CN106450305B - A kind of preparation method of lithium ion battery negative material CoP/C - Google Patents
A kind of preparation method of lithium ion battery negative material CoP/C 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
- H01M4/58—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
- H01M4/5805—Phosphides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/362—Composites
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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
- H01M4/58—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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 present invention is to provide the preparation methods of lithium ion battery negative material CoP/C a kind of.Biomass is put into cobalt salt solution and is impregnated, is dried for 24 hours at 50 °C, and is put into the calcining of tube furnace high temperature, argon gas protection is led in calcination process, obtains product A；Product A is ground, is placed in oxalic acid solution, heating water bath, obtained solution is centrifuged repeatedly cleaning, until pH value is neutrality, outwells supernatant, retains precipitating, and dry 12h, obtains product B at a temperature of being deposited in 60 DEG C；Two porcelain boats for being respectively provided with sodium hypophosphite and product B are located next to be placed in tube furnace, the high-temperature calcination under the protection of argon gas.For the present invention using biomass as carbon source, the CoP/C nanocomposite structural stability of preparation is good, and the volume expansion of CoP in charge and discharge process can be effectively relieved, and avoids volume expansion and efficiency for charge-discharge is caused to reduce and the too fast problem of capacity attenuation.
Description
Technical field
The present invention relates to a kind of preparation methods of lithium ion battery negative material.Specifically one kind, which is related to one kind, has
The preparation method of the lithium ion battery negative material CoP/C of excellent cycling performance.
Background technique
With the fast development of global economy, energy crisis and environmental problem have become this century mankind must face two
Big severe challenge, high performance Green Chemistry power supply is just in the important research of novel energy-storing material and field of energy conversion
Hold.Lithium ion battery energy density is high, small in size, light-weight, has extended cycle life, memory-less effect, self-discharge rate is low, Er Qiegong
It is wide to make temperature range, it is environmental-friendly, it is rare environmentally protective secondary power supply.
In recent years the study found that 3d transition metal phosphide not only theoretical capacity with higher, has preferable electricity
Subconductivity and lesser degree of polarization, and the volume expansion of metal phosphide is small, it is relatively low to lithium reaction potential, therefore be
A kind of novel very promising high performance lithium ionic cell cathode material.However, transition metal phosphide
Remain the problems such as preparation is difficult, cycle performance is bad.
The nanosizing and Composite of negative electrode material are to improve the conventional means of its cyclical stability.Electrode material nanosizing band
The advantage come can be summarized as follows: (1) nanostructure has big specific surface, increases the contact area of electrode and electrolyte,
The number of active sites for increasing electrode reaction reduces electrode polarization loss, to improve high rate performance and energy efficiency.
(2) electrode material of nano-scale can shorten the transportation route of electronics transportation route and lithium ion, meanwhile, nano material is at it
Also more ions and electronic defects are had in body phase, this can also promote the ion of material and electronics conduction.It is hereby achieved that
Fast mass transfer and high power density.(3) mechanical strength and structural intergrity of material are promoted.Low-dimension nano material includes receiving
Rice noodles, their bulk of the ratio such as nanometer rods and nanobelt have the ability of higher mechanical strength and the loss of higher resistance to mechanical, from
And a degree of volume change can be tolerated in certain dimensions.Composite refer to nano material is dispersed in it is certain
In matrix, the mechanical stress that active material generates in charge and discharge process is absorbed using basis material, rock-steady structure inhibits powder
Change, to improve cycle performance.Most commonly compound with carbon, on the one hand, carbon material has good ductility, is coated on
Nano grain surface or be dispersed in around it can play a buffer role in, and material dusting is inhibited simultaneously to prevent from reuniting.On the other hand, carbon has
There is excellent electric conductivity, the electric conductivity of composite material can be greatly improved.
The method of existing synthesis transition metal phosphide has the disadvantage in that a), there are height in prior synthesizing method
The defect that energy consumption, program are complicated, raw material toxicity is big, this cuts the advantage of transition metal phosphide substitution noble metal significantly
It is weak.B), in hydrothermal/solvent thermal method synthesis process, need to consume a large amount of phosphorus source, and the transition metal phosphide Chang Youtuan generated
Poly- phenomenon, granular size are tens nanometer (or even micron), and component dispersion degree is low.C), direct smelting process needs higher temperature,
And a large amount of excessive elemental phosphorous (because volatilizations of phosphorus simple substance) is needed, obtained product crystal phase mixes and is difficult to control.Therefore it opens
Sending out simple and easy method a kind of, there is the negative electrode material of good circulation performance to be of great significance for preparation.
