CN110176602A - A kind of preparation process of the long-life sodium-ion battery three-dimensional porous carbon nano-electrode material of phosphorus doping biomass - Google Patents
A kind of preparation process of the long-life sodium-ion battery three-dimensional porous carbon nano-electrode material of phosphorus doping biomass Download PDFInfo
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- CN110176602A CN110176602A CN201910559593.8A CN201910559593A CN110176602A CN 110176602 A CN110176602 A CN 110176602A CN 201910559593 A CN201910559593 A CN 201910559593A CN 110176602 A CN110176602 A CN 110176602A
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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
- 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
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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
- H01M4/36—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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
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- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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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
The invention discloses a kind of long-life sodium-ion battery preparation processes of the three-dimensional porous carbon nano-electrode material of phosphorus doping biomass, and biomass castoff deionized water is successively cleaned by ultrasonic with ethyl alcohol, then dry and be ground into powder, and sieving obtains powdery A；Phosphoric acid solution is added into powdery A, and mixture B is mixed to obtain using ultrasonic wave added；Mixture B is transferred in hydro-thermal induction kettle, and hydro-thermal induction kettle is moved into hydro-thermal induction heating equipment and reacted as induction source by the carbon cloth being added, it is then cooled to room temperature, carbon cloth is taken out, products therefrom is scraped after deionized water and ethyl alcohol cleaning filter, C is dried to obtain；It calcines, is cooled to room temperature after above-mentioned C is mixed with phosphorus source, products therefrom is obtained into D after deionized water and ethyl alcohol cleaning centrifugation；D is activated to get the three-dimensional porous carbon nano-electrode material of phosphorus doping biomass is arrived.
Description
Technical field
The invention belongs to the preparation fields of anode material of lithium-ion battery, and in particular to a kind of long-life sodium-ion battery use
The preparation process of the three-dimensional porous carbon nano-electrode material of phosphorus doping biomass.
Background technique
Lithium ion battery enters in daily life extensively.It is needed in face of growing lithium ion battery
It asks, the case where minable lithium mine is faced with resource exhaustion on the earth, from the angle of sustainable development, seeks novel battery
It is the certainty of development.Sodium element and elemental lithium are in same main group, and property is similar, and the earth abundance of sodium element is elemental lithium
More than 400 times, therefore developing novel sodium-ion battery is a kind of trend of the times.Wherein the research of anode material of lithium-ion battery has been
As hot spot.
Have abundant light weight, pore structure, large specific surface area, structure steady by the biomass carbon that biological material is prepared into
The performances such as qualitative good and excellent electric conductivity, can be applied to anode material of lithium-ion battery.It is existing research shows that biomass
Carbon has to be hoisted as its capacitance of anode material of lithium-ion battery and high rate performance.It is former that impurity is introduced into biomass carbon material
Son has become a kind of effective ways for promoting chemical property.
The introducing hetero-atoms in multiporous biological matter carbon material, such as nitrogen, sulphur, phosphorus or boron can improve its electrification significantly
It learns, mechanical or electric conductivity.Especially P elements can partially replace carbon, change the appearance structure of biomass carbon, be sodium from
The intercalation process of son provides bigger space, and can be reduced volume expansion and reduce the adsorption energy of sodium ion, improves sodium ion electricity
Tankage.Can be improved sodium ion diffusion rate after p-doped, electronic transmission performance is conducive to promote electric conductivity, thus promoted sodium from
The high rate performance of sub- battery.For example, Wang et al. ([J] .RSC Adv.2015,5 (68): 55136-55142.) use rice husk for
Raw material clean 6h with 10% hydrochloric acid at a temperature of 100 DEG C, then by its dislocation water heating kettle, hydro-thermal 2 days under the conditions of 230 DEG C,
Product is cleaned with 5% hydrofluoric acid, and hydrothermal product is finally mixed to drying with triphenylphosphine and moves to argon atmosphere tube furnace,
It rises to 1000 DEG C with the heating rate of 10 DEG C/min and keeps the temperature 1h and obtain product.The complex technical process, energy consumption is high, also to remove
The element silicon of aniseed in raw material.Therefore it is extensive to develop a kind of raw material sources, and it is low in cost, electrochemical performance and simply may be used
Control, reproducible technique are of great significance to prepare the porous carbon nanomaterial of phosphorus doping.
