CN106910891A - A kind of transition metal fluorides load the preparation method of boron dopen Nano carbon composite - Google Patents
A kind of transition metal fluorides load the preparation method of boron dopen Nano carbon composite Download PDFInfo
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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 belongs to technical field of nano material, and in particular to a kind of transition metal fluorides load the preparation method of boron dopen Nano carbon material.The inventive method, by ball milling and heating, can be prepared by transition metal fluorides load boron dopen Nano carbon composite using transition metal fluorides, boron hydride and nano-carbon material as raw material.The method has low cost, and high efficiency is economic and environment-friendly, the features such as universality is strong.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of transition metal fluorides load boron dopen Nano carbon
The preparation method of composite.
Background technology
Lithium ion battery has the advantages that energy density is high, has extended cycle life, high conversion efficiency, is widely used in electronic
Automobile, intelligent grid etc. are efficiently in energy-storage system.The positive/negative material of the lithium ion battery of current business is slotting insert-type（Example
Such as：Graphite cathode；LiCoO2Positive pole）.The theoretical specific capacity of these slotting insert-type positive and negative pole materials is relatively low（The theoretical ratio of graphite cathode
Capacity is only：375mAh g-1,LiCoO2The theoretical specific capacity of positive pole is only：140mAh g-1）, seriously constrain lithium ion battery
Energy density.[1,2] therefore, develop height ratio capacity positive/negative material be improve lithium ion battery energy density key.
In recent years, a series of researchs show transition metal fluorides（For example: FeF3、FeF2、NiF2、CoF3、CoF2、
NiF3、MnF2、CuF2、TiF4Deng）Big with specific capacity, energy density is high, is that a class is very potential the features such as cheap pollution-free
Lithium ion battery positive/negative material.[3-8] wherein, positive electrode is with FeF3To represent, its theoretical specific capacity is up to 712
mAh g-1, average working voltage is 2.74 V, and energy density is up to 1951 Wh kg-1；[4,8-10] negative material is with MnF2For
Represent, its theoretical specific capacity is up to 577mAh g-1, operating voltage is 0.8 V.[11,12] are however, transition metal fluorides exist
Poorly conductive is there is in de-/process of intercalation, Volume Changes are big, the problems such as voltage delay is serious, causes its capacity to be decayed rapidly,
Cyclical stability is poor.[4,11] research workers have carried out a series of research work for these problems.Among this,
The pre- embedding lithium of transition metal fluorides is changed into transition metal/lithium fluoride, and further compound with nano-carbon material is general at present
All over use solution, for example：After the Fe/LiF/ graphene composite materials prepared using ball milling pyrolysismethod are circulated at 180
150 mAh g can still be kept-1Specific capacity.[13] lifting of transition metal fluorides removal lithium embedded performance is attributed to：First, build
The Volume Changes in its cyclic process can effectively be alleviated in carbon complex system, and strengthen system electric conductivity；Secondly, FeF after pre- embedding lithium3
Directly full battery, MnF can be constituted Deng positive electrode without cathode of lithium with graphite, silicon etc.2Deng head of the negative material after pre- embedding lithium
Secondary coulombic efficiency is also significantly improved.Constructing transition metal/lithium fluoride/nano carbon composite material has significant advantage above, still
Deposit following deficiency：
（1）Long circulating performance is still difficult to meet practical application request, in addition it is also necessary to the carbon materials further adulterated by introducing hetero-atoms
Material improves its cycle performance [14]；
（2）The preparation of transition metal/lithium fluoride/nano carbon composite material is typically by spraying, and ball milling pyrolysis reduction, chemistry is heavy
Product, the method such as hydro-thermal realizes that preparation cost is high, and efficiency is low, is unfavorable for industrialized production, and it is difficult it is synchronous realize it is heteroatomic uniform
Doping [15,16]；
（3）Existing preparation method is generally used and is first loaded on the carrier of nano-carbon material lithium fluoride and transition metal respectively,
Cause to be difficult to combine closely between lithium fluoride and transition metal nanoparticles, increased in charging process intermediate ion/atoms permeating
Distance, has a strong impact on the degree of reversibility [13] of de-/embedding lithium electrochemical reaction.
