CN108321375A - A kind of in-situ doping type nanometer molybdenum base material, Preparation method and use - Google Patents
A kind of in-situ doping type nanometer molybdenum base material, Preparation method and use Download PDFInfo
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- CN108321375A CN108321375A CN201810117086.4A CN201810117086A CN108321375A CN 108321375 A CN108321375 A CN 108321375A CN 201810117086 A CN201810117086 A CN 201810117086A CN 108321375 A CN108321375 A CN 108321375A
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Abstract
The invention discloses a kind of in-situ doping type nanometer molybdenum base material, Preparation method and uses, belong to lithium ion battery preparation field, with 1,6 bis- (triazole) hexanes, ammonium heptamolybdate, manganese chloride, strontium chloride and phosphoric acid are starting material, and the phosphomolybdate material of the organic inorganic hybridization of manganese substitution has been synthesized by one kettle synthetic method of medium temperature hydro-thermal.Using the phosphomolybdate derivative of this modification as presoma, porous doped nano molybdenum-base composite material has successfully been made by high temperature sintering in nitrogen environment.The doping in situ of multiple element, improves the activity and stability of material surface, fundamentally improves chemical property.In addition, the porous nanostructure of coral shape that precursor process is formed realizes the regulation and control to molybdenum base material pattern, particle diameter distribution, specific surface area and tap density, and then improve performance of lithium ion battery.It is recycled 300 times under 500mA/g high current densities, the reversible capacity of lithium-ion capacitor battery remains above 95%.
Description
Technical field
The invention belongs to technical field of lithium ion, more particularly to prepared by a kind of in-situ doping type nanometer molybdenum base material
Method and purposes.
Background technology
Lithium ion battery is as clean energy resource of new generation, with small, storage energy is big, operating voltage is high, the cycle longevity
The remarkable advantages such as length, memory-less effect are ordered, are obtained in fields such as smart mobile phone, laptop, digital camera, electronic watches
It is widely applied.
Key component of the electrode material as lithium ion battery, cost occupy 50% or more of entire battery.At present to quotient
For lithium ion battery, graphite is common negative material, but the energy density of graphite and power density are relatively low, compared with
Low intercalation potential is also susceptible to safety problem, therefore develops a kind of high-energy density, and the negative material of high intercalation potential is
Very necessary.For graphite, transition metal oxide, tinbase, silicon based anode material are high due to its height ratio capacity
Current potential and abundant reserves cause the extensive concern of people in recent years.But volume will in removal lithium embedded for these negative materials
Big expansion and contraction occurs, big volume change can lead to the stress variation inside particle and cause breakage of particles and dusting,
Active material is peeled off from collector, and electrical contact is lost between active material and between active material and collector and causes to hold
Amount decaying.Because of the volume expansion of electrode material, stable solid electrolyte interface film can not be generated by making it in the electrolytic solution
(Solide Electrolyte Interface, SEI), electrolyte is constantly consumed in cyclic process forming new SEI layers causes
The cyclical stability of the low reversible capacity of electrode and difference.People use electrochemistry of a variety of strategies to such negative material thus
Performance is improved:(1) more spaces are obtained by nanosizing structure design, expand the stress brought with buffer volumes.Than
Such as:Hollow structure, porous structure, eggshell structure etc..(2) by buffering stress with other Material claddings flexible, such as with
Carbon, graphene, carbon nanotube etc. build compound.The progress of this field in recent years will be combined herein, to this kind of volume
It the structure design of intumescent lithium cell cathode material and prepares strategy and is illustrated.(3) by doping and surface cladding to existing
Material is modified and is modified, and using the synergistic effect of a variety of conductive materials, is prepared with amorphous or porous structure polynary
Composite material.But current strategy can only reach the mesh for improving material electrochemical performance by changing its pattern and particle diameter distribution
, it is difficult to control the amount of cladding and doping and the uniformity coefficient on surface, fundamentally regulate and control and improve the compatible of electrode material
Performance.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of in-situ doping type nanometer molybdenum base material, systems
Preparation Method and purposes.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of preparation method of in-situ doping type nanometer molybdenum base material, includes the following steps:
S1, with bis- (triazole) hexanes of 1,6-, ammonium heptamolybdate, manganese chloride, strontium chloride and phosphoric acid be starting material, made with water
For solvent, carry out being mixed and stirred for 60min, it is 3~4 to adjust pH value, obtains mixed liquor, wherein 1, the 6- is bis- (triazole)
Hexane, ammonium heptamolybdate, manganese chloride, strontium chloride, phosphoric acid and water molar ratio be 1:2:4:3:30:2000~2500;
S2, the mixed liquor that S1 is obtained is transferred in reaction kettle, is reacted at 160 DEG C 4~6 days, it is after reaction, natural
It is cooled to room temperature, obtains navy blue polyacid presoma;
S3, the presoma obtained in S2 is washed, filtering, drying, and in tube furnace under inert gas protection, in
600~700 DEG C of 6~8h of calcining, after calcining, cooled to room temperature obtains calcined product, and calcined product is then ground 30
~50min crosses 400 mesh sieve, obtains in-situ doping type nanometer molybdenum base lithium ion battery negative material.
