CN106450305A - Preparation method of lithium ion battery cathode material CoP/C - Google Patents
Preparation method of lithium ion battery cathode 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 invention provides a preparation method of a lithium ion battery cathode material CoP/C. The preparation method includes the steps: soaking biomass in cobalt salt solution, drying for 24 hours at the temperature of 50 DEG C, calcining in a tubular furnace at high temperature, and leading into argon to protect in the calcining process to obtain a product A; crushing the product A, placing the crushed product A into oxalic acid solution, performing water-bath heating to obtain solution, repeatedly and centrifugally cleaning until a pH (potential of hydrogen) value is neutral, pouring away supernatant liquid, reserving sedimentation, and drying the sedimentation for 12 hours at the temperature of 60 DEG C to obtain a product B; closely placing two porcelain boats respectively filled with sodium hypophosphite and the product B in the tubular furnace, and calcining at high temperature under protection of the argon. According to the preparation method, the biomass serves as carbon sources, the prepared CoP/C nano-composite material is good in structural stability, CoP volume expansion in the charge and discharge process can be effectively relieved, and the method solves the problems that charge and discharge efficiency is reduced as volume expands, and capacity are rapidly reduced.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery negative material.Specifically one kind is related to one kind and has
The preparation method of the lithium ion battery negative material CoP/C of excellent cycling performance.
Background technology
With the fast development of global economy, energy crisis and environmental problem have become two that this century mankind must face
Big severe challenge, high performance Green Chemistry power supply has just become in novel energy-storing material and the important research of field of energy conversion
Hold.Lithium ion battery energy density is high, and small volume is lightweight, has extended cycle life, memory-less effect, and self-discharge rate is low, Er Qiegong
Make temperature range width, environmental friendliness, be rare environmental protection secondary power supply.
Research in recent years finds, 3d transition metal phosphide not only has higher theoretical capacity, has preferable electricity
Electronic conductivity and less degree of polarization, and the volumetric expansion of metal phosphide is little, relatively low to lithium reaction potential, be therefore
A kind of new high performance lithium ionic cell cathode material having very much application prospect.However, transition metal phosphide
Remain that preparation is difficult, the problems such as cycle performance is good.
The nanorize of negative material and Composite are the conventional means improving its cyclical stability.Electrode material nanorize band
The advantage come can be summarized as follows：(1) nanostructured has big specific surface, increased the contact area of electrode and electrolyte,
Increased the number of active sites of electrode reaction, decreasing electrode polarization loss, thus 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, and meanwhile, nano material is at it
Also more ions and electronic defects is had, this ion that also can lift material and electronics conduct in body phase.It is hereby achieved that
Fast mass transfer and high power density.(3) mechanical strength of lifting material and structural intergrity.Low-dimension nano material includes receiving
Rice noodle, their bulk of ratio such as nanometer rods and nano belt has the ability of the resistance to mechanical loss of higher mechanical strength and Geng Gao, from
And a certain degree of change in volume can be tolerated on some dimensions.Composite refers to be dispersed in nano material certain
In matrix, the mechanical stress that produced in charge and discharge process using matrix material absorbing activity material, rock-steady structure, suppresses powder
Change, thus improving cycle performance.It is most commonly that compound with carbon, on the one hand, material with carbon element has good ductility, is coated on
Nano grain surface or be dispersed in and can play cushioning effect about, suppression material efflorescence simultaneously prevents from reuniting.On the other hand, carbon tool
There is excellent electric conductivity, the electric conductivity of composite can be greatly improved.
The method of existing synthesis transition metal phosphide suffers from the drawback that：A), there are height in prior synthesizing method
The defect that energy consumption, program are complicated, raw material toxicity is big, this makes the advantage that transition metal phosphide substitutes noble metal significantly cut
Weak.B), in hydrothermal/solvent full-boiled process building-up process, need to consume substantial amounts of phosphorus source, and the transition metal phosphide generating often has group
Poly- phenomenon, granular size is tens nanometer (or even micron), and component dispersion is low.C), direct smelting process needs higher temperature,
And needing elemental phosphorous (because volatilization of phosphorus simple substance) excessive in a large number, the product crystalline phase obtaining mixes and wayward.Therefore open
The negative material that preparation of sending out simple and easy method a kind of has good circulation performance is significant.
Content of the invention
It is an object of the invention to provide a kind of process is simple, the lithium ion battery with excellent cycling performance can be obtained
The preparation method of negative material CoP/C.
