CN108417795A - A kind of preparation method of transition metal/transition metal carbodiimide composite material - Google Patents
A kind of preparation method of transition metal/transition metal carbodiimide composite material Download PDFInfo
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- CN108417795A CN108417795A CN201810124117.9A CN201810124117A CN108417795A CN 108417795 A CN108417795 A CN 108417795A CN 201810124117 A CN201810124117 A CN 201810124117A CN 108417795 A CN108417795 A CN 108417795A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/366—Composites as layered products
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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- H—ELECTRICITY
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- 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
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- H—ELECTRICITY
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- 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
Inorganic transition metal salt and carbon containing nitrogen organic compound are obtained mixture by a kind of preparation method of transition metal/transition metal carbodiimide composite material after grinding, the quality of inorganic transition metal salt and carbon containing nitrogen organic compound is 4 in mixture:1‑1:7;Under an argon atmosphere by mixture, 30 60min are kept the temperature in 100 170 DEG C, 1h 5h is then kept the temperature at 500 700 DEG C, obtain transition metal/transition metal carbodiimide composite material.Transition metal material structure and nitrogen-doped carbon prepared by the present invention is compound, can be obviously improved electric conductivity and structural stability of the material in charge and discharge process.Transition metal/transition metal carbodiimide composite material prepared by the present invention has high sodium ion storage performance, and charge/discharge capacity is high and high rate performance is splendid.
Description
Technical field
The invention belongs to composite materials to synthesize field, and in particular to a kind of transition metal/transition metal carbodiimide is compound
The preparation method of material.
Background technology
Since lithium ion battery has energy density high, service life is long, and advantages of environment protection, recent years become
Research hotspot, and it is successfully realized commercialization.But lithium resource is relatively low in the reserves of the earth, expensive become continues
Develop a bottleneck of lithium ion battery.Because there is an urgent need to find a kind of rich reserves, kin member usually replaces lithium
Element.Sodium and the element that lithium is same main group, and sodium is higher in the reserves of the earth, and it is widely distributed.Therefore big in recent years
The researcher of amount has put into a large amount of energy in the research of sodium-ion battery, and sodium-ion battery also achieves fast in recent years
The development of speed.However, sodium element differs larger with the radius of elemental lithium, therefore volume expansion becomes restriction sodium-ion battery development
A principal element.The oxide of iron have high power capacity, low cost, derive from a wealth of sources, it is nontoxic the advantages that, with existing graphite electricity
Pole is compared, and theoretical capacity is only 372mAhg-1, has significant advantage.Transition metal nitride is because of its low and flat charge and discharge
Potential plateau, high reversible response characteristic and capacity it is big the features such as, caused the extensive concern of scientific worker.Transition metal
Nitride is a kind of negative material for causing extensive concern.Carbon material usually has good electric conductivity and structural stability, therefore
It for other active materials frequently as one of composition of composite material through providing support.If can in the synthesis of FeN materials with carbon
Synchronous material progress is compound, then is expected to solve the problems, such as set forth above.Therefore, how while synthesizing FeN materials formed with
Its compound carbon material is an important research contents.Carbodiimide transition metal salt (MNCN, M are transition metal) is a kind of
Anode material of lithium-ion battery with high charge-discharge capacity potentiality, however the material is extremely severe due to being synthetically prepared condition requirement
It carves, it is more difficult to directly obtain the material, it is more difficult to obtain the composite construction of the material, thus significantly limit the application of the material.
If can one step of inventive technique directly to construct high conductivity material compound with it, to improve its electric conductivity, and by surface cladding come
Alleviate the volume expansion occurred when embedded sodium ion and abjection, is then expected to promote the material answering in battery electrode material field
With.
Invention content
The present invention is complicated for transition metal in the prior art/transition metal carbodiimide composite material synthesis step, closes
The problems such as higher at cost, it is therefore intended that propose a kind of preparation method of transition metal/transition metal carbodiimide composite material,
By carbon coating, it can effectively solve transition metal/transition metal carbodiimide volume expansion, while two kinds of materials are compounded in
The reactivity for also improving battery is further improved, battery structure is made more to stablize, to improve the multiplying power of battery and follow
Ring performance.
To achieve the above object, technical scheme is as follows:
A kind of preparation method of transition metal/transition metal carbodiimide composite material, includes the following steps:
1) by inorganic transition metal salt and carbon containing nitrogen organic compound, mixture is obtained after grinding, it is inorganic in mixture
The quality of transition metal salt and carbon containing nitrogen organic compound is 4:1-1:7;
2) 30-60min under an argon atmosphere by mixture, is kept the temperature in 100-170 DEG C, 1h- is then kept the temperature at 500-700 DEG C
5h obtains transition metal/transition metal carbodiimide composite material.