The features of the present invention also characterized in that the inert gas in S3 is N2。
Another technical solution of the present invention is to provide a kind of in-situ doping type nanometer molybdenum base material that the above method is prepared
Material.
Another technical solution of the present invention is to provide a kind of above-mentioned in-situ doping type nanometer molybdenum base material as lithium-ion electric
The purposes of pond negative material.
The features of the present invention also characterized in that process of the in-situ doping type nanometer molybdenum base material as lithium ion battery negative material
Include the following steps:In-situ doping type nanometer molybdenum base material, conductive agent and binder are added in appropriate solvent and are uniformly mixed,
So that mixture is formed paste, is then applied on collector, in 80~120 DEG C of dry 6~12h, obtains negative electrode of lithium ion battery
Material, wherein the mass ratio of in-situ doping type nanometer molybdenum base material, conductive agent and binder is 8.0~9.5:0.2~1.0:
0.3~1.0.
The features of the present invention also characterized in that solvent is n-methyl-2-pyrrolidone (NMP).
The features of the present invention also characterized in that conductive agent is one or more of acetylene black, carbon nanotube, graphene group
It closes.
The features of the present invention also characterized in that binder is Kynoar.
The features of the present invention also characterized in that collector is one kind in copper foil, nickel foam.
The invention has the advantages and positive effects that:
The present invention has synthesized the phosphomolybdate material of the hybrid inorganic-organic of manganese substitution using one kettle synthetic method of medium temperature hydro-thermal
Material.Using the phosphomolybdate derivative of this modification as presoma, successfully it has been made porous by high temperature sintering in nitrogen environment
Doped nano molybdenum-base composite material.The doping in situ of multiple element, improves the activity and stability of material surface, from root
Chemical property is improved on this.In addition, uniform, the porous nanostructure that precursor process is formed is realized to molybdenum base material shape
The regulation and control of looks, particle diameter distribution, specific surface area and tap density, and then improve performance of lithium ion battery.By this doping in situ
Type nanometer molybdenum base material is assembled into the button cell of CR2025 models as lithium ion battery negative material, shows higher put
Electric specific capacity (1108mAh/g), high rate performance and good cycle performance, 300 are recycled under 500mA/g high current densities
Secondary, the capacity of lithium-ion capacitor battery remains above 95%.Its electrode performance is better than currently used electrode material.
Description of the drawings
Fig. 1 is that the SEM of in-situ doping type nanometer molybdenum base material schemes.
Fig. 2 be in-situ doping type nanometer molybdenum base material under 100mA/g current densities, the 10th time cycle charging and discharging curve
Figure.
Fig. 3 is multiplying power of the in-situ doping type nanometer molybdenum base material under 100,200,500,800,1000mA/g current densities
Performance map.
Fig. 4 is the cycle performance that in-situ doping type nanometer molybdenum base material recycles 300 times under 500mA/g high current densities
Figure.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, right with reference to the accompanying drawings and embodiments
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
In following embodiment, using prepared lithium ion battery negative material as working electrode, lithium piece is to electrode, 1M
LiPF6(1:1:Ethylene carbonate, dimethyl carbonate and the diethyl carbonate of 1 volume ratio are mixed solvent) it is electrolyte,
Celgard 2500 is diaphragm, is assembled into the button cell of CR2025 models, wherein the active material load of working electrode jointly
Amount is 1~3mg/cm-2。
Embodiment 1
A kind of in-situ doping type nanometer molybdenum base material provided in an embodiment of the present invention, preparation method specifically include following step
Suddenly:
S1, with bis- (triazole) hexanes of the 1,6- of 0.2200g, 2.4000g ammonium heptamolybdates, 0.6475g manganese chlorides,
0.7999g strontium chlorides and 2.00mL phosphoric acid are that starting material carries out being mixed and stirred for 60min using 36.00mL water as solvent,
It is 3 to adjust pH value with sodium hydroxide, obtains mixed liquor;
S2, the mixed liquor that S1 is obtained is transferred in reaction kettle, is reacted 4 days at 160 DEG C, it is after reaction, naturally cold
But to room temperature, precursor reagent crystal is obtained;
S3, the precursor reagent crystal obtained in S2 is washed, filtering, drying, and in N in tube furnace2Protection
Under, 8h is calcined in 600 DEG C, after calcining, cooled to room temperature obtains calcined product, and calcined product is then ground 30min,
400 mesh sieve is crossed, in-situ doping type nanometer molybdenum base material is obtained.
