CN105826521B - Polyanionic compound KTi2(PO4)3And its preparation of carbon coating object and products thereof and application - Google Patents
Polyanionic compound KTi2(PO4)3And its preparation of carbon coating object and products thereof and application Download PDFInfo
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- CN105826521B CN105826521B CN201610310715.6A CN201610310715A CN105826521B CN 105826521 B CN105826521 B CN 105826521B CN 201610310715 A CN201610310715 A CN 201610310715A CN 105826521 B CN105826521 B CN 105826521B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5805—Phosphides
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses polyanionic compound KTi2(PO4)3And its preparation method of carbon coating object and products thereof and the application as kalium ion battery electrode material.This method has lot of advantages：(1) easy to operate, using solvent thermal process, it is readily synthesized；(2) reaction temperature is relatively low, relatively mild, and yield is high；(3) raw material is the TiO that chemical property is stablized2、KH2PO4·2H2O、H3PO4And deionized water, it is at low cost；(4) reaction process does not have pernicious gas generation, pollution-free.It is characterized by a variety of methods, products therefrom pattern is uniform, the mutually pure free from admixture of object.And the present invention will have nanoscale cube structure KTi2(PO4)3With KTi2(PO4)3/ C is applied to kalium ion battery, and finds that its chemical property is very good after tested, and KTi2(PO4)3/ C chemical properties are more preferable.
Description
Technical field
The invention belongs to kalium ion battery Material Fields, and in particular to a kind of polyanionic compound KTi2(PO4)3And its
Preparation of carbon coating object and products thereof and application.
Background technology
Energy consumption is the important feature of modern social development, and efficient energy-storage system be then regenerative resource industry,
The core pillar of consumer electronics industry, transportation industry.In many energy storage modes, lithium ion battery is with light weight, capacity is high and
The advantages that memory-less effect, occupies core status in current energy storage industry.Due to lithium ion battery high-energy density and good
Cycle performance makes its use expand to electric vehicle and mixed power electric car from portable electronic device.However, lithium resource
It is rare and also be unevenly distributed, in addition growing consumption keeps its cost constantly soaring, to limit its extensive big rule
Mould application.However, in contrast, potassium resource is abundant and cost is at a fairly low.As one of alkali metal, potassium has similar with lithium
Physical/chemical.
Furthermore, it has been reported that careful professor of Tokyo university of science coltfoal et al. grinding in kalium ion battery technology of new generation
Breach is had found in hair.Researcher is successfully realized multiple charge and discharge using graphite electrode in the case where not reducing performance
Electricity.It is expected to improve 10 times than the charge/discharge rates of lithium ion battery using the novel battery of the technology, and high intensity can be corresponded to
Electric current exports bigger electric power, can be applied to the more demanding electrically driven treadmill that instantaneously raises speed.When using potassium ion, voltage
- 0.09 volt can be dropped to, and the voltage of the conventional batteries such as lithium ion can not drop to negative value.So far, battery capacity is improved
It is only improved a kind of method of cathode voltage, and kalium ion battery is expected to make global voltage be more than lithium ion by reducing cathode voltage
Equal batteries.Potassium, lithium, sodium are all alkaline elements.It is compared with lithium, the movement of potassium ion in the electrolytic solution is more active, more suitable
It closes charging in a short time and disposably discharges a large amount of electric currents, output high-power.Currently, there are charging time mistakes for electric vehicle
Long problem will improve the convenience of electric vehicle if it can complete charging in a short time.In addition, potassium from
The construction of sub- battery and lithium ion battery are essentially the same, can be produced on identical production line.In addition, potassium ion is in electrode material
There is good deintercalation performance, and among alkali metal, for metallic sodium, the current potential of potassium is closest to metal in material
Lithium.In worldwide, the electrode material for the kalium ion battery for having abundant performance is not yet developed at present, therefore to its material
The research and development of material are imperative.
Invention content
In view of this, one of the objects of the present invention is to provide a kind of polyanionic compound KTi2(PO4)3And its carbon packet
The preparation method of object is covered, this method is easy to operate, is readily synthesized；The second object of the present invention is to provide polyanionic compound
KTi2(PO4)3And its material of carbon coating object, this material morphology is uniform, the mutually pure free from admixture of object；The purpose of the present invention also exists
In the offer polyanionic compound KTi2(PO4)3And its application of this material of carbon coating object, by this kind of material application
Strive for as electrode material obtaining preferable chemical property on kalium ion battery.