Summary of the invention
The purpose of the present invention is to provide a kind of long-life sodium-ion battery three-dimensional porous carbon nanometers of phosphorus doping biomass
The preparation process of electrode material, to overcome the problems of the above-mentioned prior art, electrode material prepared by the present invention is applied to sodium
In ion battery, not only have excellent chemical property, but also have turn waste into wealth, environmentally protective economic benefit.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation process of the long-life sodium-ion battery three-dimensional porous carbon nano-electrode material of phosphorus doping biomass, packet
Include following steps:
1) biomass castoff deionized water is successively cleaned by ultrasonic with ethyl alcohol, then dries and is ground into powder, mistake
Sieve obtains powdery A；
2) phosphoric acid solution is added in Xiang Fenzhuan A, and mixture B is mixed to obtain using ultrasonic wave added；
3) mixture B is transferred in hydro-thermal induction kettle, and the carbon cloth being added moves into hydro-thermal induction kettle as induction source
In hydro-thermal induction heating equipment, with the induction frequencies of 200~500KHz by room temperature to 150~180 DEG C, and heat preservation 20~
50min is then cooled to room temperature, and takes out carbon cloth, and products therefrom is scraped after deionized water and ethyl alcohol cleaning filter, is dried
C；
4) 500~700 DEG C are risen to the heating rate of 3 DEG C/min after mixing above-mentioned C with phosphorus source, and keeps the temperature 1~3h, it is cold
But to room temperature, products therefrom is obtained into D after deionized water and ethyl alcohol cleaning centrifugation；
5) D is heated to 3~10 DEG C of heating rates to 300 DEG C, and keeps the temperature 5~8h and is activated to get phosphorus doping is arrived
The three-dimensional porous carbon nano-electrode material of biomass.
Further, biomass castoff is shuck, egg shell, coffee shell or cocoanut shell in step 1).
Further, ultrasonic cleaning frequency is 30KHz, time 1h in step 1).
Further, dry in step 1) specifically: using the dry 3~6h of infrared lamp.
Further, it is crushed into powder last 300~600 mesh of mistake in step 1) and obtains powdery A.
Further, 1~4g powdery A, and the concentration of phosphoric acid solution is added in step 2) in every 40~70mL phosphoric acid solution
For 1~3mol/L.
Further, supersonic frequency is 20~40KHz in step 2), and the time is 10~30min.
Further, the length, width and height of carbon cloth are respectively 3cm, 3cm, 0.1cm in step 3), and drying temperature is 70 in step 3)
DEG C, time 6h.
Further, phosphorus source is sodium dihydrogen phosphate, potassium dihydrogen phosphate, solid phosphoric acid or elemental phosphorous in step 4).
Further, C and the mass ratio of phosphorus source are (1~2): (1~6) in step 4).
Compared with prior art, the invention has the following beneficial technical effects:
1. the present invention selects biomass castoff as biomass carbon source, turn waste into wealth, it is environmentally protective, there is high money
Source advantage and cost advantage.
2. the preparation process of anode material of lithium-ion battery proposed by the present invention is simple, mild condition is controllable, production cost
Low, repeatability is high, easy to industrialized production.
3. anode material of lithium-ion battery synthesized by the present invention has three-D nano-porous phosphor-containing structure, have biggish
Interlamellar spacing.Conducive to sodium ion intercalation, and it is capable of providing a large amount of reactivity site, effectively increases the sodium ion rate of adsorption,
Diffusion rate and electron-transport speed.
4. the biomass porous carbon nanomaterial of phosphorus doping prepared by the present invention is applied to be obviously improved in sodium-ion battery
The cycle life of battery has high capacity and excellent cyclical stability, thermal stability, chemical stability and machinery spirit
Activity.
Detailed description of the invention
Fig. 1 is the biomass porous carbon nanomaterial SEM figure of phosphorus doping prepared by embodiment 2；
Fig. 2 is the biomass porous carbon nanomaterial XRD diagram of phosphorus doping prepared by embodiment 2；
Fig. 3 is the biomass porous carbon nanomaterial cycle performance figure of phosphorus doping prepared by embodiment 2.
Specific embodiment
Embodiments of the present invention are described in further detail below:
A kind of preparation process of the long-life sodium-ion battery three-dimensional porous carbon nano-electrode material of phosphorus doping biomass.It should
The porous carbon nanomaterial of phosphorus doping incudes through hydro-thermal, after carbonization treatment, can be formed carbon nano-structured with cellular porous three-dimensional
Sample.Electrode material preparation process is simple, raw material environmental protection, from a wealth of sources, it can be achieved that turning waste into wealth, applied to lithium ion
There is excellent long circulating performance in battery.