The object of the present invention is achieved like this：
Step one, biomass is put in cobalt salt solution and soaks, 24h is dried, and puts in tube furnace at a temperature of 50 DEG C
High-temperature calcination, in calcination process, logical argon protection, obtains product A；
Step 2, product A is ground, is placed in oxalic acid solution, heating in water bath, the solution obtaining is centrifuged repeatedly cleaning, directly
It is neutrality to pH value, outwells supernatant, retain precipitation, 12h is dried at a temperature of being deposited in 60 DEG C, obtains product B；
Step 3, two porcelain boats being respectively provided with sodium hypophosphite and product B is close to and is placed in tube furnace, in argon
Protection under high-temperature calcination, obtain final product CoP/C nano composite material.
The present invention can also include：
1st, cobalt salt solution is cobalt nitrate, cobaltous chloride or cobaltous sulfate, and concentration is 0.05～0.2mol/L.
2nd, the calcination time of high-temperature calcination described in step one is 60～180min, and calcining heat is 600～1100 DEG C.
3rd, the temperature of water-bath described in step 2 is 20～80 DEG C, and the heating in water bath time is 2～5h.
4th, the mass ratio of product B and sodium hypophosphite is 1:1～10.
5th, the calcination time of high-temperature calcination described in step 3 is 60～180min, and calcining heat is 300～600 DEG C.
6th, described biomass are Hericium erinaceus (Bull. Ex Fr.) Pers., wood flour, Auricularia or Semen Salicis babylonicae cum piluss.
The invention provides a kind of preparation method of the transition metal phosphide composite for lithium ion battery negative,
Prepare loaded down with trivial details, the not good problem of cycle performance to solve existing pure phase transition metal phosphide.
Compared with prior art, the present invention has following beneficial effect：
(1) method that the preparation that the present invention provides has the transition metal phosphide of good pattern, required primary raw material
Abundance, cheap, cost is relatively low；And the CoP pattern prepared is preferably, presents nanorod shape.
(2), by the use of biomass as carbon source, the CoP/C nano composite material structural stability of preparation is good, can for the present invention
Effectively alleviate the volumetric expansion of CoP in charge and discharge process, it is to avoid volumetric expansion and lead to efficiency for charge-discharge to reduce and capacity attenuation
Too fast problem.
Brief description
Fig. 1：The CoP/C nano composite material XRD figure of embodiment 1 preparation.
Fig. 2 (a)-Fig. 2 (b)：The CoP/C nano composite material SEM figure of embodiment 1 preparation, wherein：1000 times of Fig. 2 (a),
Figure
5000 times of 2 (b).
Fig. 3：High rate performance figure under different electric current densities for the CoP/C nano composite material of embodiment 1 preparation.
Fig. 4：The CoP/C nano composite material of embodiment 1 preparation is 1000mAg in electric current density-1Under discharge and recharge specific volume
Amount and corresponding coulombic efficiency.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this area
For personnel, without departing from the inventive concept of the premise, some deformation can also be made and improve.These broadly fall into the present invention
Protection domain.
Embodiment 1
The cobalt nitrate weighing 8.7309g is dissolved in 200ml deionized water, and appropriate Hericium erinaceus (Bull. Ex Fr.) Pers. is put leaching in cobalt nitrate solution
Bubble 24h, puts in air dry oven, 24h is dried at 50 DEG C, be placed in tube furnace, under Ar atmosphere, with 5 DEG C of min-1Liter
Warm speed rises to 850 DEG C, constant temperature 90min, grinds after natural cooling, and 45 DEG C of heating in water bath in 0.3mol/L oxalic acid solution,
It is centrifuged repeatedly cleaning, until pH is neutrality, outwell supernatant, retain precipitation, 60 DEG C are dried 12h in air dry oven, obtain
CoP presoma, by presoma and sodium hypophosphite in mass ratio 1:5 are respectively put in two adjacent porcelain boats, are placed in tube furnace,
With 10 DEG C of min-1Heating rate rise to 400 DEG C, constant temperature 150min, obtain the nano combined material of product CoP/C after natural cooling
Material.
Using X-ray diffractometer, scanning electron microscope, physicochemical property is carried out to prepared CoP/C nano composite material
Characterize, result is shown in Fig. 1, Fig. 2 (a)-Fig. 2 (b), carries out electrochemistry to prepared CoP/C nano composite material assembled battery
Can test, result is shown in Fig. 3 and Fig. 4.