The present invention, which further improves, to be, inorganic transition metal salt is zinc salt, chromic salts, manganese salt or silver salt, wherein zinc salt
For arbitrary two kinds in zinc oxalate, zinc chloride, zinc acetate, zinc sulfate, chromic salts is arbitrary in chromic acetate, chromic nitrate, chromium chloride
Two kinds, manganese salt is arbitrary two kinds in manganese salicylate, manganese acetate, manganese oxalate, and silver salt is in silver formate, silver nitrate, silver acetate
Arbitrary two kinds.
The present invention, which further improves, to be, carbon containing nitrogen organic compound is urea, melamine, dicyandiamide, cyanamide, carbon
Diimine, cyanuric acid or trithiocyanuric acid.
The present invention, which further improves, to be, with the rate of 2-20 DEG C/min from room temperature to 100-170 DEG C.
The present invention, which further improves, to be, 500-700 is warming up to from 100-170 DEG C with the heating rate of 2-20 DEG C/min
℃。
The present invention, which further improves, to be, heat preservation carries out in tube furnace.
Compared with prior art, the device have the advantages that:
1) present invention is made using carbon containing nitrogen organic compound and transition metal organic acid, inorganic transition metal salt as raw material
Standby transition metal/transition metal carbodiimide composite material, the technology synthesis material is cheap, and preparation method is simple, can show
Writing reduces the manufacturing cost of transition metal/transition metal carbodiimide composite material in prior art.
2) the transition metal material structure prepared by the present invention and nitrogen-doped carbon are compound, can be obviously improved material in charge and discharge
Electric conductivity in the process and structural stability.
3) there is transition metal/transition metal carbodiimide composite material prepared by the present invention high sodium ion to store
Performance, charge/discharge capacity is high and high rate performance is splendid.
Description of the drawings
Fig. 1 is the XRD diagram of product prepared by embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of product prepared by embodiment 1.
Fig. 3 is the transmission electron microscope picture of product prepared by embodiment 1.
Fig. 4 is assembled into button cell for 1 resulting materials of embodiment and tests its anode material of lithium-ion battery performance map.
Fig. 5 is the XRD diagram of product prepared by embodiment 2.
Fig. 6 is the scanning electron microscope (SEM) photograph of product prepared by embodiment 2.
Fig. 7 is the transmission electron microscope picture of product prepared by embodiment 2.
Specific implementation mode
Present invention will now be described in detail with reference to the accompanying drawings..
1) take certain mass analytically pure inorganic transition metal salt (can be zinc salt, chromic salts, manganese salt or silver salt, wherein
Zinc salt is arbitrary two kinds in zinc oxalate, zinc chloride, zinc acetate, zinc sulfate, and chromic salts is in chromic acetate, chromic nitrate, chromium chloride
Arbitrary two kinds, manganese salt is arbitrary two kinds in manganese salicylate, manganese acetate, manganese oxalate, and silver salt is silver formate, silver nitrate, silver acetate
In arbitrary two kinds), organic compound raw material (can be urea, melamine, dicyandiamide, cyanamide, carbodiimide, trimerization
Cyanic acid, trithiocyanuric acid etc.), obtain mixture after mixed grinding in glass mortar, in mixture transition metal source with it is organic
The quality of compound is than range from 4:1-1:7, which is denoted as A;
2) product A is placed in quartz or alumina crucible, and crucible is placed in tube furnace, under an argon atmosphere, with -2-
The rate of 20 DEG C/min keeps the temperature 30-60min from room temperature to 100-170 DEG C, then proceedes to the heating of 2-20 DEG C/min
Rate continues to keep being warming up to 500-700 DEG C, and keeps the temperature 1h-5h, and products therefrom is transition metal/transition metal carbodiimide
Composite material.
Embodiment 1
1) analytically pure zinc oxalate, zinc sulfate and urea are fully ground in glass mortar and are formed uniformly mixture A,
Wherein zinc oxalate and zinc sulfate are respectively 2.0g, urea 2.0g;
2) mixture A from mortar is transferred to silica crucible, and silica crucible is placed in tube furnace, in argon gas atmosphere
Under, 170 DEG C are warming up to the rate of 25 DEG C/min, and keep the temperature 1.5h, then proceed to continue to keep with the heating rate of 2 DEG C/min
