CN109817935A - A kind of compound iron carbodiimide cell negative electrode material and preparation method thereof - Google Patents
A kind of compound iron carbodiimide cell negative electrode material and preparation method thereof Download PDFInfo
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- CN109817935A CN109817935A CN201910099432.5A CN201910099432A CN109817935A CN 109817935 A CN109817935 A CN 109817935A CN 201910099432 A CN201910099432 A CN 201910099432A CN 109817935 A CN109817935 A CN 109817935A
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Abstract
The invention discloses a kind of compound iron carbodiimide cell negative electrode materials and preparation method thereof, this method uses solvent-thermal method to carry out confinement energy first by source of iron and carbon source, carbon is set effectively to be coated on molysite surface, molysite is set to be converted into FeNCN by solid phase reaction again, to obtain carbon compound iron carbodiimide material;The carbon compound iron carbodiimide cell negative electrode material as made from this method, it is made of iron carbodiimide and carbon-coating, because the outside of iron carbodiimide is coated with carbon-coating, so that the negative electrode material is in sodium-ion battery use process, iron carbodiimide is limited by carbon-coating and is difficult to generate big volume change, effectively solve the problems, such as transition metal carbodiimide volume expansion, and then promote electric conductivity and structural stability of the material in charge and discharge process, enhance the reactivity of battery, so that the material has excellent sodium ion storage performance, charge/discharge capacity is high and high rate performance is good.
Description
[technical field]
The invention belongs to composite materials to synthesize field, and in particular to a kind of compound iron carbodiimide cell negative electrode material and its
Preparation method.
[background technique]
Lithium ion battery is existing frequently-used battery, but lithium resource is relatively low in the reserves of the earth, it is expensive at
To continue to develop a bottleneck of lithium ion battery.Because kin member is usually there is an urgent need to find a kind of rich reserves
Replace elemental lithium.Sodium and lithium are the element of same main group, and sodium is higher in the reserves of the earth, and widely distributed.Due to sodium ion
Battery has energy density high, and long service life, advantages of environment protection becomes research hotspot recent years, and successfully
Realize commercialization.A large amount of researcher has put into a large amount of energy in the research of sodium-ion battery in recent years, sodium from
Sub- battery also achieves rapid development in recent years.
However, sodium element differs larger with the radius of elemental lithium, therefore volume expansion becomes restriction sodium-ion battery development
A principal element.Transition metal diimine compounds are because of the reaction of its low and flat charge and discharge potential platform, high reversible
The features such as characteristic and capacity are big, has caused the extensive concern of scientific worker.
Carbodiimide transition metal salt (MNCN, M are transition metal) be a kind of sodium with high charge-discharge capacity potentiality from
Sub- cell negative electrode material, however the material requires extremely harshness due to being synthetically prepared condition, it is more difficult to directly obtain the material, it more difficult to
To obtain the composite construction of the material, thus significantly limit the application of the material.Carbon material usually have good electric conductivity and
Structural stability, therefore its warp provides support frequently as one of composition of composite material for other active materials.If can be in FeNCN
Synthesis in it is synchronous with carbon material carry out it is compound, then be expected to solve the problems, such as set forth above.Therefore, how synthesis FeNCN's
Being formed simultaneously the carbon material compound with it is an important research contents.
[summary of the invention]
It is an object of the invention to overcome the above-mentioned prior art, a kind of compound iron carbodiimide battery cathode is provided
Material and preparation method thereof.This method can be effectively by carbon coating in surface by confinement preparation, then cooperates carbon material compound
The problem of then can effectively solve transition metal carbodiimide volume expansion simultaneously enhances its electric conductivity, and the reaction for enhancing battery is living
Property, keep battery structure more stable, to improve the multiplying power and cycle performance of battery.