Specifically includes the following steps:
1. by biomass castoff shuck, egg shell, coffee shell, cocoanut shell etc. with deionized water and ethyl alcohol successively with
30KHz frequency ultrasound cleans 1h, the dry 3~6h of infrared lamp, then is ground into powder with pulverizer, crosses 300~600 meshes and obtains A；
2. weighing 1~4g A, 40~70ml is added in Xiang Shangshu powdery A, concentration is the phosphoric acid solution of 1~3mol/L, and
Ultrasonic machine is used to obtain mixture B with 10~30min of frequency ultrasound of 20~40KHz.
3. mixture B is transferred in hydro-thermal induction kettle, and it is respectively 3cm that length, width and height, which are added, the carbon cloth of 3cm, 0.1cm are made
For induction source.Hydro-thermal induction kettle is moved into hydro-thermal induction heating equipment, with the induction frequencies of 200~500KHz by room temperature
To 150~180 DEG C, and 20~50min is kept the temperature, be then cooled to room temperature, taken out carbon cloth, products therefrom is scraped through deionized water
After being filtered with ethyl alcohol cleaning, 6h is dried in 70 DEG C of baking ovens and obtains C；
4. by above-mentioned C and phosphorus source (sodium dihydrogen phosphate, potassium dihydrogen phosphate, solid phosphoric acid, elemental phosphorous one or more of them),
Be C according to mass ratio: phosphorus source=2:1,1:2,1:4, dislocation tube furnace is after the proportion of 1:6 is mixed with the heating of 3 DEG C/min
Rate rises to 500~700 DEG C, and keeps the temperature 1~3h, is cooled to room temperature, by products therefrom through deionized water and ethyl alcohol cleaning centrifugation
After obtain D.
It activates 5. above-mentioned D is placed in baking oven, is heated to 3~10 DEG C of heating rates to 300 DEG C, and keep the temperature 5~8h and obtain
To the three-dimensional porous carbon nano-electrode material of phosphorus doping biomass.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
1. biomass castoff shuck deionized water and ethyl alcohol are successively cleaned into 1h with 30KHz frequency ultrasound, it is infrared
Lamp dries 3h, then is ground into powder with pulverizer, crosses 300 meshes and obtains A；
2. weighing 1g A, 40ml is added in Xiang Shangshu powdery A, concentration is the phosphoric acid solution of 1mol/L, and uses ultrasonic machine
Mixture B is obtained with the frequency ultrasound 10min of 20KHz.
3. mixture B is transferred in hydro-thermal induction kettle, and it is respectively 3cm that length, width and height, which are added, the carbon cloth of 3cm, 0.1cm are made
For induction source.Hydro-thermal induction kettle is moved into hydro-thermal induction heating equipment, with the induction frequencies of 200KHz by room temperature to 150
DEG C, and 20min is kept the temperature, it is then cooled to room temperature, takes out carbon cloth, products therefrom is scraped and is filtered through deionized water and ethyl alcohol cleaning
Afterwards, 6h is dried in 70 DEG C of baking ovens obtain C；
4. being that C: sodium dihydrogen phosphate=2:1 proportion is mixed according to mass ratio by above-mentioned C and phosphorus source sodium dihydrogen phosphate
Dislocation tube furnace rises to 500 DEG C with the heating rate of 3 DEG C/min afterwards, and keeps the temperature 1h, is cooled to room temperature, by products therefrom gone from
D is obtained after sub- water and ethyl alcohol cleaning centrifugation.
It activates, is heated to 3 DEG C of heating rates to 300 DEG C, and keep the temperature 5h and obtain phosphorus doping 5. above-mentioned D is placed in baking oven
The three-dimensional porous carbon nano-electrode material of biomass.
Embodiment 2
1. biomass castoff egg shell deionized water and ethyl alcohol are successively cleaned into 1h with 30KHz frequency ultrasound, it is infrared
Lamp dries 4h, then is ground into powder with pulverizer, crosses 400 meshes and obtains A；
2. weighing 2g A, 50ml is added in Xiang Shangshu powdery A, concentration is the phosphoric acid solution of 2mol/L, and uses ultrasonic machine
Mixture B is obtained with the frequency ultrasound 20min of 30KHz.
