CN111916741A - Preparation method and application of sodium titanium phosphate/carbon composite material - Google Patents
Preparation method and application of sodium titanium phosphate/carbon composite material Download PDFInfo
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- CN111916741A CN111916741A CN202010654686.1A CN202010654686A CN111916741A CN 111916741 A CN111916741 A CN 111916741A CN 202010654686 A CN202010654686 A CN 202010654686A CN 111916741 A CN111916741 A CN 111916741A
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- 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
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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
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
The invention discloses a preparation method and application of a sodium titanium phosphate/carbon composite material. The preparation method comprises the following steps: (1) adding a sodium source, a titanium source and a phosphorus source into an organic solvent, and performing ball milling to prepare uniform slurry; (2) filtering the slurry, and then preparing filter residues into a rough blank; (3) and calcining the rough blank in an inert atmosphere, and then cooling to obtain the carbon-coated sodium titanium phosphate composite material. The application is as follows: the carbon-coated sodium titanium phosphate composite material prepared by the preparation method is used as a negative electrode material of a sodium ion battery. The invention adopts a simple method for preparing the sodium titanium phosphate/carbon composite material by one pot, and is suitable for large-scale production; the invention takes the phosphorus pentoxide as the phosphorus source, thereby reducing the cost, not causing corrosion to production equipment, not generating harmful gas, and being green and environment-friendly. The composite material prepared by the invention is used as a negative electrode material of a sodium ion battery, and the assembled sodium ion battery can show excellent electrochemical properties such as specific capacity, long cycle and the like.
Description
Technical Field
The invention relates to the field of nano material technology and electrochemistry, in particular to a preparation method and application of a sodium titanium phosphate/carbon composite material.
Background
In the process of changing new and old energy forms, and utilizing and developing new energy, secondary batteries play an important role. Although lead-acid batteries and lithium-ion batteries are widely applied to the fields of mobile power sources, energy storage and the like, new battery systems are rapidly developed due to respective defects, new water-based batteries are attracted by attention, and sodium titanium phosphate (NaTi2(PO4)3) is an anode material of sodium-ion batteries or water-based sodium-ion batteries which are attracted by attention at present.
Sodium titanium phosphate with NASICON structure (NaTi2(PO4)3) is a polyanion material, and the three-dimensional polyanion skeleton makes it have the advantages of high ion conductivity and high structural stability. The sodium ion battery or the water system sodium ion battery cathode material can keep stable in the process of charging and discharging, and the volume change is almost zero. At present, the existing laboratory preparation technology such as a hydrothermal method or a sol-gel method is not suitable for large-scale production, and even if some technologies can realize large-scale production, the following bottlenecks exist: firstly, almost all the technologies use phosphoric acid or ammonium dihydrogen phosphate as a phosphorus source (Chinese patent), and the ammonium dihydrogen phosphate is used as the phosphorus source for preparing sodium titanium phosphate (NaTi2(PO4)3), so that the generation of corrosive harmful tail gas, namely ammonia gas, cannot be avoided, the generation of ammonia gas not only increases the risk of environmental pollution, but also greatly increases the complexity of equipment and the production cost in the subsequent treatment; phosphoric acid is a medium strong acid and has strong corrosivity, and the use of phosphoric acid as a phosphorus source has high requirements on production equipment and corrosion resistance can increase production cost. Secondly, the prior art adopts the processes of wet grinding and dispersing the raw materials and then drying in the production process, and the prior spray drying technology needs to consume a large amount of energy, so that the cost is overhigh. Thirdly, the conductivity of sodium titanium phosphate (NaTi2(PO4)3) is poor, so that the cycle performance, the charge and discharge performance, the rate capability and the like need to be improved, at present, methods such as carbon coating or compounding with graphene and carbon nano tubes and the like mainly exist, the current carbon coating technology mainly comprises the steps of firstly preparing a product, then adding a carbon source, and performing processes such as ball milling, spray drying, calcining and the like, so that the preparation process is complicated.
Disclosure of Invention
The invention aims to provide a simple method for preparing the sodium titanium phosphate/carbon composite material in one pot, which has low cost, no harmful or corrosive gas emission in the preparation process, and is more environment-friendly; the prepared carbon-coated sodium titanium phosphate composite material is used as a negative electrode material of a sodium ion battery, and shows excellent electrochemical properties such as specific capacity, long cycle and the like.