600 DEG C are warming up to, and keeps the temperature 1.5h, obtains product B.
Product B is analyzed using Rigaku D/max2000PCX- x ray diffractometer xs, the XRD of products therefrom is shown in attached drawing 1.It will
The sample is observed under scanning electron microscope and transmission electron microscope, as can be seen that shell-like structure, knot is presented in product from Fig. 2 and Fig. 3
Structure surface has more polyhedral structure.The product of gained is prepared into button-shaped lithium ion battery, specific encapsulation step
It is as follows:By activity powder, conductive agent (Super P), bonding agent (carboxyl methyl cellulose) is 8 according to mass ratio:1:1 proportioning
After grinding uniformly, slurry is made, equably slurry is applied on copper foil with coating device, then in 80 DEG C of dryings of vacuum drying chamber
12h.Electrode slice is assembled into sodium ion half-cell later, constant current charge-discharge survey is carried out to battery using new prestige electrochemical workstation
Resulting materials are assembled into button cell and test its anode material of lithium-ion battery by examination, test voltage 0.01V-3.0V
Can, as shown in figure 4, battery presents the capacity of 700mAh/g under the current density of 100mA/g, under the current density of 5A/g
The still capacity with 300mAh/g or more, it is seen that material has excellent high rate performance and charge/discharge capacity.
Embodiment 2
1) analytically pure chromic acetate, chromium chloride and melamine are fully ground in glass mortar and are formed uniformly mixing
Object A, wherein chromic acetate 1g, chromium chloride 1g, melamine 2g;
2) mixture A from mortar is transferred to silica crucible, and silica crucible is placed in tube furnace, in argon gas atmosphere
Under, 200 DEG C are warming up to the rate of 25 DEG C/min, and keep the temperature 10min, then proceed to the heating rate with 3 DEG C/min after continuation of insurance
It holds and is warming up to 700 DEG C, and keep the temperature 1h, obtain product B.
Product B is analyzed using Rigaku D/max2000PCX- x ray diffractometer xs, the XRD of products therefrom is shown in attached drawing 5.It will
The sample is observed under scanning electron microscope and transmission electron microscope, it can be seen from figures 6 and 7 that the multi-panel of accumulation is presented in product
Body structure and polyhedron are grown on the carbon shell structure surface of thin layer.
Embodiment 3
1) it by inorganic transition metal salt and carbon containing nitrogen organic compound, is fully ground uniformly, obtains in glass mortar
Mixture, the quality of inorganic transition metal salt and carbon containing nitrogen organic compound is 4 in mixture:1;Wherein, inorganic transition metal
Salt is the mixture of silver formate and silver nitrate.Carbon containing nitrogen organic compound is melamine.
2) mixture is transferred to silica crucible from mortar, and silica crucible is placed in tube furnace, in argon gas atmosphere
Under, 60min to 100 DEG C and is kept the temperature from room temperature with the rate of 2 DEG C/min, then proceedes to the heating rate liter with 2 DEG C/min
Temperature is to 500 DEG C and keeps the temperature 5h, obtains transition metal/transition metal carbodiimide composite material.
Embodiment 4
1) it by inorganic transition metal salt and carbon containing nitrogen organic compound, is fully ground uniformly, obtains in glass mortar
Mixture, the quality of inorganic transition metal salt and carbon containing nitrogen organic compound is 1 in mixture:7;Wherein, inorganic transition metal
Salt is the mixture of chromic acetate and chromic nitrate.Carbon containing nitrogen organic compound is dicyandiamide.
2) mixture is transferred to silica crucible from mortar, and silica crucible is placed in tube furnace, in argon gas atmosphere
Under, 50min to 120 DEG C and is kept the temperature from room temperature with the rate of 5 DEG C/min, then proceedes to the heating rate liter with 5 DEG C/min
Temperature is to 700 DEG C and keeps the temperature 1h, obtains transition metal/transition metal carbodiimide composite material.
Embodiment 5
1) it by inorganic transition metal salt and carbon containing nitrogen organic compound, is fully ground uniformly, obtains in glass mortar
Mixture, the quality of inorganic transition metal salt and carbon containing nitrogen organic compound is 2 in mixture:1;Wherein, inorganic transition metal
Salt is the mixture of manganese salicylate and manganese oxalate.Carbon containing nitrogen organic compound is carbodiimide.
2) mixture is transferred to silica crucible from mortar, and silica crucible is placed in tube furnace, in argon gas atmosphere
Under, 40min to 160 DEG C and is kept the temperature from room temperature with the rate of 8 DEG C/min, then proceedes to the heating rate liter with 13 DEG C/min
Temperature is to 600 DEG C and keeps the temperature 3h, obtains transition metal/transition metal carbodiimide composite material.
Embodiment 6
1) it by inorganic transition metal salt and carbon containing nitrogen organic compound, is fully ground uniformly, obtains in glass mortar
Mixture, the quality of inorganic transition metal salt and carbon containing nitrogen organic compound is 20 in mixture:7;Wherein, inorganic transition metal
Salt is the mixture of zinc sulfate and zinc acetate.Carbon containing nitrogen organic compound is cyanuric acid.