Summary of the invention
The purpose of the present invention is to provide a kind of simple processes, can obtain the lithium ion battery with excellent cycling performance
The preparation method of negative electrode material CoP/C.
The object of the present invention is achieved like this:
Biomass is put into cobalt salt solution and impregnates by step 1, dries for 24 hours at 50 °C, and be put into tube furnace
High-temperature calcination leads to argon gas protection in calcination process, obtains product A；
Product A is ground, is placed in oxalic acid solution by step 2, and heating water bath, obtained solution is centrifuged repeatedly cleaning, directly
It is neutrality to pH value, outwells supernatant, retain precipitating, dry 12h, obtains product B at a temperature of being deposited in 60 DEG C；
Step 3, by two porcelain boats for being respectively provided with sodium hypophosphite and product B next to being placed in tube furnace, in argon gas
Protection under high-temperature calcination, obtain final product CoP/C nanocomposite.
The present invention may also include:
1, cobalt salt solution is cobalt nitrate, cobalt chloride or cobaltous sulfate, and concentration is 0.05~0.2mol/L.
2, the calcination time of high-temperature calcination described in step 1 is 60~180min, and calcination temperature is 600~1100 DEG C.
3, the temperature of water-bath described in step 2 is 20~80 DEG C, and the heating water bath time is 2~5h.
4, product B and the mass ratio of sodium hypophosphite are 1:1~10.
5, the calcination time of high-temperature calcination described in step 3 is 60~180min, and calcination temperature is 300~600 DEG C.
6, the biomass is Hericium erinaceus, sawdust, agaric or catkin.
The present invention provides a kind of preparation method of transition metal phosphide composite material for negative electrode of lithium ion battery,
Cumbersome, the bad problem of cycle performance is prepared to solve existing pure phase transition metal phosphide.
Compared with prior art, the present invention have it is following the utility model has the advantages that
(1) preparation provided by the invention has the method for the transition metal phosphide of good pattern, required primary raw material
Abundance, cheap, cost is relatively low；And the CoP pattern of preparation is preferable, shows nanorod shape.
(2) for the present invention using biomass as carbon source, the CoP/C nanocomposite structural stability of preparation is good, can
The volume expansion of CoP in charge and discharge process is effectively relieved, avoids volume expansion and leads to efficiency for charge-discharge reduction and capacity attenuation
Too fast problem.
Detailed description of the invention
Fig. 1: CoP/C nanocomposite XRD diagram prepared by embodiment 1.
Fig. 2 (a)-Fig. 2 (b): CoP/C nanocomposite SEM figure prepared by embodiment 1, in which: 1000 times of Fig. 2 (a),
Figure
2 (b) 5000 times.
Fig. 3: the high rate performance figure of CoP/C nanocomposite prepared by embodiment 1 under different current densities.
Fig. 4: CoP/C nanocomposite prepared by embodiment 1 is 1000mAg in current density-1Under charge and discharge specific volume
Amount and corresponding coulombic efficiency.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment 1
The cobalt nitrate for weighing 8.7309g is dissolved in 200ml deionized water, and suitable Hericium erinaceus is put in cobalt nitrate solution and is soaked
Bubble for 24 hours, is put into air dry oven, and drying for 24 hours, is placed in tube furnace, under Ar atmosphere, with 5 DEG C of min at 50 DEG C-1Liter
Warm rate rises to 850 DEG C, constant temperature 90min, grinds after natural cooling, and 45 DEG C of heating water baths in 0.3mol/L oxalic acid solution,
It is centrifuged repeatedly cleaning, until pH is neutrality, supernatant is outwelled, retains precipitating, 60 DEG C of dry 12h, obtain in air dry oven
Presoma and sodium hypophosphite 1:5 in mass ratio are respectively put into two adjacent porcelain boats, are placed in tube furnace by CoP presoma,
With 10 DEG C of min-1Heating rate rise to 400 DEG C, constant temperature 150min, the nano combined material of product CoP/C is obtained after natural cooling
Material.
Physicochemical property is carried out to prepared CoP/C nanocomposite using X-ray diffractometer, scanning electron microscope
Characterization, the result is shown in Figure 1, Fig. 2 (a)-Fig. 2 (b) carry out electrochemistry to prepared CoP/C nanocomposite assembled battery
It can test, as a result see Fig. 3 and Fig. 4.