In order to achieve the above objectives, the present invention is achieved by the following scheme:
A kind of preparation method of carbon compound iron carbodiimide cell negative electrode material, comprising the following steps:
Step 1, after source of iron and carbon source being mixed according to mass ratio 1:(1-2), mixture A is limited by hot solvent method
Process product B will be made after reaction product centrifugation, drying in domain synthetic reaction;
Step 2, process product B and urea generate carbon compound iron carbodiimide cell negative electrode material by solid phase reaction,
Chemical structural formula is FeNCN@C.
A further improvement of the present invention is that:
Preferably, the step of hot solvent method are as follows: mixture A and ethyl alcohol proportionally (2-3) g:(50-70) mL is mixed
It is being reacted into reactor after conjunction, reaction temperature is 200 DEG C, reaction time 12-36h.
Preferably, source of iron is organic acid molysite or inorganic transition metal salt, and organic acid molysite includes ironic citrate, oxalic acid
Iron, ferric formate and ferric acetate;Inorganic transition metal salt includes iron chloride, ferric nitrate and ferric sulfate.
Preferably, carbon source is any one of sucrose, chitosan, glucose, melamine or ammonium oxalate.
Preferably, in step 1, centrifugal rotational speed 8000r/min is centrifuged 3-6 times, and each centrifugation time is 3-8min.
Preferably, in step 1, the centrifugation product drying temperature after reaction product centrifugation is 60-80 DEG C.
Preferably, in step 2, process product B and urea is mixed according to mass ratio 1:(1.5-3) and carry out solid phase reaction.
Preferably, in step 2, the temperature of solid phase reaction is 300~600 DEG C.
A kind of carbon compound iron carbodiimide cell negative electrode material prepared by preparation method described in above-mentioned any one,
Iron carbodiimide surface recombination has a carbon-coating, the carbon-coating with a thickness of 70-500nm.
Compared with prior art, the invention has the following advantages:
The invention discloses a kind of preparation method of carbon compound iron carbodiimide cell negative electrode material, this method passes through source of iron
It uses solvent-thermal method to carry out confinement energy first with carbon source, so that carbon is effectively coated on molysite surface, then pass through solid phase reaction
Molysite is set to be converted into FeNCN, to obtain carbon compound iron carbodiimide material;This method uses common source of iron and carbon source conduct
Reaction raw materials, so that entirely reacts is low in cost, raw material are easy to get, and carry out confinement synthetic reaction by solvent-thermal method, so that
Entire reaction is limited to the outside of molysite, generates carbon-coating in the outer layer of molysite, carbon-coating coats molysite while reaction.This hair
Bright need single step reaction can outside source of iron compound carbon-coating, be not required to additional complex reaction step, eventually by solid phase reaction,
So that internal molysite is changed, carbon compound iron carbodiimide negative electrode material, the preparation method are synthesized by two-step reaction
Process is simple, and yield is high, and the yield range that this method prepares negative electrode material is 18-25%.
The invention also discloses a kind of carbon compound iron carbodiimide cell negative electrode materials, and the material is by iron carbodiimide and carbon
Layer composition, the outside of iron carbodiimide is coated with one layer of carbon-coating, because the outside of iron carbodiimide is coated with carbon-coating, so that the cathode
In sodium-ion battery use process, iron carbodiimide is limited by carbon-coating and is difficult to generate big volume change material, effectively solves
Certainly the problem of the volume expansion of transition metal carbodiimide, and then promote electric conductivity and stable structure of the material in charge and discharge process
Property, the reactivity of battery is enhanced, (FeNCN first is in storage sodium so that the material has excellent sodium ion storage performance
Ions just have good performance, add its excellent electric conductivity, are close to the electric conductivity of metal.Secondly, of the invention
The FeNCN being synthesized can not only play the excellent properties of itself, and to this material in high intensity for a long time
The powder phenomenon-tion generated in charge and discharge cycles because volume expansion is shunk has given control, so that the excellent properties of the material are able to
Keep for a long time), charge/discharge capacity is high and high rate performance is good.