Therefore, a kind of carbon material by lithium fluoride and transition metal nanoparticles synchronized loading to Heteroatom doping is developed,
And have inexpensive and efficient preparation method concurrently and have very important significance.
Bibliography
[1] Croguennec, L.; Palacin, M. R. J. Am. Chem. Soc. 2015,137, 3140.
[2] Goodenough, J. B.; Kim, Y. Chem. Mater. 2010,22, 587.
[3] Li, H.; Richter, G.; Maier, J. Adv. Mater. 2003,15, 736.
[4]Li, H.; Balaya, P.; Maier, J. J. Electrochem. Soc. 2004,151, 1878.
[5]Amatucci, G. G.; Pereira, N. J. Fluorine Chem. 2007,128, 243.
[6]Teng, Y. T.; Pramana, S. S.; Ding, J.; Wu, T.; Yazami, R. Electrochim. Acta 2013,107, 301.
[7]Hua, X.; Robert, R.; Du, L. S.; Wiaderek, K. M.; Leskes, M.; Chapman,
K. W.; Chupas, P. J.; Grey, C. P. J. Phys. Chem. C 2014,118, 15169.
[8]Wang, F.; Robert, R.; Chernova, N. A.; Pereira, N.; Omenya, F.;
Badway, F.; Hua, X.; Ruotolo, M.; Zhang, R.; Wu, L.; Volkov, V.; Su, D.; Key,
B.; Whittingham, M. S.; Grey, C. P.; Amatucci, G. G.; Zhu, Y.; Graetz, J. J. Am. Chem. Soc. 2011,133, 18828.
[9]Liu, P.; Vajo, J. J.; Wang, J. S.; Li, W.; Liu, J. J. Phys. Chem. C
2012,116, 6467.
[10]Ma, D. L.; Cao, Z. Y.; Wang, H. G.; Huang, X. L.; Wang, L. M.; Zhang,
X. B. Energy Environ. Sci. 2012,5, 8538.
[11]Rui, K.; Wen, Z.; Lu, Y.; Jin, J.; Shen, C. Adv. Energy Mater. 2015,5, 1401716.
[12]Rui, K.; Wen, Z.; Huang, X.; Lu, Y.; Jin, J.; Shen, C. Phys. Chem. Chem. Phys. 2016,18, 3780.
[13]Ma, R.; Dong, Y.; Xi, L.; Yang, S.; Lu, Z.; Chung, C. ACS Appl. Mater. Interfaces 2013,5, 892.
[14]Kumagae, K.; Okazaki, K.; Matsui, K.; Horino, H.; Hirai, T.; Yamaki,
J.; Ogumi, Z. J. Electrochem. Soc. 2016,163, 1633.
[15]Sun, Y.; Liu, N.; Cui, Y. Nature Energy 2016,1, 16071.
[16] Rui, K.; Wen, Z.; Lu, Y.; Shen, C.; Jin, J. ACS Appl. Mater. Interfaces 2016,8, 1819.。
The content of the invention
It is an object of the invention to provide the preparation that a kind of transition metal fluorides load boron dopen Nano carbon composite
Method, makes transition metal and the nano particle of lithium fluoride be dispersed in combining closely on nano-carbon material matrix, and can be synchronously real
Existing boron doping.The method has low cost, and efficiency high is economic and environment-friendly, the features such as universality is strong.
The transition metal fluorides that the present invention is provided load the preparation method of boron dopen Nano carbon composite, specific steps
It is as follows：
（1）By transition metal fluorides, boron hydride（LiBH4）, nano-carbon material be added in ball grinder, transition metal fluorination
Thing and LiBH4Molar ratio be 1:1~1:4, the quality of nano-carbon material accounts for oeverall quality ratio for 5wt%~80wt%, is protecting
Ball milling 2~48 hours under shield atmosphere；
It is preferred that transition metal fluorides and LiBH4Molar ratio be 1:1~1:2.5, the quality of nano-carbon material accounts for total constitution
Than being 5wt%~40wt%, Ball-milling Time is 20~48 hours to amount；
（2）Ball milling product is heated to 120~500 DEG C under the conditions of dynamic vacuum, and is incubated 1~48 hour, be then cooled to
Room temperature, collects product, obtains final product transition metal fluorides load boron dopen Nano carbon composite.
