcining is combination more than one or both of argon gas, nitrogen, air.
Preferably, the temperature of the calcining be 300~900 DEG C, for example, 330 DEG C, 390 DEG C, 450 DEG C, 520 DEG C, 600
DEG C, 650 DEG C, 710 DEG C, preferably 820 DEG C, 880 DEG C etc., 400~800 DEG C.
Preferably, the time of the calcining is 0.5~5h, for example, 0.7h, 1.2h, 1.5h, 1.9h, 2.2h, 2.8h,
3.5h, 4.2h, 4.7h etc., preferably 1~3h.
Preferably, the heating rate during calcining is 1~7 DEG C/min, for example, 1.5 DEG C/min, 2 DEG C/min, 3 DEG C/
Min, 4.5 DEG C/min, 5.5 DEG C/min, 6.3 DEG C/min etc., preferably 1~5 DEG C/min.
An object of the present invention, which also resides in, provides molybdenum oxide prepared by the preparation method of the present invention, and its molecular formula is
MoyOz, wherein y:Z=1:2~1:3, preferably pattern is one or more kinds of in sheet, banding, spherical, cube
Combination.
The present invention compared with prior art, has advantages below and high-lighting effect：The preparation method of the present invention is simple, closes
It is few into required reactant species, it is low for equipment requirements, it is easy to large-scale production.Molybdenum oxide prepared by the present invention has spy
Different pattern, there is the characteristics of good crystallinity, Stability Analysis of Structures, good cycle, initial discharge specific capacity is 710mAhg-1More than,
Optimal reachable 953mAhg-1, can be most preferably more than 99.5% through 50 circulation specific discharge capacity conservation rates, show fabulous follow
Ring stability, had a good application prospect in lithium ion battery negative material field.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of molybdenum oxide prepared by the embodiment of the present invention；
Fig. 2 is the scanning electron microscope diagram of molybdenum oxide prepared by the embodiment of the present invention；
Fig. 3 is the discharge cycle performance curve of molybdenum oxide negative material prepared by the embodiment of the present invention.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for help and understands the present invention, is not construed as the concrete restriction to the present invention.
Embodiment 1：
(1) 4.78g molybdenum powders are dissolved in 20mL hydrogen peroxide and molybdenum precursor solution is made, wherein, raw material molybdenum powder and hydrogen peroxide
Mol ratio is 1:3.92；
(2) weigh and be sufficiently stirred directly in 0.375g polyethylene glycol (weight average molecular weight 30000) addition 100mL deionized waters
To being completely dissolved, wherein, the addition mole of polyethylene glycol is the 1/4000 of molybdenum, and the volume ratio of hydrogen peroxide and deionized water is 1:
5；
(3) (1) and (2) is mixed and reacts 20h in 200 DEG C, sediment is filtered, washed, dries obtained hybrid；
(4) above-mentioned prepared hybrid is pushed flakiness and is put into crucible in 10MPa pressure and be built in Muffle furnace,
With 3 DEG C/min heating rate from room temperature to 500 DEG C, 3h is incubated, room temperature is finally naturally cooled to, produces molybdenum oxide and bear
Pole material.
A is the X-ray diffractogram of the molybdenum oxide prepared by embodiment 1 in Fig. 1, and the molybdenum oxide is as seen from the figure
Rhombic MoO3；
A is the scanning electron microscope diagram of the molybdenum oxide prepared by embodiment 1 in Fig. 2, as seen from the figure the MoO3
Pattern be banding；
A is the MoO prepared by embodiment 1 in Fig. 33As the cyclic curve of lithium ion battery negative material, in 0.01-3V
Voltage range, to carry out discharge and recharge, first discharge specific capacity 952.9mAhg under 0.1C multiplying powers-1, discharge specific volume after 50 circulations
Amount can be maintained at 829.9mAhg-1, show good cyclical stability.
Embodiment 2：
(1) 4.78g molybdenum powders are dissolved in 30mL hydrogen peroxide and molybdenum precursor solution is made, wherein, raw material molybdenum powder and hydrogen peroxide
Mol ratio is 1:5.88；
(2) weigh and fully stirred in 0.5g polyvinylpyrrolidones (weight average molecular weight 20000) addition 75mL deionized waters
Mix until be completely dissolved, wherein, the addition mole of polyvinylpyrrolidone is the 1/2000 of molybdenum, hydrogen peroxide and deionized water
Volume ratio is 1:2.5；
(3) (1) and (2) is mixed and reacts 30h in 60 DEG C, sediment is filtered, washed, dries obtained hybrid；
(4) above-mentioned prepared hybrid is pushed flakiness and is put into crucible in 25MPa pressure and be built in Muffle furnace,
With 10 DEG C/min heating rate from room temperature to 900 DEG C, 0.5h is incubated, finally naturally cools to room temperature, produce molybdenum oxidation
Thing.