The invention is realized by the following technical scheme:
a preparation method of a sodium titanium phosphate/carbon composite material is characterized by comprising the following steps:
(1) adding a sodium source, a titanium source and a phosphorus source into an organic solvent, and performing ball milling to prepare uniform slurry;
(2) filtering the slurry, and then preparing filter residues into a rough blank;
(3) calcining the rough blank in an inert atmosphere, and naturally cooling to room temperature to obtain the carbon-coated sodium titanium phosphate composite material (NaTi)2(PO4)3/C)。
Further, the mass ratio of the sodium source, the titanium source and the phosphorus source in the step (1) is (0.5-1): 4: and 3, the molar volume ratio of the sodium source to the organic solvent is 0.125-0.25mol/L, and the ball milling time is 1-5 hours.
Further, in the step (1), the sodium source is any one of anhydrous sodium citrate, anhydrous sodium malate, disodium ethylene diamine tetraacetate, sodium carbonate and sodium bicarbonate.
Further, in the step (1), the titanium source is titanium dioxide or metatitanic acid.
Further, in the step (1), the phosphorus source is phosphorus pentoxide. With phosphorus pentoxide (P)2O5) As a phosphorus source, the phosphorus source is not corrosive to the prepared equipment, harmful tail gas except water is not generated, and meanwhile, the phosphorus pentoxide is cheap, and the phosphorus pentoxide is used as the phosphorus source, so that the preparation cost of the whole carbon-coated titanium sodium phosphate composite material can be reduced.
Further, the organic solvent in the step (1) is any one of toluene, n-hexane and cyclohexane. The organic solvent is used as a dispersing agent in the ball milling process.
Further, the slurry is pressed into a high-pressure filtering kettle in the step (2), pressure filtering is carried out, and then filter residue is collected and pressed into a rough blank.
Further, in the step (3), the calcination is carried out by heating up in a tubular atmosphere furnace, wherein the calcination temperature is 800-1000 ℃, the heating up rate is 2-5 ℃/min, and the temperature is kept for 3-12 hours after heating up.
The application of the sodium titanium phosphate/carbon composite material is characterized in that the carbon-coated sodium titanium phosphate composite material (NaTi) prepared by the preparation method of the sodium titanium phosphate/carbon composite material2(PO4)3and/C) is used as a negative electrode material of the sodium ion battery. The prepared carbon-coated sodium titanium phosphate composite material is used as a negative electrode material of a sodium ion battery, and the assembled sodium ion battery can show excellent electrochemical properties such as specific capacity, long cycle and the like.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention adopts a method for preparing sodium titanium phosphate/carbon composite material (NaTi) in one pot2(PO4)3The simple method of the/C) does not need to be distributed, has low energy consumption and simpler preparation process, and is suitable for large-scale production;
(2) the invention uses phosphorus pentoxide (P)2O5) As a preparation of sodium titanium phosphate/carbon composite material (NaTi)2(PO4)3The phosphorus source of the/C) can avoid the problem that the traditional preparation method uses phosphoric acid as the phosphorus source and has equipment corrosivity for production; and isThe phosphorus pentoxide is used as a phosphorus source, so that the problem of environmental pollution caused by harmful tail gas, namely ammonia gas, generated by using ammonium dihydrogen phosphate as the phosphorus source in the traditional preparation method can be solved, and the method is more environment-friendly; meanwhile, the phosphorus pentoxide is cheap, and the production cost of the carbon-coated sodium titanium phosphate composite material is reduced;
(3) the carbon-coated sodium titanium phosphate composite material (NaTi) prepared by the invention2(PO4)3the/C) is used as the cathode material of the sodium ion battery, and the assembled sodium ion battery can show excellent specific capacity, long cycle and other electrochemical properties, thereby being an ideal cathode material of the sodium ion battery.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is an XRD pattern for example 1, example 2 and example 3 of the present invention;
FIG. 2 shows a carbon-coated sodium titanium phosphate composite (NaTi) prepared in example 1 of the present invention2(PO4)3/C) cycle capacity plot under assembled lithium ion battery 5C conditions.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a sodium titanium phosphate/carbon composite material comprises the following steps:
(1) 0.5mol (129g) of anhydrous sodium citrate (C)6H5Na3O7) 4.0mol (320g) of titanium dioxide (TiO)2) And 3.0mol (426g) of phosphorus pentoxide (P)2O5) Adding the mixture into dried 4.0L of toluene, and then placing the mixture into a planetary ball mill for ball milling for 5 hours to prepare uniform slurry;
(2) pressing the obtained slurry into a high-pressure filtering kettle, carrying out pressure filtration, collecting filter residues, and pressing the filter residues into a rough blank;