In order to achieve the above objectives, the present invention provides the following technical solutions：
1, polyanionic compound KTi2(PO4)3Preparation method, described method includes following steps：
A, with mass volume ratio (g：g：mL：ML it is) 1:1~2:1~2:1~2 weighs anatase titania, two water phosphorus
Acid dihydride potassium, phosphoric acid, deionized water are ground and are mixed in homogeneous solution；
B, by mixed solution described in step a, hydro-thermal reaction 6-72h obtains reaction solution under 180-240 DEG C of constant temperature；
C, reaction solution obtained by step b is cooled to 20~25 DEG C, and filtering solution obtains solid, is used in combination ethyl alcohol and deionized water clear
Solid is washed, solid is dried in vacuo 6-72h to get KTi under the conditions of temperature is 20~100 DEG C2(PO4)3。
Preferably, phosphoric acid quality score described in step a be 85%, the titanium dioxide, dihydrogen phosphate dihydrate potassium, phosphoric acid with
And deionized water quality volume ratio (g：g：mL：ML it is) 1:1:1:1.
Preferably, the reaction time described in step b is for 24 hours.
The polyanionic compound KTi prepared by the method2(PO4)3。
The polyanionic compound KTi2(PO4)3Application as kalium ion battery electrode material.
2, carbon coating polyanionic compound KTi2(PO4)3Preparation method, described method includes following steps：By quality
Than 5~9:1~5 takes KTi2(PO4)3With sucrose mixing and ball milling 6-24h, by gains be put into the tube furnace of argon atmosphere and
2-6h is annealed under 300-600 DEG C of temperature condition to get carbon-coated KTi2(PO4)3。
Preferably, the KTi2(PO4)3Mass ratio with sucrose is 8:2.
The carbon coating polyanionic compound KTi prepared by the method2(PO4)3。
The carbon coating polyanionic compound KTi2(PO4)3Application as kalium ion battery electrode material.
The beneficial effects of the present invention are：
Prepared by first passage solvent thermal process of the present invention has synthesized the KTi with nanoscale cube structure2(PO4)3With carbon
KTi after cladding2(PO4)3/ C-material.This method has lot of advantages：(1) easy to operate, using solvent thermal process, it is easy to close
At；(2) reaction temperature is relatively low, relatively mild, and yield is high；(3) raw material is the TiO that chemical property is stablized2、KH2PO4·
2H2O、 H3PO4And deionized water, it is at low cost；(4) reaction process does not have pernicious gas generation, pollution-free.Pass through a variety of method tables
Sign, products therefrom pattern is uniform, the mutually pure free from admixture of object.
The present invention has nanoscale cube structure KTi by solvent-thermal method preparation synthesis2(PO4)3With KTi2(PO4)3/C
Applied to kalium ion battery, by test comparison find it is carbon-coated under the conditions of so that its chemical property is improved.In 64mA/
It is 46.3mAh/g by the potassium discharge capacity of the cell of electrode material of KTP when g (0.5 C) current density；After carbon coating
KTP/C is that the potassium discharge capacity of the cell of electrode material is 62.5mAh/g, and has good capacity retention energy, is passed through
100 circle cycles so have good capacity performance with successor.
Description of the drawings
In order to keep the purpose of the present invention, technical solution and advantageous effect clearer, the present invention provides following attached drawing：Below
Polyanionic compound KTi in attached drawing2(PO4)3Referred to as " KTi2(PO4)3", carbon coating polyanionic compound KTi2(PO4)3
Referred to as " KTi2(PO4)3/C”。
(a) indicates there is nanoscale cube structure KTi in Fig. 12(PO4)3Scanning electron microscope (SEM) photograph, wherein (b) indicate have
Nanoscale cube structure KTi2(PO4)3The scanning electron microscope (SEM) photograph of/C；
Fig. 2 indicates KTi2(PO4)3X ray diffracting spectrum；
(a) (b) is KTi respectively in Fig. 32(PO4)3And KTi2(PO4)3/ C is under the voltage window of 1.2~2.8V with 0.2mV
s-1The CV curves for sweeping the different number of turns under speed；
(a) (b) is KTi respectively in Fig. 42(PO4)3And KTi2(PO4)3/ C is under the voltage window of 1.2~2.8V with 0.5C
The charging and discharging curve of difference number of turns when current density is tested；
(a) (b) is KTi respectively in Fig. 52(PO4)3And KTi2(PO4)3/ C is under the voltage window of 1.2~2.8V with 0.5C
Cycle performance when current density is tested.
Specific implementation mode
The preferred embodiment of the present invention is described in detail below.The experiment side of actual conditions is not specified in embodiment
Method, usually according to conventional conditions or according to the manufacturer's recommendations.