Fig. 1 is the XRD diagram of resulting materials, and the material that reference standard card can be seen that synthesis is the CoP of standard.Fig. 2
(a)-Fig. 2 (b) is the scanning electron microscope (SEM) photograph of the present embodiment CoP/C, and the amplification factor of Fig. 2 (b) is 5000 times.It can from figure
Out, the CoP material synthesized is tens nanometers of diameter, a length of a few micrometers of nanometer rods.Fig. 3 is the nano combined material of CoP/C
Expect high rate performance figure under different current densities, electrochemical property test be shown in current density be 50,100,200,500,
1000、2000、5000mAg-1Under charge-discharge velocity, their average discharge capacity can also remain 486,384,298,238,
182、145、97mAhg-1, when current density is from 1000mAg-1Come back to 50mAg-1When, average discharge capacity also reaches
340mAhg-1, keep the 70% of original charge/discharge capacity.It in current density is 1000mAg that Fig. 4, which is CoP/C nanocomposite,-1
When cycle performance figure, by 1000 circle circulation after, capacity remains 153.6mAhg-1, keep the 98% of existing capacity.
Embodiment 2
The cobalt nitrate for weighing 8.7309g is dissolved in 200ml deionized water, and suitable dried fungus is put in cobalt nitrate solution and is soaked
Bubble for 24 hours, is then placed in air dry oven, and drying for 24 hours, is placed in tube furnace, under Ar atmosphere, with 5 DEG C of min at 50 DEG C-1's
Heating rate rises to 850 DEG C, constant temperature 90min, takes out and grinds after cooling, and 45 DEG C of water-baths add in 0.3mol/L oxalic acid solution
Heat is centrifuged repeatedly cleaning, until pH is neutrality, outwells supernatant, retains precipitating, 60 DEG C of dry 12h, obtain in air dry oven
To CoP presoma, presoma and sodium hypophosphite 1:5 in mass ratio are respectively put into two adjacent porcelain boats, tube furnace is placed in
In, with 10 DEG C of min-1Heating rate rise to 400 DEG C, constant temperature 150min, it is nano combined to obtain product CoP/C after natural cooling
Material.
It is 50,100,200,500,1000,2000,5000mAg that electrochemical property test, which is shown in current density,-1Charge and discharge
Under rate, their average discharge capacity can also remain 465,357,278,204,158,129,78mAhg-1, work as current density
From 1000mAg-1Come back to 50mAg-1When, average discharge capacity has also reached 321mAhg-1, keep original charge/discharge capacity
70%.CoP/C nanocomposite is 1000mAg in current density-1When current density under, by 1000 circle circulation it
Afterwards, capacity remains 144mAhg-1, keep the 91% of existing capacity.
Embodiment 3
The cobalt chloride for weighing 7.1379g is dissolved in 200ml deionized water, and suitable Hericium erinaceus is put in cobalt chloride solution and is soaked
Bubble for 24 hours, is then placed in air dry oven, and drying for 24 hours, is placed in tube furnace, under Ar atmosphere, with 5 DEG C of min at 50 DEG C-1's
Heating rate rises to 850 DEG C, constant temperature 90min, takes out and grinds after cooling, and 45 DEG C of water-baths add in 0.3mol/L oxalic acid solution
Heat is centrifuged repeatedly cleaning, until pH is neutrality, outwells supernatant, retains precipitating, 60 DEG C of dry 12h, obtain in air dry oven
To CoP presoma, presoma and sodium hypophosphite 1:5 in mass ratio are put into different porcelain boats, are placed in tube furnace, with 10
℃·min-1Heating rate rise to 400 DEG C, constant temperature 150min, product CoP/C nanocomposite is obtained after natural cooling.
It is 50,100,200,500,1000,2000,5000mAg that electrochemical property test, which is shown in current density,-1Charge and discharge
Under rate, their average discharge capacity can also remain 445,346,258,194,142,116,71mAhg-1, work as current density
From 1000mAg-1Come back to 50mAg-1When, average discharge capacity has also reached 343mAhg-1, keep original charge/discharge capacity
77%.CoP/C nanocomposite is 1000mAg in current density-1When current density under, by 1000 circle circulation it
Afterwards, capacity remains 121mAhg-1, keep the 85% of existing capacity.