Process of the in-situ doping type nanometer molybdenum base material provided in an embodiment of the present invention as lithium ion battery negative material
Specifically comprise the following steps:By 480mg in-situ doping type nanometer molybdenum bases lithium ion battery negative material, 60mg acetylene blacks and 60mg
Kynoar is added in appropriate NMP, so that mixture is formed paste, is then applied on copper foil, in 80 DEG C of dry 12h, obtains
To lithium ion battery negative material.
Embodiment 2
A kind of in-situ doping type nanometer molybdenum base material provided in an embodiment of the present invention, preparation method specifically include following step
Suddenly:
S1, with bis- (triazole) hexanes of the 1,6- of 0.2200g, 2.4000g ammonium heptamolybdates, 0.6475g manganese chlorides,
0.7999g strontium chlorides and 2.00mL phosphoric acid are that starting material carries out being mixed and stirred for 60min using 40.50mL water as solvent,
It is 3.5 to adjust pH value with sodium hydroxide, obtains mixed liquor;
S2, the mixed liquor that S1 is obtained is transferred in reaction kettle, is reacted 5 days at 160 DEG C, it is after reaction, naturally cold
But to room temperature, reaction solution is obtained;
S3, the reaction solution obtained in S2 is washed, filtering, drying, and in N in tube furnace2Under protection, in 650 DEG C
7h is calcined, after calcining, cooled to room temperature obtains calcined product, and calcined product is then ground 40min, crosses 400 mesh sieve,
Obtain in-situ doping type nanometer molybdenum base material.
Process of the in-situ doping type nanometer molybdenum base material provided in an embodiment of the present invention as lithium ion battery negative material
Specifically comprise the following steps:By 510mg in-situ doping type nanometer molybdenum bases lithium ion battery negative material, 54mg acetylene blacks and 36mg
Kynoar is added in appropriate NMP, so that mixture is formed paste, is then applied on copper foil, in 100 DEG C of dry 10h, obtains
To lithium ion battery negative material.
Embodiment 3
A kind of in-situ doping type nanometer molybdenum base material provided in an embodiment of the present invention, preparation method specifically include following step
Suddenly:
S1, with bis- (triazole) hexanes of the 1,6- of 0.2200g, 2.4000g ammonium heptamolybdates, 0.6475g manganese chlorides,
0.7999g strontium chlorides and 2.00mL phosphoric acid are that starting material carries out being mixed and stirred for 60min using 45.00mL water as solvent,
It is 4 to adjust pH value with sodium hydroxide, obtains mixed liquor;
S2, the mixed liquor that S1 is obtained is transferred in reaction kettle, is reacted 6 days at 160 DEG C, it is after reaction, naturally cold
But to room temperature, reaction solution is obtained;
S3, the reaction solution obtained in S2 is washed, filtering, drying, and in N in tube furnace2Under protection, in 700 DEG C
6h is calcined, after calcining, cooled to room temperature obtains calcined product, and calcined product is then ground 50min, crosses 400 mesh sieve,
Obtain in-situ doping type nanometer molybdenum base material.
Process of the in-situ doping type nanometer molybdenum base material provided in an embodiment of the present invention as lithium ion battery negative material
Specifically comprise the following steps:By 540mg in-situ doping type nanometer molybdenum bases lithium ion battery negative material, 30mg acetylene blacks and 30mg
Kynoar is added in appropriate NMP, so that mixture is formed paste, is then applied on copper foil, in 120 DEG C of dry 6h, obtains
To lithium ion battery negative material.
In the specific embodiment of the invention, the pattern of material is characterized with scanning electron microscope (SEM), and passes through new prestige constant current charge and discharge
Electrical measurement test system carries out charge and discharge, the test of high rate performance and cycle performance, the potential range tested to the battery assembled
For 0.01-3.0V (vs.Li/Li+), test current density be 100,200,500,800,1000mA/g.