3. mixture B is transferred in hydro-thermal induction kettle, and it is respectively 3cm that length, width and height, which are added, the carbon cloth of 3cm, 0.1cm are made
For induction source.Hydro-thermal induction kettle is moved into hydro-thermal induction heating equipment, with the induction frequencies of 300KHz by room temperature to 160
DEG C, and 30min is kept the temperature, it is then cooled to room temperature, takes out carbon cloth, products therefrom is scraped and is filtered through deionized water and ethyl alcohol cleaning
Afterwards, 6h is dried in 70 DEG C of baking ovens obtain C；
4. carrying out mixing according to mass ratio for C: potassium dihydrogen phosphate=1:2 proportion and moving back above-mentioned C and potassium dihydrogen phosphate
It sets tube furnace and rises to 600 DEG C with the heating rate of 3 DEG C/min, and keep the temperature 2h, be cooled to room temperature, by products therefrom through deionized water
D is obtained with after ethyl alcohol cleaning centrifugation.
It activates, is heated to 5 DEG C of heating rates to 300 DEG C, and keep the temperature 6h and obtain phosphorus doping 5. above-mentioned D is placed in baking oven
The three-dimensional porous carbon nano-electrode material of biomass.
Embodiment 3
1. biomass castoff coffee shell deionized water and ethyl alcohol are successively cleaned into 1h with 30KHz frequency ultrasound, it is infrared
Lamp dries 5h, then is ground into powder with pulverizer, crosses 500 meshes and obtains A；
2. weighing 3g A, 60ml is added in Xiang Shangshu powdery A, concentration is the phosphoric acid solution of 2mol/L, and uses ultrasonic machine
Mixture B is obtained with the frequency ultrasound 20min of 30KHz.
3. mixture B is transferred in hydro-thermal induction kettle, and it is respectively 3cm that length, width and height, which are added, the carbon cloth of 3cm, 0.1cm are made
For induction source.Hydro-thermal induction kettle is moved into hydro-thermal induction heating equipment, with the induction frequencies of 400KHz by room temperature to 170
DEG C, and 40min is kept the temperature, it is then cooled to room temperature, takes out carbon cloth, products therefrom is scraped and is filtered through deionized water and ethyl alcohol cleaning
Afterwards, 6h is dried in 70 DEG C of baking ovens obtain C；
4. above-mentioned C mix moving back according to mass ratio with phosphorus source solid phosphoric acid for C: solid phosphoric acid=1:4 proportion
It sets tube furnace and rises to 600 DEG C with the heating rate of 3 DEG C/min, and keep the temperature 2h, be cooled to room temperature, by products therefrom through deionized water
D is obtained with after ethyl alcohol cleaning centrifugation.
It activates, is heated to 5 DEG C of heating rates to 300 DEG C, and keep the temperature 7h and obtain phosphorus doping 5. above-mentioned D is placed in baking oven
The three-dimensional porous carbon nano-electrode material of biomass.
Embodiment 4
1. biomass castoff cocoanut shell deionized water and ethyl alcohol are successively cleaned into 1h with 30KHz frequency ultrasound, it is infrared
Lamp dries 6h, then is ground into powder with pulverizer, crosses 600 meshes and obtains A；
2. weighing 4g A, 70ml is added in Xiang Shangshu powdery A, concentration is the phosphoric acid solution of 3mol/L, and uses ultrasonic machine
Mixture B is obtained with the frequency ultrasound 30min of 40KHz.
3. mixture B is transferred in hydro-thermal induction kettle, and it is respectively 3cm that length, width and height, which are added, the carbon cloth of 3cm, 0.1cm are made
For induction source.Hydro-thermal induction kettle is moved into hydro-thermal induction heating equipment, with the induction frequencies of 500KHz by room temperature to 180
DEG C, and 50min is kept the temperature, it is then cooled to room temperature, takes out carbon cloth, products therefrom is scraped and is filtered through deionized water and ethyl alcohol cleaning
Afterwards, 6h is dried in 70 DEG C of baking ovens obtain C；
4. above-mentioned C and phosphorus source is elemental phosphorous, it is C: dislocation pipe after the proportion of elemental phosphorous=1:6 is mixed according to mass ratio
Formula furnace rises to 700 DEG C with the heating rate of 3 DEG C/min, and keeps the temperature 3h, is cooled to room temperature, by products therefrom through deionized water and second
D is obtained after alcohol cleaning centrifugation.
It activates 5. above-mentioned D is placed in baking oven, is heated to 10 DEG C of heating rates to 300 DEG C, and keep the temperature 8h and obtain phosphorus and mix
The miscellaneous three-dimensional porous carbon nano-electrode material of biomass.