Fig. 1 is the XRD figure 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, the amplification of Fig. 2 (b) is 5000 times.Can from figure
Go out, synthesize the CoP material obtaining and be tens nanometers of diameter, the nanometer rods of a length of a few micrometers.Fig. 3 is the nano combined material of CoP/C
High rate performance figure under different electric current densities for the material, electrochemical property test be shown in electric 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 electric 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.Fig. 4 is 1000mAg for CoP/C nano composite material in electric current density-1
When cycle performance figure, through 1000 circle circulations after, capacity remains 153.6mAhg-1, keep the 98% of existing capacity.
Embodiment 2
The cobalt nitrate weighing 8.7309g is dissolved in 200ml deionized water, and appropriate dried Auricularia is put leaching in cobalt nitrate solution
Bubble 24h, is then placed in air dry oven, 24h is dried at 50 DEG C, be placed in tube furnace, under Ar atmosphere, with 5 DEG C of min-1's
Heating rate rises to 850 DEG C, constant temperature 90min, takes out and grinds, and 45 DEG C of water-baths add in 0.3mol/L oxalic acid solution after cooling
Heat, is centrifuged repeatedly cleaning, until pH is neutrality, outwells supernatant, retains precipitation, 60 DEG C are dried 12h in air dry oven, obtain
To CoP presoma, by presoma and sodium hypophosphite in mass ratio 1:5 are respectively put in two adjacent porcelain boats, are placed in tube furnace
In, with 10 DEG C of min-1Heating rate rise to 400 DEG C, constant temperature 150min, obtain product CoP/C after natural cooling nano combined
Material.
Electrochemical property test be shown in electric current density be 50,100,200,500,1000,2000,5000mAg-1Discharge and recharge
Under speed, their average discharge capacity can also remain 465,357,278,204,158,129,78mAhg-1, work as electric 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 nano composite material is 1000mAg in electric current density-1When electric current density under, through 1000 circle circulations it
Afterwards, capacity remains 144mAhg-1, keep the 91% of existing capacity.
Embodiment 3
The cobaltous chloride weighing 7.1379g is dissolved in 200ml deionized water, and appropriate Hericium erinaceus (Bull. Ex Fr.) Pers. is put leaching in cobalt chloride solution
Bubble 24h, is then placed in air dry oven, 24h is dried at 50 DEG C, be placed in tube furnace, under Ar atmosphere, with 5 DEG C of min-1's
Heating rate rises to 850 DEG C, constant temperature 90min, takes out and grinds, and 45 DEG C of water-baths add in 0.3mol/L oxalic acid solution after cooling
Heat, is centrifuged repeatedly cleaning, until pH is neutrality, outwells supernatant, retains precipitation, 60 DEG C are dried 12h in air dry oven, obtain
To CoP presoma, by presoma and sodium hypophosphite in mass ratio 1:5 put in different porcelain boats, are placed in tube furnace, with 10
℃·min-1Heating rate rise to 400 DEG C, constant temperature 150min, obtain product CoP/C nano composite material after natural cooling.
Electrochemical property test be shown in electric current density be 50,100,200,500,1000,2000,5000mAg-1Discharge and recharge
Under speed, their average discharge capacity can also remain 445,346,258,194,142,116,71mAhg-1, work as electric 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 nano composite material is 1000mAg in electric current density-1When electric current density under, through 1000 circle circulations it
Afterwards, capacity remains 121mAhg-1, keep the 85% of existing capacity.
Embodiment 4
The cobalt nitrate weighing 3.5682g is dissolved in 200ml deionized water, appropriate Semen Salicis babylonicae cum piluss is put in cobalt nitrate solution and soaks
24h, is then placed in air dry oven, 24h is dried at 50 DEG C, is placed in tube furnace, under Ar atmosphere, with 5 DEG C of min-1Liter
Warm speed rises to 850 DEG C, constant temperature 90min, takes out and grind after cooling, and 45 DEG C of heating in water bath in 0.3mol/L oxalic acid solution,
It is centrifuged repeatedly cleaning, until pH is neutrality, outwell supernatant, retain precipitation, 60 DEG C are dried 12h in air dry oven, obtain
CoP presoma, by presoma and sodium hypophosphite in mass ratio 1:5 put in different porcelain boats, are placed in tube furnace, with 10 DEG C
min-1Heating rate rise to 400 DEG C, constant temperature 150min, obtain product CoP/C nano composite material after natural cooling.