In following embodiment, polyanionic compound KTi2(PO4)3Referred to as " KTi2(PO4)3", carbon coating polyanion
Compound K Ti2(PO4)3Referred to as " KTi2(PO4)3/C”。
Embodiment 1
Polyanionic compound KTi2(PO4)3Preparation process it is specific as follows：
1) anatase titania (TiO that 0.5g average grain diameters are 25nm is weighed2), 0.5g dihydrogen phosphate dihydrate potassium
(KH2PO4·2H2O), 85% phosphoric acid (H of volume 0.5mL are measured3PO4), 0.5mL deionized waters be fully ground it is uniformly mixed.
2) mixture of above-mentioned gained is transferred to ptfe autoclave liner, puts into stainless steel casing, tightens,
It is reacted for 24 hours for 180-240 DEG C in constant temperature oven.
3) after being cooled to room temperature, product is collected by filtration, ethyl alcohol and deionized water is used in combination respectively to wash 3 times, 60 DEG C of gained powder
12h is dried in vacuo to get KTi has been arrived2(PO4)3。
Embodiment 2
Carbon coating polyanionic compound KTi2(PO4)3Preparation process it is specific as follows：
The KTi of Example 1 after drying2(PO4)3With a certain amount of sucrose (mass ratio 8:2) high-energy planetary ball mill is carried out
Gains are put into the tube furnace of argon atmosphere under the conditions of 300-600 DEG C the 2-6h that anneals to get to carbon-coated by 6-24 h
KTi2(PO4)3, KTi2(PO4)3/C。
The KTi that embodiment 1 and embodiment 2 are prepared respectively2(PO4)3And KTi2(PO4)3/ C carry out electron-microscope scanning obtain as
Scanning electron microscope (SEM) photograph shown in Fig. 1, wherein (a) indicates there is nanoscale cube structure KTi2(PO4)3Scanning electron microscope (SEM) photograph；(b)
Indicate that there is nanoscale cube structure KTi2(PO4)3The scanning electron microscope (SEM) photograph of/C.As seen from Figure 1, KTi2(PO4)3Cube knot
Configuration looks are uniform and have smaller size, KTi2(PO4)3The carbon-coating of/C claddings is than more uniform.
The KTi that embodiment 1 and embodiment 2 are prepared respectively2(PO4)3And KTi2(PO4)3/ C powder carries out X-ray diffraction,
X-ray diffractogram as shown in Figure 2 is obtained, as seen from Figure 2, the standard PDF cards for being 79-1880 with number are kissed completely
It closes, without apparent miscellaneous peak, object is mutually pure.Further, since the comparision contents of carbon coated are few and are unbodied carbon, KTi2(PO4)3/
C does not show the diffraction maximum of obvious carbon.
Application Example kalium ion battery assembles and performance test:
(1) prepared by electrode：By products therefrom (KTi2(PO4)3And KTi2(PO4)3/ C) with conductive acetylene is black and binder
PVDF in mass ratio (70:20:10) it mixes, a certain amount of 1-Methyl-2-Pyrrolidone (NMP) is added, is fully ground into paste,
It was evenly coated on diameter 14mm, on thick about 9 μm of copper foil, then it is dried in vacuo 12h for 120 DEG C.After cooling, take out spare.
(2) battery assembles：Upper step electrode slice is transferred in the glove box full of argon gas, using CR2025 type button cells
Shell, diameter 16mm metallic potassium pieces are used as to electrode, and 2325 type polypropylene films of Celgard are dissolved with 1M KPF as diaphragm6
EC and DEC (volume ratios 1:1) mixed liquor is as electrolyte.The battery standing 10h being completed is to be measured.
(3) battery performance test：Performance test carries out in Land test systems.Voltage window is 1.2-2.8V, electric current
Density is 64mA g-1。
(a) (b) is KTi respectively in Fig. 32(PO4)3And KTi2(PO4)3/ C is under the voltage window of 1.2~2.8V with 0.2mV
s-1The CV curves for sweeping the different number of turns under speed.It can be seen that by Fig. 3 (a), KTi2(PO4)3CV curves have apparent redox
Peak, and first three circle is relatively stablized；By Fig. 3 (b) it can be seen that compared to KTi2(PO4)3, KTi2(PO4)3The CV curves of/C
Other than first three circle with more obvious redox peaks, more stablized, CV area under the curve biggers show KTi2
(PO4)3/ C has higher capacity.
(a) (b) is KTi respectively in Fig. 42(PO4)3And KTi2(PO4)3/ C is under the voltage window of 1.2~2.8V with 0.5C
The charging and discharging curve of difference number of turns when current density is tested.It can be seen that by Fig. 4 (a), KTi2(PO4)3The discharge capacity of first circle is only
46.5 mAh g-1, have apparent discharge platform in 1.6V or so, but severe with the comparison for increasing its capacity attenuation of the number of turns；
It can be seen that by Fig. 4 (b), KTi2(PO4)3The discharge capacity of/C first circles is increased to 60.7mAh g-1, begin with decaying slightly it
Afterwards there are one the promotion of capacity, 76.5mAh g are reached in the 50th capacity-1, hereafter capacity have certain decaying but opposite
It is more stable, and have obvious platform, it is available capacity to show this.
