CN105826521A - Polyanion compound KTi2(PO4)3, preparation of carbon coating thereof and application of product of polyanion compound KYi(PO4)3 - Google Patents
Polyanion compound KTi2(PO4)3, preparation of carbon coating thereof and application of product of polyanion compound KYi(PO4)3 Download PDFInfo
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- CN105826521A CN105826521A CN201610310715.6A CN201610310715A CN105826521A CN 105826521 A CN105826521 A CN 105826521A CN 201610310715 A CN201610310715 A CN 201610310715A CN 105826521 A CN105826521 A CN 105826521A
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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 a polyanion compound KYi(PO4)3, a preparation method of a carbon coating thereof and application of a product of the polyanion compound KYi(PO4)3 and the polyanion compound KYi(PO4)3 as a potassium ion battery electrode material. The method has the advantages that operation is easy and convenient, a solvothermal method is adopted, and synthesis is easy; the reaction temperature is low, reactions are mild, and the yield is high; raw materials are TiO2, KH2PO4.2H2O, H3PO4 and deionized water with the stable chemical properties, and the cost is low; no harmful gas is generated in the reaction process, and no pollution is caused. Various methods show that the product is uniform in morphology, the phase is pure, and no impurity is generated. The KYi2(PO4)3 and KTi2(PO4)3/C with the nanoscale cube structures are applied to a potassium ion battery, and tests show that the electrochemical performance of the potassium ion battery is good, and the electrochemical performance of KTi2(PO4)3/C is better.
Description
Technical field
The invention belongs to kalium ion battery Material Field, be specifically related to a kind of polyanionic compound KTi2(PO4)3And the preparation of carbon coating and products thereof and application.
Background technology
Energy resource consumption is the key character of modern social development, and efficient energy-storage system is then the core pillar of regenerative resource industry, consumer electronics industry, transportation industry.In many energy storage modes, lithium ion battery, with advantages such as light weight, capacity height and memory-less effects, occupies core status in current energy storage industry.Due to lithium ion battery high-energy-density and good cycle performance so that it is use and expand to electric automobile and mixed power electric car from portable electric appts.But, lithium resource rare and skewness, add that growing consumption makes its cost constantly rise, thus limit its large-scale application widely.But, by contrast, potassium resource is abundant and cost is at a fairly low.As one of alkali metal, potassium and lithium, there is similar physical/chemical.
Furthermore, it has been reported that careful professor in Tokyo university of science coltfoal field et al. have found breach in the research and development of a new generation's kalium ion battery technology.Research worker uses graphite electrode to be successfully realized repeatedly discharge and recharge in the case of not reducing performance.The novel battery using this technology is expected to improve 10 times than the charge/discharge rates of lithium ion battery, and can corresponding high-intensity currrent, export bigger electric power, can be applicable to the electrically driven treadmill higher to instantaneous speed-raising requirement.The when of using potassium ion, voltage can drop to-0.09 volt, and the voltage of the conventional batteries such as lithium ion cannot drop to negative value.So far, battery capacity to be improved only is improved cathode voltage one method, and kalium ion battery is expected to make global voltage exceed the batteries such as lithium ion by reduction cathode voltage.Potassium, lithium, sodium are all alkaline elements.Comparing with lithium, potassium ion movement in the electrolytic solution is more active, is more suitable for charging at short notice and a large amount of electric currents of disposable release, output high-power.At present, there is charging interval long problem in electric automobile, if charging can be completed at short notice, will improve the convenience of electric automobile.Additionally, the structure of kalium ion battery is essentially the same with lithium ion battery, can produce on identical production line.Additionally, potassium ion has good deintercalation performance in electrode material, and among alkali metal, for metallic sodium, the current potential of potassium is closest to lithium metal.In worldwide, the most not yet developing the electrode material of the kalium ion battery possessing abundant performance, therefore the research and development to its material are imperative.