[Detailed description of the invention]
Fig. 1 is the XRD diagram that the embodiment of the present invention 1 prepares product;
Fig. 2 is that the embodiment of the present invention 1 prepares product low power scanning electron microscope (SEM) photograph;
Fig. 3 is that the embodiment of the present invention 1 prepares the low power scanning electron microscope (SEM) photograph after product removes internal FeNCN;
Fig. 4 is that the embodiment of the present invention 1 prepares scanning electron microscope (SEM) photograph of the product under 5000 times of amplification factors;
Fig. 5 is that the embodiment of the present invention 1 is prepared to product to be applied in battery, the charge-discharge test figure of battery;
Fig. 6 is the XRD diagram that the embodiment of the present invention 2 prepares product;
Fig. 7 is the scanning electron microscope (SEM) photograph that the embodiment of the present invention 2 prepares product.
[specific embodiment]
The invention will be described in further detail with attached drawing combined with specific embodiments below, and the invention discloses a kind of compound
It is specific to prepare carbon compound iron carbodiimide this method by this method for iron carbodiimide cell negative electrode material and preparation method thereof
The following steps are included:
Step 1, source of iron and carbon source are shone into mass ratio 1:(1-2) it is placed in mortar, by ground and mixed, mix the two
Sufficiently obtained mixture A, wherein source of iron is the organic acid molysite or inorganic transition metal salt that can be dissolved in water, the organic acid iron
Salt includes ironic citrate, ferric oxalate, ferric formate and ferric acetate etc., inorganic transition metal salt such as iron chloride, ferric nitrate and ferric sulfate
It is organic matter raw material, such as sucrose, chitosan, glucose, melamine, ammonium oxalate Deng, carbon source;Mixture A is placed in
In reaction kettle, and ethyl alcohol is added in a kettle, the ratio of mixture A and ethyl alcohol is (2-3) g:(50-70) mL, by reaction kettle
Be placed in and reacted into reactor, reaction temperature be 200 DEG C, reaction time 12-36h, heating rate be 10 DEG C/
Min collects products therefrom and is centrifuged, and centrifugal rotational speed 8000r/min is centrifuged 3-6 times, and each centrifugation time is 3-8min,
Product after centrifugation is dry at 60-80 DEG C, and the dry ethyl alcohol solute into product is evaporated, and process product B, process is made
Product B is the molysite that external sheath has carbon-coating, and the molysite is FexOy@C, wherein FexOyFor iron oxide, ferrous oxide and four oxygen
Change the mixture of three-iron, therefore uses FexOyIt indicates;The step carries out confinement synthesis by hot solvent method, is reacting molysite surface
Direct carbon coated in journey does not need the additional step of other carbon coating molysite;Preparation method is simple, at low cost, and yield is high, produces
Rate is up to 18-25%), direct carbon coating does not need other steps and completes cladding process.
Step 2, process product B and urea are mixed according to mass ratio 1:(1.5-3) and are placed in quartz or alumina crucible,
And crucible is placed in tube furnace, under an argon atmosphere, 300~600 DEG C are at the uniform velocity warming up to the heating rate of 5-20 DEG C/min,
Solid phase reaction is carried out, the solid phase reaction is FexOyIt is reacted with urea, generates molysite, i.e., the core coated by carbon-coating is by iron
Oxide becomes molysite FeNCN, after reaction, collects after entire reaction system is cooling and obtains reaction product FeNCN@C,
Middle carbon-coating with a thickness of 70-500nm;By the solid phase reaction of the step, so that the molysite inside product is converted into FeNCN, in turn
Obtain carbon compound iron carbodiimide negative electrode material.
FeNCN@C obtained above is prepared into button-shaped sodium-ion battery, encapsulation step is as follows: by carbon compound iron carbon
Diimine subsidiary engine material, conductive agent (Super P), the proportion that bonding agent (carboxyl methyl cellulose) is 8:1:1 according to mass ratio
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 oven
Electrode slice is assembled into sodium ion half-cell later by 12h.Above-mentioned sodium ion half-cell is used into new prestige electrochemical workstation pair
Battery carries out constant current charge-discharge test, and resulting materials are assembled into button cell and test it by test voltage 0.01V-3.0V
Anode material of lithium-ion battery performance.