(a) (b) is KTi respectively in Fig. 52(PO4)3And KTi2(PO4)3/ C is under the voltage window of 1.2~2.8V with 0.5C
Cycle performance when current density is tested.It compares for two width figures, after carbon coating, potassium battery capacity is had
Effect is promoted, and has reached nearly 70mAh g-1Charge/discharge capacity, and cyclical stability is also improved.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (9)
1. polyanionic compound KTi2(PO4)3Preparation method, which is characterized in that described method includes following steps：
A, with mass volume ratio for 1:1~2:1~2:1 ~ 2 weigh anatase titania, dihydrogen phosphate dihydrate potassium, phosphoric acid, go from
Sub- water grinds and mixes in homogeneous solution；The unit of the mass volume ratio is g：g：mL：mL；
B, by solution described in step a, hydro-thermal reaction 6-72 h obtain reaction solution under 180-240 DEG C of constant temperature；
C, reaction solution obtained by step b is cooled to 20 ~ 25 DEG C, and filtering solution obtains solid, is used in combination ethyl alcohol and deionized water to clean solid
Solid is dried in vacuo 6-72 h to get KTi by body under the conditions of temperature is 20 ~ 100 DEG C2(PO4)3。
2. polyanionic compound KTi according to claim 12(PO4)3Preparation method, which is characterized in that described in step a
Phosphoric acid quality score is 85%, and the titanium dioxide, dihydrogen phosphate dihydrate potassium, phosphoric acid and deionized water quality volume ratio are 1:
1:1:1；The unit of the mass volume ratio is g：g：mL：mL.
3. polyanionic compound KTi according to claim 12(PO4)3Preparation method, which is characterized in that described in step b
Reaction time is for 24 hours.
4. the polyanionic compound KTi prepared by any one of claim 1 ~ 3 the method2(PO4)3。
5. polyanionic compound KTi described in claim 42(PO4)3Application as kalium ion battery electrode material.
6. carbon coating polyanionic compound KTi2(PO4)3Preparation method, which is characterized in that the polyanionic compound
KTi2(PO4)3For the polyanionic compound KTi prepared by any one of claim 1 ~ 3 the method2(PO4)3；The method
Include the following steps：
In mass ratio 5 ~ 9:1 ~ 5 takes KTi2(PO4)3With sucrose mixing and ball milling 6-24 h, gains are put into the tubular type of argon atmosphere
2-6 h are annealed in stove and under 300-600 DEG C of temperature condition to get carbon-coated KTi2(PO4)3。
7. carbon coating polyanionic compound KTi according to claim 62(PO4)3Preparation method, which is characterized in that institute
State KTi2(PO4)3Mass ratio with sucrose is 8:2.
8. carbon coating polyanionic compound KTi prepared by any one of claim 6 ~ 7 the method2(PO4)3。
9. carbon coating polyanionic compound KTi described in claim 82(PO4)3Application as kalium ion battery electrode material.
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| CN106910888A (en) * | 2017-01-14 | 2017-06-30 | 复旦大学 | A kind of potassium/Prussian blue secondary cell |
| CN106887579B (en) * | 2017-04-07 | 2019-09-10 | 武汉理工大学 | Carbon-coated titanium phosphate potassium nano particle and its preparation method and application |
| CN111354943A (en) * | 2018-12-20 | 2020-06-30 | 中国科学院深圳先进技术研究院 | Use of fluorinated oxalate materials and products comprising fluorinated oxalate materials, methods of making and uses thereof |
| CN111634899B (en) * | 2020-06-14 | 2022-11-18 | 南开大学 | Preparation method for deriving and synthesizing carbon-coated titanium potassium phosphate nanoflower based on metal-organic framework |
| CN111883766B (en) * | 2020-07-30 | 2023-05-23 | 西南大学 | Polyanion electrode material and preparation method and application thereof |
| CN113394382B (en) * | 2021-06-11 | 2022-11-15 | 北京化工大学 | Potassium titanium phosphate @ carbon-reduced graphene oxide material, preparation method thereof and potassium ion battery |
| CN114639817B (en) * | 2022-04-13 | 2023-12-26 | 厦门稀土材料研究所 | Super-ion conductor KTi 2 (PO 4 ) 3 With TiO 2 Preparation and application of composite material |
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