Embodiment 4
The cobalt nitrate for weighing 3.5682g is dissolved in 200ml deionized water, and suitable catkin is put in cobalt nitrate solution and is impregnated
For 24 hours, it is then placed in air dry oven, drying for 24 hours, is placed in tube furnace, under Ar atmosphere, with 5 DEG C of min at 50 DEG C-1Liter
Warm rate rises to 850 DEG C, constant temperature 90min, takes out and grinds after cooling, and 45 DEG C of heating water baths in 0.3mol/L oxalic acid solution,
It is centrifuged repeatedly cleaning, until pH is neutrality, supernatant is outwelled, retains precipitating, 60 DEG C of dry 12h, obtain in air dry oven
Presoma and sodium hypophosphite 1:5 in mass ratio are put into different porcelain boats, are placed in tube furnace, with 10 DEG C by CoP presoma
min-1Heating rate rise to 400 DEG C, constant temperature 150min, product CoP/C nanocomposite is obtained after natural cooling.
It is 50,100,200,500,1000,2000,5000mAg that electrochemical property test, which is shown in current density,-1Charge and discharge
Under rate, their average discharge capacity can also remain 439,353,256,189,143,114,76mAhg-1, work as current density
From 1000mAg-1Come back to 50mAg-1When, average discharge capacity has also reached 313mAhg-1, keep original charge/discharge capacity
71%.CoP/C nanocomposite is 1000mAg in current density-1When current density under, by 1000 circle circulation it
Afterwards, capacity remains 109mAhg-1, keep the 76% of existing capacity.
Claims (7)
1. a kind of preparation method of lithium ion battery negative material CoP/C, it is characterized in that:
Biomass is put into cobalt salt solution and impregnates by step 1, at 50 °C it is dry for 24 hours, and be put into tube furnace,
600~1100 DEG C of high-temperature calcinings, argon gas protection is led in calcination process, obtains product A；
Product A is ground, is placed in oxalic acid solution by step 2, and heating water bath, obtained solution is centrifuged repeatedly cleaning, until pH
Value is neutrality, outwells supernatant, retains precipitating, and dry 12h, obtains product B at a temperature of being deposited in 60 DEG C；
Step 3, by two porcelain boats for being respectively provided with sodium hypophosphite and product B next to being placed in tube furnace, in the guarantor of argon gas
It protects, high-temperature calcination at a temperature of 300~600 DEG C, obtains final product CoP/C nanocomposite.
2. the preparation method of lithium ion battery negative material CoP/C according to claim 1, it is characterized in that: cobalt salt solution
For cobalt nitrate, cobalt chloride or cobaltous sulfate, concentration is 0.05~0.2mol/L.
3. the preparation method of lithium ion battery negative material CoP/C according to claim 1, it is characterized in that: in step 1
The calcination time of the high-temperature calcination is 60~180min.
4. the preparation method of lithium ion battery negative material CoP/C according to claim 1, it is characterized in that: in step 2
The temperature of the water-bath is 20~80 DEG C, and the heating water bath time is 2~5h.
5. the preparation method of lithium ion battery negative material CoP/C according to claim 1, it is characterized in that: product B and time
The mass ratio of sodium phosphite is 1:1~10.
6. the preparation method of lithium ion battery negative material CoP/C according to claim 1, it is characterized in that: in step 3
The calcination time of the high-temperature calcination is 60~180min.
7. the preparation method of lithium ion battery negative material CoP/C according to claim 1, it is characterized in that: the biology
Matter is sawdust or catkin.
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| CN107275639B (en) * | 2017-06-30 | 2019-11-26 | 武汉理工大学 | The CoP/C classifying nano line and its preparation method and application of nano particle assembling |
| CN109273676B (en) * | 2018-08-16 | 2020-08-18 | 浙江大学 | Sulfur-mould spore carbon sphere/phosphide composite material and preparation method and application thereof |
| CN109378540B (en) * | 2018-09-18 | 2020-08-21 | 余姚市鑫和电池材料有限公司 | Preparation method of high-purity ternary precursor |
| CN109411842B (en) * | 2018-09-18 | 2020-10-20 | 余姚市鑫和电池材料有限公司 | Environment-friendly preparation method of ternary precursor |
| CN114300676B (en) * | 2021-11-01 | 2023-07-18 | 北京航空航天大学 | Flexible sodium ion battery negative electrode material, preparation method thereof and battery negative electrode |
| CN114284496B (en) * | 2021-11-16 | 2023-07-25 | 石家庄科林电气股份有限公司 | Preparation method of three-dimensional large-framework multi-stage structure electrode material |
| CN114335516B (en) * | 2021-12-28 | 2023-06-13 | 哈尔滨工程大学 | Synthesis method of carbon-limited mesoporous Kong Liu flocculent tin phosphorus sulfide composite nano-structure material |
| CN115141031B (en) * | 2022-05-18 | 2023-07-04 | 安徽大学 | Electromagnetic wave absorption composite material and preparation method and application thereof |
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