2) mixture is transferred to silica crucible from mortar, and silica crucible is placed in tube furnace, in argon gas atmosphere
Under, 40min to 150 DEG C and is kept the temperature from room temperature with the rate of 10 DEG C/min, is then proceeded to the heating rate of 17 DEG C/min
It is warming up to 550 DEG C and keeps the temperature 4h, obtain transition metal/transition metal carbodiimide composite material.
Embodiment 7
1) it by inorganic transition metal salt and carbon containing nitrogen organic compound, is fully ground uniformly, obtains in glass mortar
Mixture, the quality of inorganic transition metal salt and carbon containing nitrogen organic compound is 5 in mixture:7;Wherein, inorganic transition metal
Salt is the mixture of manganese acetate and manganese oxalate.Carbon containing nitrogen organic compound is trithiocyanuric acid.
2) mixture is transferred to silica crucible from mortar, and silica crucible is placed in tube furnace, in argon gas atmosphere
Under, 45min to 140 DEG C and is kept the temperature from room temperature with the rate of 15 DEG C/min, is then proceeded to the heating rate of 20 DEG C/min
It is warming up to 650 DEG C and keeps the temperature 2h, obtain transition metal/transition metal carbodiimide composite material.
Embodiment 8
1) it by inorganic transition metal salt and carbon containing nitrogen organic compound, is fully ground uniformly, obtains in glass mortar
Mixture, the quality of inorganic transition metal salt and carbon containing nitrogen organic compound is 24 in mixture:7;Wherein, inorganic transition metal
Salt is the mixture of silver formate and silver acetate.Carbon containing nitrogen organic compound is cyanamide.
2) mixture is transferred to silica crucible from mortar, and silica crucible is placed in tube furnace, in argon gas atmosphere
Under, 30min to 170 DEG C and is kept the temperature from room temperature with the rate of 20 DEG C/min, is then proceeded to the heating rate of 10 DEG C/min
It is warming up to 700 DEG C and keeps the temperature 1h, obtain transition metal/transition metal carbodiimide composite material.
Claims (6)
1. a kind of preparation method of transition metal/transition metal carbodiimide composite material, which is characterized in that including following step
Suddenly:
1) by inorganic transition metal salt and carbon containing nitrogen organic compound, mixture is obtained after grinding, inorganic transition in mixture
The quality of metal salt and carbon containing nitrogen organic compound is 4:1-1:7;
2) 30-60min under an argon atmosphere by mixture, is kept the temperature in 100-170 DEG C, 1h-5h is then kept the temperature at 500-700 DEG C,
Obtain transition metal/transition metal carbodiimide composite material.
2. a kind of preparation method of transition metal according to claim 1/transition metal carbodiimide composite material, special
Sign is, inorganic transition metal salt is zinc salt, chromic salts, manganese salt or silver salt, wherein zinc salt be zinc oxalate, zinc chloride, zinc acetate,
Arbitrary two kinds in zinc sulfate, chromic salts is arbitrary two kinds in chromic acetate, chromic nitrate, chromium chloride, and manganese salt is manganese salicylate, acetic acid
Arbitrary two kinds in manganese, manganese oxalate, silver salt is arbitrary two kinds in silver formate, silver nitrate, silver acetate.
3. a kind of preparation method of transition metal according to claim 1/transition metal carbodiimide composite material, special
Sign is that carbon containing nitrogen organic compound is urea, melamine, dicyandiamide, cyanamide, carbodiimide, cyanuric acid or three polysulfides
Cyanic acid.
4. a kind of preparation method of transition metal according to claim 1/transition metal carbodiimide composite material, special
Sign is, with the rate of 2-20 DEG C/min from room temperature to 100-170 DEG C.
5. a kind of preparation method of transition metal according to claim 1/transition metal carbodiimide composite material, special
Sign is, 500-700 DEG C is warming up to from 100-170 DEG C with the heating rate of 2-20 DEG C/min.
6. a kind of preparation method of transition metal according to claim 1/transition metal carbodiimide composite material, special
Sign is that heat preservation carries out in tube furnace.
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CN109817935A (en) * | 2019-01-31 | 2019-05-28 | 陕西科技大学 | A kind of compound iron carbodiimide cell negative electrode material and preparation method thereof |
CN111129456A (en) * | 2019-12-18 | 2020-05-08 | 西安工业大学 | Co-doped FeNCN/C and preparation method and application thereof |
CN113023785A (en) * | 2021-02-25 | 2021-06-25 | 陕西科技大学 | Iron-carbon diimine nano material based on dense growth of carbon cloth and preparation method and application thereof |
CN113224303A (en) * | 2021-05-08 | 2021-08-06 | 陕西科技大学 | Preparation method of iron cyanamide material for realizing graphitized carbon coating by in-situ autocatalysis |
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CN113224303A (en) * | 2021-05-08 | 2021-08-06 | 陕西科技大学 | Preparation method of iron cyanamide material for realizing graphitized carbon coating by in-situ autocatalysis |
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