Embodiment 1
1) 1g ironic citrate and 1.5g glucose are put into mortar and are sufficiently mixed grinding, 60mL is added in mixture A
Ethyl alcohol, be put into reaction kettle and in homogeneous reactor with 10 DEG C/min be warming up to 200 DEG C reaction for 24 hours, collect products therefrom into
Row centrifugation, is centrifuged 4 times, is centrifuged 6min every time, and centrifugation product is dried to obtain process product B at 60 DEG C.
2) 0.5g process product B is mixed with 1g urea and is placed in alumina crucible, and crucible is placed in tube furnace,
Under argon atmosphere, 500 DEG C are at the uniform velocity warming up to the heating rate of 10 DEG C/min, solid phase reaction is carried out, after reaction, to entire
It is collected after reaction system is cooling and obtains reaction product FeNCN@C.
Product, reaction product made from the present embodiment are analyzed using Rigaku D/max2000PCX- x ray diffractometer x
The XRD diagram of FeNCN@C as shown in Figure 1, the scanning electron microscope (SEM) photograph of reaction product as shown in figs 2-4, as can be seen from Figure 2
FeNCN external sheath has one layer C layers, is clearer statement,, can be with referring to Fig. 3 after the FeNCN removing in reaction product
Clearly seeing clearly has one layer of C, it can be seen that the polyhedral structure and more of accumulation is presented in product from the high power scanning electron microscope (SEM) photograph of Fig. 4
Face body is grown on the carbon shell structure surface of thin layer.
Reaction product FeNCN C obtained is assembled into sodium ion button cell according to above-mentioned battery assembly method, and is carried out
Charge-discharge test, test results are shown in figure 5, and battery presents the capacity of 700mAh/g under the current density of 100mA/g,
Still with the capacity of 300mAh/g or more under the current density of 5A/g, it is seen that material has excellent high rate performance and charge and discharge capacitor
Amount.
Embodiment 2
1) 1g ferric nitrate is put into mortar and is sufficiently mixed grinding with 2g ammonium oxalate, 60mL ethyl alcohol is added in mixture A,
Be put into reaction kettle and 200 DEG C of reaction 12h be warming up to 10 DEG C/min in homogeneous reactor, collect products therefrom carry out from
The heart is centrifuged 4 times, is centrifuged 6min every time, and centrifugation product is dried to obtain process product B at 60 DEG C.
2) 0.5g process product B is mixed with 1.5g urea and is placed in alumina crucible, and crucible is placed in tube furnace,
Under an argon atmosphere, 570 DEG C are at the uniform velocity warming up to the heating rate of 20 DEG C/min, solid phase reaction are carried out, after reaction, to whole
It is collected after a reaction system is cooling and obtains reaction product FeNCN@C.
Product D is analyzed using Rigaku D/max2000PCX- x ray diffractometer x, the XRD of products therefrom is shown in Fig. 6, by this
Sample is observed under scanning electron microscope, as shown in fig. 7, it can be seen from figure 7 that product present accumulation polyhedral structure and
Polyhedron is grown on the carbon shell structure surface of thin layer, but polyhedron stand density (analysis original low compared with product made from embodiment 1
Because heating rate is very fast, the reaction time is too short in the generation temperature range of FeNCN, causes portion of product not generate, institute
It is lower with the density of distribution).
Embodiment 3
1) 1g ferric oxalate and 1g sucrose are put into mortar and are sufficiently mixed grinding, 50mL ethyl alcohol is added in mixture A, puts
Enter in reaction kettle and be warming up to 200 DEG C of reaction 36h with 10 DEG C/min in homogeneous reactor, collects products therefrom and be centrifuged,
Centrifugation 3 times, is centrifuged 8min every time, and centrifugation product is dried to obtain process product B at 65 DEG C.