B is the X-ray diffractogram of the molybdenum oxide prepared by embodiment 2 in Fig. 1, and molybdenum oxide is oblique as seen from the figure
The MoO of prismatic crystal system3；
B is the scanning electron microscope diagram of the molybdenum oxide prepared by embodiment 2 in Fig. 2, as seen from the figure the MoO3
Pattern be sheet；
B is the MoO prepared by embodiment 2 in Fig. 33As the cyclic curve of lithium ion battery negative material, in 0.01-3V
Voltage range, to carry out discharge and recharge, first discharge specific capacity 951.2mAhg under 0.1C multiplying powers-1, discharge specific volume after 50 circulations
Measure as 625.6mAhg-1。
Embodiment 3：
(1) 4.78g molybdenum powders are dissolved in 51mL hydrogen peroxide and molybdenum precursor solution is made, wherein, raw material molybdenum powder and hydrogen peroxide
Mol ratio is 1:10；
(2) weigh 3.84g polyethylene glycol (weight average molecular weight 1000) add 51mL deionized waters in be sufficiently stirred until
It is completely dissolved, wherein, the addition mole of polyethylene glycol is the 1/13 of molybdenum, and the volume ratio of hydrogen peroxide and deionized water is 1:1；
(3) (1) and (2) is mixed and reacts 12h in 90 DEG C, sediment is filtered, washed, dries obtained hybrid；
(4) above-mentioned prepared hybrid is pushed flakiness and is put into crucible in 5MPa pressure and be built in Muffle furnace,
With 1 DEG C/min heating rate from room temperature to 300 DEG C, 5h is incubated, room temperature is finally naturally cooled to, produces molybdenum oxide and bear
Pole material.
The molybdenum oxide that this method is prepared is MoO3, pattern is sheet, has good electrochemical cycle stability.
Embodiment 4：
(1) 4.78g molybdenum powders are dissolved in 40mL hydrogen peroxide and molybdenum precursor solution is made, wherein, raw material molybdenum powder and hydrogen peroxide
Mol ratio is 1:7.84；
(2) weigh 5g PEG-PPO-PEG (weight average molecular weight 5800) add 60mL deionized waters in be sufficiently stirred until
It is completely dissolved, wherein, the addition mole of PEG-PPO-PEG triblock copolymers is the 1/58 of molybdenum, hydrogen peroxide and deionized water
Volume ratio be 1:1.5；
(3) (1) and (2) is mixed and reacts 18h in 70 DEG C, sediment is filtered, washed, dries obtained hybrid；
(4) above-mentioned prepared hybrid is put into crucible to be built in tube furnace, in a nitrogen atmosphere with 5 DEG C/min's
Heating rate is incubated 1h, finally naturally cools to room temperature, produce molybdenum oxide from room temperature to 600 DEG C.
C is the X-ray diffractogram of the molybdenum oxide prepared by embodiment 4 in Fig. 1, and molybdenum oxide is as seen from the figure
MoO2。
C is the scanning electron microscope diagram of the molybdenum oxide prepared by embodiment 4 in Fig. 2, as seen from the figure the MoO2
For spheric granules, size is between 2~5 μm.
C is the MoO prepared by embodiment 4 in Fig. 32As the cyclic curve of lithium ion battery negative material, in 0.01-3V
Voltage range, to carry out discharge and recharge, first discharge specific capacity 768mAhg under 0.1C multiplying powers-1, specific discharge capacity after 50 circulations
For 744mAhg-1, it can be seen that the molybdenum oxide has good cyclical stability.
Embodiment 5：
(1) 4.78g molybdenum powders are dissolved in 45mL hydrogen peroxide and molybdenum precursor solution is made, wherein, raw material molybdenum powder and hydrogen peroxide
Mol ratio is 1:8.81；
(2) weigh and be sufficiently stirred in 10g polyvinylpyrrolidones (weight average molecular weight 8000) addition 90mL deionized waters
Until be completely dissolved, wherein, the addition mole of polyvinylpyrrolidone is the 1/40 of molybdenum, the volume of hydrogen peroxide and deionized water
Than for 1:2；
(3) (1) and (2) is mixed and reacts 16h in 80 DEG C, sediment is filtered, washed, dries obtained hybrid；
(4) above-mentioned prepared hybrid is put into crucible to be built in tube furnace, under an argon atmosphere with 4 DEG C/min's
Heating rate is incubated 4h, finally naturally cools to room temperature, produce molybdenum oxide from room temperature to 700 DEG C.
The molybdenum oxide that this method is prepared is MoO2, pattern is spherical, has excellent electrochemical cycle stability.