Fig. 1 a and Fig. 1 b are respectively SEM figure of the in-situ doping type nanometer molybdenum base material under different amplification, from Fig. 1 a
With as can be seen that the molybdenum base material after calcination has the three-dimensional porous surface topography of coralliform, significantly increase material in Fig. 1 b
Surface area so that it can realize the storage and release of a large amount of charges within the extremely short time.
Fig. 2 be in-situ doping type nanometer molybdenum base material under 100mA/g current densities, the 10th time cycle charging and discharging curve
Figure.From figure 2 it can be seen that the reversible capacity after the 10th cycle of in-situ doping type nanometer molybdenum base material is 1108mAh/g.
Fig. 3 is multiplying power of the in-situ doping type nanometer molybdenum base material under 100,200,500,800,1000mA/g current densities
Performance map.From figure 3, it can be seen that in-situ doping type nanometer molybdenum base material is 100,200,500,800,1000mA/g electric currents it is close
Corresponding reversible capacity under degree is respectively 1059,957,839,726,652mAh/g.
Fig. 4 is the cycle performance that in-situ doping type nanometer molybdenum base material recycles 300 times under 500mA/g high current densities
Figure.Figure 4, it is seen that in-situ doping type nanometer molybdenum base material, under 500mA/g high current densities, initial discharge capacity is
852mAh/g, after recycling 300 times, discharge capacity remains at 826mAh/g, and capacity retention ratio remains above 95%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (9)
1. a kind of preparation method of in-situ doping type nanometer molybdenum base material, which is characterized in that include the following steps:
S1, with bis- (triazole) hexanes of 1,6-, ammonium heptamolybdate, manganese chloride, strontium chloride and phosphoric acid for starting material, using water as molten
Agent be mixed and stirred for 60min, and it is 3~4 to adjust pH value, obtains mixed liquor, wherein bis- (triazole) hexanes of 1, the 6-,
Ammonium heptamolybdate, manganese chloride, strontium chloride, phosphoric acid and water molar ratio be 1:2:4:3:30:2000~2500;
S2, the mixed liquor that S1 is obtained is transferred in reaction kettle, 4~6 days, after reaction, natural cooling is reacted at 160 DEG C
To room temperature, navy blue polyacid presoma is obtained;
S3, the presoma obtained in S2 is washed, filtering, drying, and in tube furnace under inert gas protection, in 600
~700 DEG C calcining 6~8h, after calcining, cooled to room temperature obtains calcined product, then by calcined product grind 30~
50min crosses 400 mesh sieve, obtains in-situ doping type nanometer molybdenum base material.
2. a kind of preparation method of in-situ doping type nanometer molybdenum base material according to claim 1, which is characterized in that described
Inert gas in S3 is N2。
3. the in-situ doping type nanometer molybdenum base material that claim 1-2 any one of them methods are prepared.
4. purposes of the in-situ doping type nanometer molybdenum base material as lithium ion battery negative material described in claim 3.
5. purposes according to claim 4, which is characterized in that the in-situ doping type nanometer molybdenum base material is as lithium ion
The process of cell negative electrode material specifically comprises the following steps:In-situ doping type nanometer molybdenum base material, conductive agent and binder are added
Enter into appropriate solvent and be uniformly mixed, so that mixture is formed paste, be then applied on collector, in 80~120 DEG C dry 6~
12h obtains lithium ion battery negative material, wherein the in-situ doping type nanometer molybdenum base material, conductive agent and binder matter
Amount is than being 8.0~9.5:0.2~1.0:0.3~1.0.
6. purposes of the in-situ doping type nanometer molybdenum base material according to claim 5 as lithium ion battery negative material,
It is characterized in that, the solvent is n-methyl-2-pyrrolidone.
7. purposes of the in-situ doping type nanometer molybdenum base material according to claim 5 as lithium ion battery negative material,
It is characterized in that, the conductive agent is the combination of one or more of acetylene black, carbon nanotube, graphene.
8. purposes of the in-situ doping type nanometer molybdenum base material according to claim 5 as lithium ion battery negative material,
It is characterized in that, the binder is Kynoar.
9. purposes of the in-situ doping type nanometer molybdenum base material according to claim 5 as lithium ion battery negative material,
It is characterized in that, the collector is one kind in copper foil, nickel foam.
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US11869714B2 (en) | 2022-01-20 | 2024-01-09 | Imam Abdulrahman Bin Faisal University | Method for making a nanocomposite electrode and supercapacitor |
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