Summary of the invention
In view of this, an object of the present invention is to provide a kind of polyanionic compound KTi2(PO4)3And the preparation method of carbon coating, the method is easy and simple to handle, is readily synthesized；The two of the purpose of the present invention are to provide polyanionic compound KTi2(PO4)3And the material of carbon coating, this material morphology is homogeneous, the mutually pure free from admixture of thing；The present invention also aims to provide described polyanionic compound KTi2(PO4)3And the application of this material of carbon coating, strive for obtaining preferable chemical property as electrode material on kalium ion battery using this kind of materials application.
For reaching above-mentioned purpose, the invention provides following technical scheme:
1, polyanionic compound KTi2(PO4)3Preparation method, described method comprises the steps:
A, with mass volume ratio (g:g:mL:mL), as 1:1～2:1～2:1～2 weighs anatase titania, dihydrogen phosphate dihydrate potassium, phosphoric acid, deionized water grind and mix in homogeneous solution；
B, hydro-thermal reaction 6-72h under 180-240 DEG C of constant temperature of mixed solution described in step a is obtained reaction solution；
C, step b gained reaction solution are cooled to 20～25 DEG C, and filtering solution obtains solid, and cleans solid with ethanol and deionized water, solid is vacuum dried under the conditions of temperature is 20～100 DEG C 6-72h, obtains KTi2(PO4)3。
Preferably, phosphoric acid quality mark described in step a is 85%, and described titanium dioxide, dihydrogen phosphate dihydrate potassium, phosphoric acid and deionized water quality volume ratio (g:g:mL:mL) are 1:1:1:1.
Preferably, the response time described in step b is 24h.
The polyanionic compound KTi prepared by described method2(PO4)3。
Described polyanionic compound KTi2(PO4)3Application as kalium ion battery electrode material.
2, carbon cladding polyanionic compound KTi2(PO4)3Preparation method, described method comprises the steps: that in mass ratio 5～9:1～5 take KTi2(PO4)3With sucrose mixing and ball milling 6-24h, gains are put in the tube furnace of argon atmosphere and the 2-6h that anneals under 300-600 DEG C of temperature conditions, obtain the KTi of carbon cladding2(PO4)3。
Preferably, described KTi2(PO4)3It is 8:2 with the mass ratio of sucrose.
The carbon cladding polyanionic compound KTi prepared by described method2(PO4)3。
Described carbon cladding polyanionic compound KTi2(PO4)3Application as kalium ion battery electrode material.
The beneficial effects of the present invention is:
First passage solvent thermal process of the present invention preparation has synthesized the KTi with nanoscale cube structure2(PO4)3KTi after being coated with carbon2(PO4)3/ C-material.The method has lot of advantages: (1) is easy and simple to handle, uses solvent thermal process, is readily synthesized；(2) reaction temperature ratio is relatively low, relatively mild, and productivity is high；(3) raw material is the TiO of stable chemical nature2、KH2PO4·2H2O、H3PO4And deionized water, low cost；(4) course of reaction does not has harmful gas to produce, pollution-free.Being characterized by multiple method, products therefrom pattern is homogeneous, the mutually pure free from admixture of thing.
The present invention has nanoscale cube structure KTi by solvent-thermal method preparation synthesis2(PO4)3With KTi2(PO4)3/ C is applied to kalium ion battery, makes its chemical property be improved under conditions of test comparison finds carbon cladding.When 64mA/g (0.5C) electric current density, the potassium discharge capacity of the cell with KTP as electrode material is as 46.3mAh/g；The KTP/C after being coated with the carbon potassium discharge capacity of the cell as electrode material is as 62.5mAh/g, and has good capacity retention energy, so has good capacity to show through 100 circle circulations with successor.