2) 1g process product B is mixed with 3g urea and is placed in alumina crucible, and crucible is placed in tube furnace, in argon
Under gas atmosphere, 300 DEG C are at the uniform velocity warming up to the heating rate of 10 DEG C/min, carries out solid phase reaction, after reaction, to entire anti-
It is collected after answering system cooling and obtains reaction product FeNCN@C.
Embodiment 4
1) 1g ferric formate and 1.2g chitosan are put into mortar and are sufficiently mixed grinding, 55mL second is added in mixture A
Alcohol is put into reaction kettle and is warming up to 200 DEG C of reaction 20h in homogeneous reactor with 10 DEG C/min, collects products therefrom and carries out
Centrifugation is centrifuged 6 times, is centrifuged 3min every time, and centrifugation product is dried to obtain process product B at 70 DEG C.
2) 1g process product B is mixed with 1.5g urea and is placed in alumina crucible, and crucible is placed in tube furnace,
Under argon atmosphere, 600 DEG C are at the uniform velocity warming up to the heating rate of 10 DEG C/min, solid phase reaction is carried out, after reaction, to entire
It is collected after reaction system is cooling and obtains reaction product FeNCN@C.
Embodiment 5
1) 1g ferric acetate and 1.4g melamine are put into mortar and are sufficiently mixed grinding, 60mL is added in mixture A
Ethyl alcohol is put into reaction kettle and is warming up to 200 DEG C of reaction 15h in homogeneous reactor with 10 DEG C/min, collect products therefrom into
Row centrifugation, is centrifuged 5 times, is centrifuged 4min every time, and centrifugation product is dried to obtain process product B at 75 DEG C.
2) 1g process product B is mixed with 1.8g urea and is placed in alumina crucible, and crucible is placed in tube furnace,
Under argon atmosphere, 400 DEG C are at the uniform velocity warming up to the heating rate of 10 DEG C/min, solid phase reaction is carried out, after reaction, to entire
It is collected after reaction system is cooling and obtains reaction product FeNCN@C.
Embodiment 6
1) 1g iron chloride and 1.6g glucose are put into mortar and are sufficiently mixed grinding, 65mL second is added in mixture A
Alcohol is put into reaction kettle and is warming up to 200 DEG C of reaction 25h in homogeneous reactor with 10 DEG C/min, collects products therefrom and carries out
Centrifugation is centrifuged 3 times, is centrifuged 5min every time, and centrifugation product is dried to obtain process product B at 80 DEG C.
2) 1g process product B is mixed with 2.2g urea and is placed in alumina crucible, and crucible is placed in tube furnace,
Under argon atmosphere, 600 DEG C are at the uniform velocity warming up to the heating rate of 10 DEG C/min, solid phase reaction is carried out, after reaction, to entire
It is collected after reaction system is cooling and obtains reaction product FeNCN@C.
Embodiment 7
1) 1g ferric nitrate and 1.7g ammonium oxalate are put into mortar and are sufficiently mixed grinding, 65mL second is added in mixture A
Alcohol is put into reaction kettle and is warming up to 200 DEG C of reaction 30h in homogeneous reactor with 10 DEG C/min, collects products therefrom and carries out
Centrifugation is centrifuged 5 times, is centrifuged 7min every time, and centrifugation product is dried to obtain process product B at 70 DEG C.
2) 1g process product B is mixed with 2.4g urea and is placed in alumina crucible, and crucible is placed in tube furnace,
Under argon atmosphere, 350 DEG C are at the uniform velocity warming up to the heating rate of 10 DEG C/min, solid phase reaction is carried out, after reaction, to entire
It is collected after reaction system is cooling and obtains reaction product FeNCN@C.
Embodiment 8
1) 1g ferric sulfate and 1.9g sucrose are put into mortar and are sufficiently mixed grinding, 70mL ethyl alcohol is added in mixture A,
Be put into reaction kettle and 200 DEG C of reaction 32h be warming up to 10 DEG C/min in homogeneous reactor, collect products therefrom carry out from
The heart is centrifuged 6 times, is centrifuged 3min every time, and centrifugation product is dried to obtain process product B at 80 DEG C.