(3) placing the obtained rough blank in a tubular atmosphere furnace for heating and calcining, then introducing inert gas (the airflow speed of the inert gas is 200mL/min) into the furnace, setting the heating rate of the tubular atmosphere furnace to be 2 ℃/min, heating to 900 ℃, preserving heat for 6 hours after the heating is finished, stopping introducing the inert gas after the heat preservation is finished, and naturally cooling to room temperature to obtain the carbon-coated titanium sodium phosphate composite material (NaTi)2(PO4)3/C)。
Example 2
A preparation method of a sodium titanium phosphate/carbon composite material comprises the following steps:
(1) 1.0mol (178g) of anhydrous sodium malate (C)4H4O5Na2) 4.0mol (392g) of metatitanic acid (i.e. hydrated titanium dioxide TiO (OH))2) And 3.0mol (426g) of phosphorus pentoxide (P)2O5) Adding the mixture into 4.0L of n-hexane, and then placing the mixture into a planetary ball mill for ball milling for 1 hour to prepare uniform slurry;
(2) pressing the obtained slurry into a high-pressure filtering kettle, carrying out pressure filtration, collecting filter residues, and pressing the filter residues into a rough blank;
(3) placing the obtained rough blank in a tubular atmosphere furnace for heating and calcining, then introducing inert gas (the airflow speed of the inert gas is 200mL/min) into the furnace, setting the heating rate of the tubular atmosphere furnace to be 5 ℃/min, heating to 1000 ℃, preserving heat for 3 hours after the heating is finished, stopping introducing the inert gas after the heat preservation is finished, and naturally cooling to room temperature to obtain the finished productObtaining the carbon-coated sodium titanium phosphate composite material (NaTi)2(PO4)3/C)。
Example 3
A preparation method of a sodium titanium phosphate/carbon composite material comprises the following steps:
(1) 0.6mol (223.3g) of disodium ethylenediaminetetraacetate (C)10H14N2Na2O8) 4.0mol (392g) of metatitanic acid (i.e. hydrated titanium dioxide TiO (OH))2) And 3.0mol (426g) of phosphorus pentoxide (P)2O5) Adding the mixture into 4.0L of cyclohexane, and then placing the mixture into a planetary ball mill for ball milling for 3 hours to prepare uniform slurry;
(2) pressing the obtained slurry into a high-pressure filtering kettle, carrying out pressure filtration, collecting filter residues, and pressing the filter residues into a rough blank;
(3) placing the obtained rough blank in a tubular atmosphere furnace for heating and calcining, then introducing inert gas (the airflow speed of the inert gas is 200mL/min) into the furnace, setting the heating rate of the tubular atmosphere furnace to be 4 ℃/min, heating to 800 ℃, preserving heat for 12 hours after the heating is finished, stopping introducing the inert gas after the heat preservation is finished, and naturally cooling to room temperature to obtain the carbon-coated titanium sodium phosphate composite material (NaTi)2(PO4)3/C)。
Example 4
A preparation method of a sodium titanium phosphate/carbon composite material comprises the following steps:
(1) 0.8mol (67.5g) of sodium hydrogencarbonate (NaHCO)3) 4.0mol (320g) of titanium dioxide (TiO)2) And 3.0mol (426g) of phosphorus pentoxide (P)2O5) Adding the mixture into 4.0L of methylbenzene, and then placing the mixture into a planetary ball mill for ball milling for 2 hours to prepare uniform slurry;
(2) pressing the obtained slurry into a high-pressure filtering kettle, carrying out pressure filtration, collecting filter residues, and pressing the filter residues into a rough blank;
(3) placing the obtained rough blank in a tubular atmosphere furnace for heating and calcining, then introducing inert gas (the gas flow velocity of the inert gas is 200mL/min) into the furnace, setting the heating rate of the tubular atmosphere furnace to be 5 ℃/min, and heating to 850 DEG CKeeping the temperature for 8 hours after the temperature rise is finished, stopping introducing inert gas after the temperature is finished, and naturally cooling to room temperature to obtain the carbon-coated sodium titanium phosphate composite material (NaTi)2(PO4)3/C)。
Example 5
A preparation method of a sodium titanium phosphate/carbon composite material comprises the following steps:
(1) 0.7mol (74.2g) of sodium carbonate (Na) are added2CO3) 4.0mol (320g) of titanium dioxide (TiO)2) And 3.0mol (426g) of phosphorus pentoxide (P)2O5) Adding the mixture into 4.0L of methylbenzene, and then placing the mixture into a planetary ball mill for ball milling for 4 hours to prepare uniform slurry;
(2) pressing the obtained slurry into a high-pressure filtering kettle, carrying out pressure filtration, collecting filter residues, and pressing the filter residues into a rough blank;
(3) placing the obtained rough blank in a tubular atmosphere furnace for heating and calcining, then introducing inert gas (the airflow speed of the inert gas is 200mL/min) into the furnace, setting the heating rate of the tubular atmosphere furnace to be 3 ℃/min, heating to 930 ℃, preserving heat for 10 hours after the heating is finished, stopping introducing the inert gas after the heat preservation is finished, and naturally cooling to room temperature to obtain the carbon-coated titanium sodium phosphate composite material (NaTi)2(PO4)3/C)。
Test example 1
XRD testing of the carbon-coated sodium titanium phosphate composites prepared in examples 1, 2 and 3 above, as shown in FIG. 1, revealed that the products prepared in examples 1, 2 and 3 according to the present invention were sodium titanium phosphate/carbon composites (NaTi)2(PO4)3C) phases of matter.