The phosphorus doping biomass nano material that it can be seen from the SEM figure of Fig. 1 prepared by embodiment 2 has big small-bore same
When existing three-dimensional honeycomb shape appearance structure, and there is relatively thin hole wall.2 sample of embodiment it can be seen from the XRD diagram of Fig. 2
Being 24 ° and 43 ° in 2 θ angles has more apparent graphite peaks, shows that the sample degree of graphitization is higher.By Fig. 3 cycle performance figure
As can be seen that embodiment 2 sample assembly at after sodium-ion battery in 50mAg-1Current density under, capacity is up to 307mAhg-1, capacity retention ratio is 90% or more after 500 circle of circulation, capacity with higher and excellent cyclical stability.
Claims (10)
1. a kind of long-life sodium-ion battery preparation process of the three-dimensional porous carbon nano-electrode material of phosphorus doping biomass, special
Sign is, comprising the following steps:
1) biomass castoff deionized water is successively cleaned by ultrasonic with ethyl alcohol, then dries and is ground into powder, be sieved
To powdery A；
2) phosphoric acid solution is added in Xiang Fenzhuan A, and mixture B is mixed to obtain using ultrasonic wave added；
3) mixture B is transferred in hydro-thermal induction kettle, and hydro-thermal induction kettle is moved into hydro-thermal as induction source by the carbon cloth being added
In induction heating equipment, with the induction frequencies of 200~500KHz by room temperature to 150~180 DEG C, and 20~50min is kept the temperature,
It is then cooled to room temperature, takes out carbon cloth, products therefrom is scraped after deionized water and ethyl alcohol cleaning filter, C is dried to obtain；
4) 500~700 DEG C are risen to the heating rate of 3 DEG C/min after mixing above-mentioned C with phosphorus source, and keeps the temperature 1~3h, is cooled to
Products therefrom is obtained D after deionized water and ethyl alcohol cleaning centrifugation by room temperature；
5) D is heated to 3~10 DEG C of heating rates to 300 DEG C, and keeps the temperature 5~8h and is activated to get biological to phosphorus doping
The three-dimensional porous carbon nano-electrode material of matter.
2. a kind of long-life sodium-ion battery according to claim 1 three-dimensional porous carbon nano-electrode of phosphorus doping biomass
The preparation process of material, which is characterized in that biomass castoff is shuck, egg shell, coffee shell or cocoanut shell in step 1).
3. a kind of long-life sodium-ion battery according to claim 1 three-dimensional porous carbon nano-electrode of phosphorus doping biomass
The preparation process of material, which is characterized in that ultrasonic cleaning frequency is 30KHz, time 1h in step 1).
4. a kind of long-life sodium-ion battery according to claim 1 three-dimensional porous carbon nano-electrode of phosphorus doping biomass
The preparation process of material, which is characterized in that dry in step 1) specifically: using the dry 3~6h of infrared lamp.
5. a kind of long-life sodium-ion battery according to claim 1 three-dimensional porous carbon nano-electrode of phosphorus doping biomass
The preparation process of material, which is characterized in that be crushed into powder last 300~600 mesh of mistake in step 1) and obtain powdery A.
6. a kind of long-life sodium-ion battery according to claim 1 three-dimensional porous carbon nano-electrode of phosphorus doping biomass
The preparation process of material, which is characterized in that 1~4g powdery A is added in step 2) in every 40~70mL phosphoric acid solution, and phosphoric acid is molten
The concentration of liquid is 1~3mol/L.
7. a kind of long-life sodium-ion battery according to claim 1 three-dimensional porous carbon nano-electrode of phosphorus doping biomass
The preparation process of material, which is characterized in that supersonic frequency is 20~40KHz in step 2), and the time is 10~30min.
8. a kind of long-life sodium-ion battery according to claim 1 three-dimensional porous carbon nano-electrode of phosphorus doping biomass
The preparation process of material, which is characterized in that the length, width and height of carbon cloth are respectively 3cm, 3cm, 0.1cm in step 3), are dried in step 3)
Dry temperature is 70 DEG C, time 6h.
9. a kind of long-life sodium-ion battery according to claim 1 three-dimensional porous carbon nano-electrode of phosphorus doping biomass
The preparation process of material, which is characterized in that phosphorus source is sodium dihydrogen phosphate, potassium dihydrogen phosphate, solid phosphoric acid or simple substance in step 4)
Phosphorus.
10. a kind of long-life sodium-ion battery according to claim 1 three-dimensional porous carbon nanometer electricity of phosphorus doping biomass
The preparation process of pole material, which is characterized in that C and the mass ratio of phosphorus source are (1~2): (1~6) in step 4).
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| CN112010302A (en) * | 2020-09-07 | 2020-12-01 | 合肥工业大学 | Method for preparing hierarchical porous phosphorus-doped carbon material from biomass |
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