2) 1g process product B is mixed with 2.6g urea and is placed in alumina crucible, and crucible is placed in tube furnace,
Under argon atmosphere, 450 DEG C are at the uniform velocity warming up to the heating rate of 10 DEG C/min, solid phase reaction is carried out, after reaction, to entire
It is collected after reaction system is cooling and obtains reaction product FeNCN@C.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of carbon compound iron carbodiimide cell negative electrode material, which comprises the following steps:
Step 1, after source of iron and carbon source being mixed according to mass ratio 1:(1-2), mixture A is subjected to confinement conjunction by hot solvent method
At reaction, process product B will be made after reaction product centrifugation, drying;
Step 2, process product B and urea generate carbon compound iron carbodiimide cell negative electrode material, chemistry by solid phase reaction
Structural formula is FeNCN@C.
2. a kind of preparation method of carbon compound iron carbodiimide cell negative electrode material according to claim 1, feature exist
In, the hot solvent method the step of are as follows: to anti-after mixing mixture A and ethyl alcohol proportionally (2-3) g:(50-70) mL
It answers in device and is reacted, reaction temperature is 200 DEG C, reaction time 12-36h.
3. a kind of preparation method of carbon compound iron carbodiimide cell negative electrode material according to claim 1, feature exist
In source of iron is organic acid molysite or inorganic transition metal salt, and organic acid molysite includes ironic citrate, ferric oxalate, ferric formate and second
Sour iron;Inorganic transition metal salt includes iron chloride, ferric nitrate and ferric sulfate.
4. a kind of preparation method of carbon compound iron carbodiimide cell negative electrode material according to claim 1, feature exist
In carbon source is any one of sucrose, chitosan, glucose, melamine or ammonium oxalate.
5. a kind of preparation method of carbon compound iron carbodiimide cell negative electrode material according to claim 1, feature exist
In in step 1, centrifugal rotational speed 8000r/min is centrifuged 3-6 times, and each centrifugation time is 3-8min.
6. a kind of preparation method of carbon compound iron carbodiimide cell negative electrode material according to claim 1, feature exist
In in step 1, the centrifugation product drying temperature after reaction product centrifugation is 60-80 DEG C.
7. a kind of preparation method of carbon compound iron carbodiimide cell negative electrode material according to claim 1, feature exist
In in step 2, by process product B and urea according to mass ratio 1:(1.5-3) mixing progress solid phase reaction.
8. a kind of preparation method of carbon compound iron carbodiimide cell negative electrode material according to claim 1, feature exist
In in step 2, the temperature of solid phase reaction is 300~600 DEG C.
9. a kind of carbon compound iron carbodiimide battery cathode prepared by preparation method described in claim 1-8 any one
Material, which is characterized in that iron carbodiimide surface recombination has a carbon-coating, the carbon-coating with a thickness of 70-500nm.
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CN111129456B (en) * | 2019-12-18 | 2022-06-24 | 西安工业大学 | Co-doped FeNCN/C and preparation method and application thereof |
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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 |
CN113130903A (en) * | 2021-04-14 | 2021-07-16 | 陕西科技大学 | Aluminum oxide coated iron cyanamide material prepared by sol-gel method and preparation method and application thereof |
CN113130903B (en) * | 2021-04-14 | 2022-11-29 | 陕西科技大学 | Aluminum oxide coated iron cyanamide material prepared by sol-gel method and preparation method and application thereof |
CN113224302A (en) * | 2021-05-08 | 2021-08-06 | 陕西科技大学 | Iron cyanamide material for realizing graphitized carbon coating by in-situ autocatalysis and application thereof |
CN114956122A (en) * | 2022-06-20 | 2022-08-30 | 中国科学院上海硅酸盐研究所 | Copper-based metal cyanamide compound catalyst and preparation method and application thereof |
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