Accompanying drawing explanation
In order to make the purpose of the present invention, technical scheme and beneficial effect clearer, the present invention provides drawings described below: polyanionic compound KTi in the following drawings2(PO4)3Referred to as " KTi2(PO4)3", carbon cladding polyanionic compound KTi2(PO4)3Referred to as " KTi2(PO4)3/C”。
In Fig. 1, (a) represents have nanoscale cube structure KTi2(PO4)3Scanning electron microscope (SEM) photograph, wherein (b) represent there is nanoscale cube structure KTi2(PO4)3The scanning electron microscope (SEM) photograph of/C；
Fig. 2 represents KTi2(PO4)3X ray diffracting spectrum；
In Fig. 3, (a) (b) is KTi respectively2(PO4)3And KTi2(PO4)3/ C under the voltage window of 1.2～2.8V with 0.2mVs-1The CV curve sweeping under speed the different number of turns；
In Fig. 4, (a) (b) is KTi respectively2(PO4)3And KTi2(PO4)3The charging and discharging curve of difference number of turns when/C tests with 0.5C electric current density under the voltage window of 1.2～2.8V；
In Fig. 5, (a) (b) is KTi respectively2(PO4)3And KTi2(PO4)3Cycle performance when/C tests with 0.5C electric current density under the voltage window of 1.2～2.8V.
Detailed description of the invention
Below the preferred embodiments of the present invention are described in detail.The experimental technique of unreceipted actual conditions in embodiment, generally according to normal condition or according to the condition proposed by manufacturer.
In following example, polyanionic compound KTi2(PO4)3Referred to as " KTi2(PO4)3", carbon cladding polyanionic compound KTi2(PO4)3Referred to as " KTi2(PO4)3/C”。
Embodiment 1
Polyanionic compound KTi2(PO4)3Preparation process specific as follows:
1) anatase titania (TiO that 0.5g mean diameter is 25nm is weighed2), 0.5g dihydrogen phosphate dihydrate potassium (KH2PO4·2H2O), volume 0.5mL85% phosphoric acid (H is measured3PO4), 0.5mL deionized water be fully ground mix homogeneously.
2) mixture of above-mentioned gained is transferred to politef reactor inner bag, put into stainless steel casing, tighten, 180-240 DEG C of reaction 24h in constant temperature oven.
3) after being cooled to room temperature, product is collected by filtration, and respectively washes 3 times with ethanol and deionized water, 60 DEG C of gained powder vacuum drying 12h, i.e. obtain KTi2(PO4)3。
Embodiment 2
Carbon cladding polyanionic compound KTi2(PO4)3Preparation process specific as follows:
Example 1 KTi after drying2(PO4)3Carry out high-energy planetary ball mill 6-24h with a certain amount of sucrose (mass ratio 8:2), gains are put into the 2-6h that anneals under the conditions of 300-600 DEG C in the tube furnace of argon atmosphere, has i.e. obtained the KTi of carbon cladding2(PO4)3, KTi2(PO4)3/C。
The KTi that embodiment 1 and embodiment 2 are prepared respectively2(PO4)3And KTi2(PO4)3/ C carries out electron-microscope scanning and obtains scanning electron microscope (SEM) photograph as shown in Figure 1, and wherein (a) represents have nanoscale cube structure KTi2(PO4)3Scanning electron microscope (SEM) photograph；B () represents have nanoscale cube structure KTi2(PO4)3The scanning electron microscope (SEM) photograph of/C.As seen from Figure 1, KTi2(PO4)3Cube structure pattern is homogeneous and has less size, KTi2(PO4)3The carbon-coating ratio of/C cladding is 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, obtains X-ray diffractogram as shown in Figure 2, and as seen from Figure 2, it fits like a glove with the standard PDF card of numbered 79-1880, and without obvious miscellaneous peak, thing is mutually pure.Additionally, due to the comparision contents of carbon coated is few and be unbodied carbon, KTi2(PO4)3/ C does not demonstrate the diffraction maximum of obvious carbon.