Electrochemical property test be shown in electric current density be 50,100,200,500,1000,2000,5000mAg-1Discharge and recharge
Under speed, their average discharge capacity can also remain 439,353,256,189,143,114,76mAhg-1, work as electric 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 nano composite material is 1000mAg in electric current density-1When electric current density under, through 1000 circle circulations 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, is characterized in that：
Step one, biomass is put in cobalt salt solution and soaks, 24h is dried, and puts into tube furnace high temperature at a temperature of 50 DEG C
Calcining, in calcination process, logical argon protection, obtains product A；
Step 2, product A is ground, is placed in oxalic acid solution, heating in water bath, the solution obtaining is centrifuged repeatedly cleaning, until pH
It is worth for neutrality, outwells supernatant, retain precipitation, 12h is dried at a temperature of being deposited in 60 DEG C, obtains product B；
Step 3, two porcelain boats being respectively provided with sodium hypophosphite and product B is close to and is placed in tube furnace, in the guarantor of argon
The lower high-temperature calcination of shield, obtains final product CoP/C nano composite material.
2. the preparation method of lithium ion battery negative material CoP/C according to claim 1, is characterized in that：Cobalt salt solution
For cobalt nitrate, cobaltous 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, is characterized in that：In step
The calcination time of described high-temperature calcination is 60～180min, and calcining heat is 600～1100 DEG C.
4. the preparation method of lithium ion battery negative material CoP/C according to claim 1, is characterized in that：In step 2
The temperature of described water-bath is 20～80 DEG C, and the heating in water bath time is 2～5h.
5. the preparation method of lithium ion battery negative material CoP/C according to claim 1, is characterized in that：Product B with 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, is characterized in that：In step 3
The calcination time of described high-temperature calcination is 60～180min, and calcining heat is 300～600 DEG C.
7. the preparation method of lithium ion battery negative material CoP/C according to claim 1, is characterized in that：Described biology
Matter is Hericium erinaceus (Bull. Ex Fr.) Pers., wood flour, Auricularia or Semen Salicis babylonicae cum piluss.
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| CN107275639A (en) * | 2017-06-30 | 2017-10-20 | 武汉理工大学 | CoP/C classifying nano lines of nano particle assembling and its preparation method and application |
| CN109273676A (en) * | 2018-08-16 | 2019-01-25 | 浙江大学 | A kind of sulphur-mycotic spore carbon ball/phosphide composite material and preparation method and application |
| CN109378540A (en) * | 2018-09-18 | 2019-02-22 | 余姚市鑫和电池材料有限公司 | A kind of preparation method of high-purity ternary precursor |
| CN109411842A (en) * | 2018-09-18 | 2019-03-01 | 余姚市鑫和电池材料有限公司 | A kind of environment-friendly preparation method of ternary precursor |
| CN114284496A (en) * | 2021-11-16 | 2022-04-05 | 石家庄科林电气股份有限公司 | Preparation method of three-dimensional large-framework multi-level structure electrode material |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN107275639A (en) * | 2017-06-30 | 2017-10-20 | 武汉理工大学 | CoP/C classifying nano lines of nano particle assembling and its preparation method and application |
| CN109273676A (en) * | 2018-08-16 | 2019-01-25 | 浙江大学 | A kind of sulphur-mycotic spore carbon ball/phosphide composite material and preparation method and application |
| 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 |
| CN109411842A (en) * | 2018-09-18 | 2019-03-01 | 余姚市鑫和电池材料有限公司 | A kind of environment-friendly preparation method of ternary precursor |
| 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 |
| CN109378540A (en) * | 2018-09-18 | 2019-02-22 | 余姚市鑫和电池材料有限公司 | A kind of preparation method of high-purity ternary precursor |
| CN114300676A (en) * | 2021-11-01 | 2022-04-08 | 北京航空航天大学 | Flexible sodium-ion battery negative electrode material, preparation method thereof and battery negative electrode |
| CN114284496A (en) * | 2021-11-16 | 2022-04-05 | 石家庄科林电气股份有限公司 | Preparation method of three-dimensional large-framework multi-level structure electrode material |
| 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 |
| CN114335516A (en) * | 2021-12-28 | 2022-04-12 | 哈尔滨工程大学 | Synthesis method of carbon-confined mesoporous catkin-like phosphorus tin sulfide composite nano-structure 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 |
| CN115141031A (en) * | 2022-05-18 | 2022-10-04 | 安徽大学 | Electromagnetic wave absorption composite material and preparation method and application thereof |
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