Application example 1
The carbon-coated sodium titanium phosphate composite (NaTi) prepared in example 1 was used2(PO4)3/C) as a negative electrode material for sodium ion battery, sodium ion battery was assembled and tested by blue cell test system under 5C (meaning 5 times of charging in 1 hour) condition, as shown in FIG. 2, from which it can be seen that 6 times of charging was still achieved under the condition of very fast chargingThe specific capacity of 0mAh/g is only slightly reduced after 2000 cycles, which shows that the prepared material has good stability; and it can be seen from fig. 2 that the charge-discharge efficiency of the battery is almost 100%, which indicates that there is no side reaction during charge-discharge and the energy utilization rate is high.
The above-mentioned preferred embodiments of the present invention are provided for illustration only and not for the purpose of limiting the invention. Obvious variations or modifications of the present invention are within the scope of the present invention.
Claims (9)
1. A preparation method of a sodium titanium phosphate/carbon composite material is characterized by comprising the following steps:
(1) adding a sodium source, a titanium source and a phosphorus source into an organic solvent, and performing ball milling to prepare uniform slurry;
(2) filtering the slurry, and then preparing filter residues into a rough blank;
(3) and calcining the rough blank in an inert atmosphere, and then cooling to obtain the carbon-coated sodium titanium phosphate composite material.
2. The method for preparing the sodium/carbon titanium phosphate composite material according to claim 1, wherein the amount ratio of the sodium source, the titanium source and the phosphorus source in step (1) is (0.5-1): 4: and 3, the molar volume ratio of the sodium source to the organic solvent is 0.125-0.25mol/L, and the ball milling time is 1-5 hours.
3. The method for preparing a sodium titanium phosphate/carbon composite material according to claim 1, wherein the sodium source in step (1) is any one of anhydrous sodium citrate, anhydrous sodium malate, disodium ethylenediaminetetraacetate, sodium carbonate and sodium bicarbonate.
4. The method for preparing a sodium titanium phosphate/carbon composite material according to claim 1, wherein the titanium source in the step (1) is titanium dioxide or metatitanic acid.
5. The method for preparing a sodium titanium phosphate/carbon composite material according to claim 1, wherein the phosphorus source in step (1) is phosphorus pentoxide.
6. The method for preparing a sodium titanium phosphate/carbon composite material according to claim 1, wherein the organic solvent in step (1) is any one of toluene, n-hexane and cyclohexane.
7. The method for preparing a sodium titanium phosphate/carbon composite material according to claim 1, wherein the slurry is pressed into a high-pressure filter kettle in the step (2), pressure filtration is carried out, and then filter residue is collected and pressed into a rough blank.
8. The method for preparing sodium titanium phosphate/carbon composite material according to claim 1, wherein in the step (3), the calcination is performed by heating in a tubular atmosphere furnace, the calcination temperature is 800-1000 ℃, the heating rate is 2-5 ℃/min, and the temperature is maintained for 3-12 hours after heating.
9. The application of the sodium titanium phosphate/carbon composite material is characterized in that the carbon-coated sodium titanium phosphate composite material prepared by the preparation method of the sodium titanium phosphate/carbon composite material according to any one of claims 1 to 8 is used as a negative electrode material of a sodium ion battery.
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| CN114873573A (en) * | 2022-04-19 | 2022-08-09 | 江苏理工学院 | NaTi 2 (PO4) 3 @ C micro-nano composite material and preparation method and application thereof |
| CN115626623A (en) * | 2022-10-07 | 2023-01-20 | 蚌埠学院 | Preparation method of carbon composite titanium phosphate sodium aqueous sodium nano negative electrode material and battery thereof |
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