The assembling of Application Example kalium ion battery and performance test:
(1) prepared by electrode: by products therefrom (KTi2(PO4)3And KTi2(PO4)3/ C) black with conductive acetylene in binding agent PVDF in mass ratio (70:20:10) mix, add a certain amount of 1-Methyl-2-Pyrrolidone (NMP), it is fully ground into pasty state, it is uniformly coated on diameter 14mm, on the Copper Foil of thick about 9 μm, then 120 DEG C of vacuum drying 12h.After cooling, take out standby.
(2) battery assembling: being transferred to upper step electrode slice be full of in the glove box of argon, use CR2025 type button cell shell, diameter 16mm metallic potassium sheet is as to electrode, and Celgard2325 type polypropylene film, as barrier film, is dissolved with 1MKPF6The mixed liquor of EC and DEC (volume ratio 1:1) as electrolyte.The battery standing 10h being completed is to be measured.
(3) battery performance test: performance test is carried out in Land test system.Voltage window is 1.2 2.8V, and electric current density is 64mAg-1。
In Fig. 3, (a) (b) is KTi respectively2(PO4)3And KTi2(PO4)3/ C under the voltage window of 1.2～2.8V with 0.2mVs-1The CV curve sweeping under speed the different number of turns.Be can be seen that by Fig. 3 (a), KTi2(PO4)3CV curve there is obvious oxidoreduction peak, and first three circle is the most stable；By Fig. 3 (b) it can be seen that compared to KTi2(PO4)3, KTi2(PO4)3The CV curve of/C is in addition to having more obvious oxidoreduction peak, first three more stable circle, and its CV area under the curve is bigger, shows KTi2(PO4)3/ C has higher capacity.
In Fig. 4, (a) (b) is KTi respectively2(PO4)3And KTi2(PO4)3The charging and discharging curve of difference number of turns when/C tests with 0.5C electric current density under the voltage window of 1.2～2.8V.Be can be seen that by Fig. 4 (a), KTi2(PO4)3The discharge capacity of first circle is only 46.5mAhg-1, there is obvious discharge platform at about 1.6V, but along with the comparison increasing its capacity attenuation of the number of turns is severe；Be can be seen that by Fig. 4 (b), KTi2(PO4)3The discharge capacity of/C first circle brings up to 60.7mAhg-1, after beginning with decay somewhat, have the lifting of a capacity, reached 76.5mAhg at the 50th capacity-1, hereafter capacity has had certain decay but the most stable, and has obvious platform, and indicating this is available capacity.
In Fig. 5, (a) (b) is KTi respectively2(PO4)3And KTi2(PO4)3Cycle performance when/C tests with 0.5C electric current density under the voltage window of 1.2～2.8V.Comparing for two width figures, after carbon is coated with, its potassium battery capacity has obtained effective lifting, has reached nearly 70mAhg-1Charge/discharge capacity, and cyclical stability is also improved.
Finally illustrate is, preferred embodiment above is only in order to illustrate technical scheme and unrestricted, although the present invention being described in detail by above preferred embodiment, but skilled artisan would appreciate that, in the form and details it can be made various change, without departing from claims of the present invention limited range.
Claims (9)
1. polyanionic compound KTi2(PO4)3Preparation method, it is characterised in that described method comprises the steps:
A, with mass volume ratio (g:g:mL:mL), as 1:1～2:1～2:1～2 weighs anatase titania, dihydrogen phosphate dihydrate potassium, phosphoric acid, deionized water grind and mix in homogeneous solution；
B, hydro-thermal reaction 6-72h under 180-240 DEG C of constant temperature of solution described in step a is obtained reaction solution；
C, step b gained reaction solution are cooled to 20～25 DEG C, and filtering solution obtains solid, and cleans solid with ethanol and deionized water, solid is vacuum dried under the conditions of temperature is 20～100 DEG C 6-72h, obtains KTi2(PO4)3。
Polyanionic compound KTi the most according to claim 12(PO4)3Preparation method, it is characterised in that phosphoric acid quality mark described in step a is 85%, and described titanium dioxide, dihydrogen phosphate dihydrate potassium, phosphoric acid and deionized water quality volume ratio (g:g:mL:mL) are 1:1:1:1.