It is preferred that heating-up temperature is 320~400 DEG C, soaking time is 30~45 hours.
Step（1）In, described transition metal fluorides are FeF3、FeF2、NiF2、NiF3、CoF3、CoF2、MnF2、CuF2、
TiF4、ZnF2In any one, it is or therein several.Described nano-carbon material be graphite, Graphene, SWCN,
Any one in multi-walled carbon nano-tubes, carbon nano rod, carbon fiber, carbon nanocoils, carbon nanometer rod, it is or therein several.It is described
Protective atmosphere be any one in hydrogen, nitrogen, argon gas, helium.
Step（2）In, described transition metal is any one in Fe, Ti, Ni, Co, Cu, Mn, Zn, or therein several
Kind.
The good effect of the inventive method is：
（1）This method is simple to operate, required ball milling and vacuum degasser, is industrial common production equipment, it is required most
High-temperature is only 500 DEG C, therefore this method efficiency high, can be applied to large-scale industrial production；
（2）This method preparation process is without waste liquid/thing discharge, and required transition metal fluorides, lithium borohydride and nano carbon material
Material is industrial common raw materials, therefore this method is economic and environment-friendly, low production cost；
（3）This method can prepare various transition metal fluorides load boron dopen Nano carbon such as Mn, Fe, Ti, Ni, Co, Cu, Zn and answer
Condensation material, lithium fluoride and transition metal are dispersed in nano-sized carbon with combining closely with form of nanoparticles in the composite
On carrier, and the content of doped chemical boron, pattern and distribution etc. can further be regulated and controled according to preparation condition.
Brief description of the drawings
Fig. 1 is the X ray diffracting spectrum of synthesized boron doped Mn/LiF/ graphite composite materials.
Fig. 2 is the high power transmission electron microscope image of synthesized boron doped Mn/LiF/ graphite composite materials.
Fig. 3 is the embedding de- lithium performance of circulation of synthesized boron doped Mn/LiF/ graphite composite materials.
Fig. 4 is the scanning electron microscope image of synthesized boron doped Fe/LiF/ graphite composite materials.
Fig. 5 is the X-ray energy distribution collection of illustrative plates of synthesized boron doped Fe/LiF/ graphite composite materials.
Specific embodiment
Preparation method of the invention is described in detail with accompanying drawing below in conjunction with example.
Embodiment 1：The preparation of boron doped Mn/LiF/ graphite composite materials and its electrochemical lithium storage characteristic
In inert atmosphere glove box, by 0.465g MnF2、0.22 g LiBH4Load ball milling with the mixing of 0.2 g powdered graphites
In tank, the h of ball milling 24 in a hydrogen atmosphere, rotational speed of ball-mill is 400 revs/min, and ratio of grinding media to material is 30:1.Ball milling product is persistently taken out
Vacuum, and it is gradually heating to 140 DEG C, room temperature is down to naturally after 12 h of insulation, can obtain boron doped Mn/LiF/ graphite and be combined
Material.The X ray diffracting spectrum and high power transmission electron microscope figure of synthesized boron doped Mn/LiF/ graphite composite materials
As difference as illustrated in fig. 1 and 2.Fig. 1 shows that the method is successfully prepared LiF.The nano particle of visible Mn and boron is dispersed in Fig. 2
On amorphous graphite layer.Illustrate that the method can both prepare transition metal/lithium fluoride/Nano Carbon material with reference to Fig. 1 and Fig. 2
Material, can synchronously realize that boron adulterates again.Fig. 3 gives the long circulating of prepared boron doped Mn/LiF/ graphite composite materials
Performance.In 1 A g-1Current density under, by 1500 circulation, synthesized boron doped Mn/LiF/ graphite composite materials
The 423 mAh g that can still keep-1Specific capacity, illustrate the method prepare boron doped Mn/LiF/ graphite composite materials tool
There is excellent cycle performance.