Embodiment 6：
(1) 4.78g molybdenum powders are dissolved in 25mL hydrogen peroxide and molybdenum precursor solution is made, wherein, raw material molybdenum powder and hydrogen peroxide
Mol ratio is 1:4.9；
(2) weigh and be sufficiently stirred in 15g polyethylene glycol (weight average molecular weight 6000) addition 80mL deionized waters until complete
Fully dissolved, wherein, the addition mole of polyvinylpyrrolidone is the 1/20 of molybdenum, and the volume ratio of hydrogen peroxide and deionized water is 1:
3.2；
(3) (1) and (2) is mixed and reacts 24h in 120 DEG C, sediment is filtered, washed, dries obtained hybrid；
(4) above-mentioned prepared hybrid is put into crucible to be built in tube furnace, in a nitrogen atmosphere with 7 DEG C/min's
Heating rate is incubated 2.5h, finally naturally cools to room temperature, produce molybdenum oxide from room temperature to 450 DEG C.
D is the X-ray diffractogram of the molybdenum oxide prepared by embodiment 6 in Fig. 1, and molybdenum oxide is as seen from the figure
MoO2。
D is the scanning electron microscope diagram of the molybdenum oxide prepared by embodiment 6 in Fig. 2, as seen from the figure the MoO2
For cubic granules, size is between 1~2 μm.
D is the MoO prepared by embodiment 6 in Fig. 32As the cyclic curve of lithium ion battery negative material, in 0.01-3V
Voltage range, to carry out discharge and recharge, first discharge specific capacity 720.1mAhg under 0.1C multiplying powers-1, discharge specific volume after 50 circulations
Measure as 716.6mAhg-1, it can be seen that the molybdenum oxide has good cyclical stability.
Applicant states that the present invention illustrates the detailed process equipment of the present invention and technological process by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, that is, it is above-mentioned detailed not mean that the present invention has to rely on
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, selection of concrete mode etc., all fall within the present invention's
Within the scope of protection domain and disclosure.
Claims (10)
1. a kind of preparation method of lithium ion battery negative material, comprises the following steps：
(1) molybdenum precursor solution and template solution hybrid reaction are prepared into hybrid；
(2) by calcination processing after the hybrid dinectly bruning obtained by step (1) or hybrid tabletting, molybdenum oxide negative pole material is obtained
Material.
2. preparation method according to claim 1, it is characterised in that template described in step (1) is with hydroxyl base
Group week reduction material, preferably in polyvinylpyrrolidone, polyethylene glycol, PEG-PPO-PEG it is one or two kinds of with
On mixing；
Preferably, the weight average molecular weight of the template is 1000~30000Da, preferably 6000~20000Da.
3. preparation method according to claim 1 or 2, it is characterised in that molybdenum precursor solution passes through described in step (1)
Molybdenum powder is dissolved in hydrogen peroxide and is made；
Preferably, the mol ratio of the molybdenum powder and hydrogen peroxide is 1:3.92~1:10, preferably 1:5~1:8.
4. according to the preparation method described in claim any one of 1-3, it is characterised in that template solution described in step (1)
It is made by adding to dissolve template in deionized water；
Preferably, the addition mole of the template is 1/4000~1/13, preferably the 1/3000~1/300 of molybdenum powder；
Preferably, the volume ratio of the hydrogen peroxide and deionized water is 1:1~1:5, preferably 1:1~1:3.
5. according to the preparation method described in claim any one of 1-4, it is characterised in that the temperature reacted described in step (2)
For 60~200 DEG C, preferably 70~180 DEG C；
Preferably, the time of the reaction is 12~30h, preferably 16~28h.
6. according to the preparation method described in claim any one of 1-5, it is characterised in that point of hybrid described in step (2)
Minor is H2MoOx, wherein 3≤x≤5, or be unformed；
Preferably, the pattern of the hybrid is one or more kinds of combinations in banding, spherical, cube.
7. according to the preparation method described in claim any one of 1-6, it is characterised in that the pressure in step (3) during tabletting is 5
~25MPa, preferably 8~20MPa.
8. according to the preparation method described in claim any one of 1-7, it is characterised in that gas when being calcined described in step (3)
Atmosphere is combination more than one or both of argon gas, nitrogen, air；
Preferably, the temperature of the calcining is 300~900 DEG C, preferably 400~800 DEG C；
Preferably, the time of the calcining is 0.5~5h, preferably 1~3h；
Preferably, the heating rate during calcining is 1~7 DEG C/min, preferably 1~5 DEG C/min.
9. lithium ion battery negative material prepared by a kind of any one of claim 1-8 methods described, its molecular formula is MoyOz, its
Middle y:Z=1:2~1:3.
10. lithium ion battery negative material according to claim 9, it is characterised in that the pattern of the negative material is
One or more kinds of combinations in sheet, banding, spherical, cube.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112299483A (en) * | 2020-10-29 | 2021-02-02 | 中国科学院过程工程研究所 | Nano molybdenum dioxide and preparation method and application thereof |
| CN112338198A (en) * | 2020-10-29 | 2021-02-09 | 中国科学院过程工程研究所 | Micron-sized molybdenum powder and preparation method and application thereof |
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