Polyanionic compound KTi the most according to claim 12(PO4)3Preparation method, it is characterised in that the response time described in step b is 24h.
4. the polyanionic compound KTi prepared by method described in any one of claims 1 to 32(PO4)3。
5. polyanionic compound KTi described in claim 42(PO4)3Application as kalium ion battery electrode material.
6. carbon cladding polyanionic compound KTi2(PO4)3Preparation method, it is characterised in that described method comprises the steps: that in mass ratio 5～9:1～5 take KTi2(PO4)3With sucrose mixing and ball milling 6-24h, gains are put in the tube furnace of argon atmosphere and the 2-6h that anneals under 300-600 DEG C of temperature conditions, obtain the KTi of carbon cladding2(PO4)3。
Carbon cladding polyanionic compound KTi the most according to claim 62(PO4)3Preparation method, it is characterised in that described KTi2(PO4)3It is 8:2 with the mass ratio of sucrose.
8. the carbon cladding polyanionic compound KTi that prepared by method described in any one of claim 6～72(PO4)3。
9. carbon cladding polyanionic compound KTi described in claim 82(PO4)3Application as kalium ion battery electrode material.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106887579A (en) * | 2017-04-07 | 2017-06-23 | 武汉理工大学 | Titanium phosphate potassium nano particle of carbon coating and its preparation method and application |
| CN106910888A (en) * | 2017-01-14 | 2017-06-30 | 复旦大学 | A kind of potassium/Prussian blue secondary cell |
| WO2020124648A1 (en) * | 2018-12-20 | 2020-06-25 | 中国科学院深圳先进技术研究院 | Application of fluorinated oxalate material, and product containing fluorinated oxalate material and preparation method therefor and use thereof |
| CN111634899A (en) * | 2020-06-14 | 2020-09-08 | 南开大学 | Preparation method for deriving and synthesizing carbon-coated titanium potassium phosphate nanoflower based on metal-organic framework |
| CN111883766A (en) * | 2020-07-30 | 2020-11-03 | 西南大学 | Polyanion electrode material and preparation method and application thereof |
| CN113394382A (en) * | 2021-06-11 | 2021-09-14 | 北京化工大学 | Titanium potassium phosphate @ carbon-redox graphene material, preparation method thereof and potassium ion battery |
| CN114639817A (en) * | 2022-04-13 | 2022-06-17 | 厦门稀土材料研究所 | Super ion conductor KTi2(PO4)3With TiO2Preparation and use of composite materials |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106910888A (en) * | 2017-01-14 | 2017-06-30 | 复旦大学 | A kind of potassium/Prussian blue secondary cell |
| CN106887579A (en) * | 2017-04-07 | 2017-06-23 | 武汉理工大学 | Titanium phosphate potassium nano particle of carbon coating and its preparation method and application |
| WO2020124648A1 (en) * | 2018-12-20 | 2020-06-25 | 中国科学院深圳先进技术研究院 | Application of fluorinated oxalate material, and product containing fluorinated oxalate material and preparation method therefor and use thereof |
| CN111634899A (en) * | 2020-06-14 | 2020-09-08 | 南开大学 | Preparation method for deriving and synthesizing carbon-coated titanium potassium phosphate nanoflower based on metal-organic framework |
| CN111883766A (en) * | 2020-07-30 | 2020-11-03 | 西南大学 | Polyanion electrode material and preparation method and application thereof |
| CN113394382A (en) * | 2021-06-11 | 2021-09-14 | 北京化工大学 | Titanium potassium phosphate @ carbon-redox graphene material, preparation method thereof and potassium ion battery |
| CN114639817A (en) * | 2022-04-13 | 2022-06-17 | 厦门稀土材料研究所 | Super ion conductor KTi2(PO4)3With TiO2Preparation and use of composite materials |
| 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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