Embodiment 2：The preparation of boron doped Fe/LiF/ graphite composite materials
In inert atmosphere glove box, by 0.47 g FeF2、0.25 g LiBH4Load ball milling with the mixing of 0.15 g powdered graphites
In tank, the h of ball milling 48 under an argon atmosphere, rotational speed of ball-mill is 400 revs/min, and ratio of grinding media to material is 40:1.Ball milling product is persistently taken out
Vacuum, and it is gradually heating to 450 DEG C, room temperature is down to naturally after 12 h of insulation, can obtain boron doped Fe/LiF/ graphite and be combined
Material.Fig. 4 and Fig. 5 sets forth prepared boron doped Fe/LiF/ graphite composite materials SEM and
Its corresponding X-ray energy distribution collection of illustrative plates.The granular size of visible prepared Fe/Li/ graphite composite materials is 50 in Fig. 4
Nm or so.Clearly visible B, C, F, Fe element in Fig. 5, illustrates that the method can prepare Fe/LiF/ graphite composite materials, and synchronous real
Existing boron doping.
Embodiment 3：The preparation of boron doped Ni/LiF/ graphene composite materials
In inert atmosphere glove box, by 0.485 g NiF2、0.32 g LiBH4Load ball with the mixing of 0.1 g graphene powders
In grinding jar, the h of ball milling 6 in a nitrogen atmosphere, rotational speed of ball-mill is 350 revs/min, and ratio of grinding media to material is 40:1.Ball milling product is persistently taken out
Vacuum, and it is gradually heating to 350 DEG C, room temperature is down to naturally after 6 h of insulation, can obtain boron doped Ni/LiF/ Graphenes and be combined
Material.
Embodiment 4：The preparation of boron doped Co/LiF/ multi-wall carbon nano-tube composite materials
In inert atmosphere glove box, by 0.485 g CoF2、0.25 g LiBH4Mix with 0.2 g multi-wall carbon nano-tubes pipe powder
It is fitted into ball grinder, in a hydrogen atmosphere the h of ball milling 4, rotational speed of ball-mill is 300 revs/min, and ratio of grinding media to material is 30:1.By ball milling product
Persistently vacuumize, and be gradually heating to 500 DEG C, room temperature is down to naturally after 10 h of insulation, can obtain many walls of boron doped Co/LiF/
Carbon nano tube compound material.
Embodiment 5：The preparation of boron doped Mn/LiF/ SWCNs composite
In inert atmosphere glove box, by 0.47 g MnF2With 0.3 g LiBH4Mix with 0.25 g singles pipe powder
It is fitted into ball grinder, in a hydrogen atmosphere the h of ball milling 36, rotational speed of ball-mill is 300 revs/min, and ratio of grinding media to material is 40:1.Ball milling is produced
Thing is persistently vacuumized, and is gradually heating to 280 DEG C, and room temperature is down to naturally after 12 h of insulation, can obtain boron doped Mn/LiF/
SWCN composite.
Claims (3)
1. a kind of transition metal fluorides load the preparation method of boron dopen Nano carbon composite, comprise the following steps that：
（1）By transition metal fluorides, LiBH4, nano-carbon material be added in ball grinder, transition metal fluorides and LiBH4's
Molar ratio is 1:1~1：4, the quality of nano-carbon material accounts for oeverall quality ratio for 5wt%~80wt%, the ball milling under protective atmosphere
2~48 hours；
（2）Ball milling product is heated to 120~500 DEG C under the conditions of dynamic vacuum, and is incubated 1~48 hour, be then cooled to
Room temperature, collects product, obtains final product transition metal fluorides load boron dopen Nano carbon composite.
2. the preparation method according to claim, it is characterised in that step（1）In, described transition metal fluorides are
FeF3、FeF2、NiF2、NiF3、CoF3、CoF2、MnF2、CuF2、TiF4、ZnF2In any one, it is or therein several；It is described
Nano-carbon material for graphite, Graphene, SWCN, multi-walled carbon nano-tubes, carbon nano rod, carbon fiber, carbon nanocoils,
Any one in carbon nanometer rod, it is or therein several；Described protective atmosphere is any in hydrogen, nitrogen, argon gas, helium
It is a kind of.
3. the preparation method according to claim, it is characterised in that step（2）In, described transition metal is Fe, Ti,
Any one in Ni, Co, Cu, Mn, Zn, or it is therein several.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109148831A (en) * | 2018-09-11 | 2019-01-04 | 安徽工业大学 | A kind of preparation method of fluoride sodium ion battery electrode material |
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| WD01 | Invention patent application deemed withdrawn after publication |