CN113401905A - High purity phase multilayer V2Preparation method and application of material C - Google Patents
High purity phase multilayer V2Preparation method and application of material C Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title abstract description 10
- 239000012071 phase Substances 0.000 claims abstract description 41
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000002244 precipitate Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 13
- 239000007790 solid phase Substances 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 9
- 229910001416 lithium ion Inorganic materials 0.000 claims description 9
- 239000007773 negative electrode material Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 abstract description 5
- 238000001308 synthesis method Methods 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000013543 active substance Substances 0.000 description 3
- 239000010406 cathode material Substances 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 229910009819 Ti3C2 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 229910004349 Ti-Al Inorganic materials 0.000 description 1
- 229910004692 Ti—Al Inorganic materials 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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Abstract
High purity phase multilayer V2The invention discloses a preparation method and application of a C material, and relates to preparation of a high-purity-phase multilayer V2C material method, the invention is to solve the problem of the existing multilayer V etched by HF solution2The purity of C is low, and the synthesis method is complicated. The preparation method comprises the following steps: firstly, mixing 0.6-1 g V2Placing the AlC powder into 40-60 mL of HF aqueous solution with the mass concentration of 30% -50%, and stirring and reacting at room temperature for 240-288 hours to obtain a reaction solution; repeatedly centrifuging the reaction solution at 5000-12000 r/min by using a centrifuge, carrying out centrifugal cleaning until the pH value of the supernatant is 5-7, and collecting solid-phase precipitate; thirdly, drying the solid-phase precipitate. The invention controls the reaction time and the acid amount to ensure that the chemical reaction is more active and complete, and the prepared cathode has high performanceSpecific capacity, stable circulation, long service life and the like.
Description
Technical Field
The invention relates to a method for preparing high purityPhase multilayer V2Method for producing C material, and high-purity phase multilayer V2And the material C is applied as a lithium ion battery cathode material.
Background
In 2004, the graphite of Novoselov et al successfully exfoliated flakes consisting of only one layer of carbon atoms, and after the unique electronic properties of graphene were discovered, great attention was paid to two-dimensional materials. 2011, Yury Gogotsi and Barsum collaboratively discover a novel two-dimensional material Ti3C2Since then, the attention of a large number of MXenes materials has been paid. Among the MXenes materials, they have been most widely studied in the field of energy storage due to their good capacitive properties and electrical conductivity and their lower Ti-Al bond, which makes them easier to prepare. V2C is a member of MXenes materials, which also possesses surface hydrophilicity, metal conductivity and excellent electrochemical properties, but is comparable to high-purity phase Ti3C2Preparation of high purity phase multilayer V2The preparation of C is very difficult. To date, no one has corroded high purity multi-layer V2C. V was first assigned by Michael Naguib and Yury Gogotsi et al in 20132The AlC powder is immersed in HF solution to synthesize multilayer V2And C, the reaction time is 90h, and the temperature is room temperature. However V prepared by this method2C does not crystallize well by XRD and it is reported that there is about 15 wt% V2AlC does not participate in the reaction, which also means that the purity of the AlC is not high, and the AlC can reach 210mAh/g after circulation is stable under the current density of 1C through testing the electrical performance of the electrode, and the purity of the AlC is not high, so that the multilayer V cannot be completely reflected2And C is excellent in performance. In 2015, Zhou Patrio et al studied HF vs. V under different temperature and time conditions2The result of the corrosion behavior of AlC shows that V is at 50-65 DEG C2Corresponding V can not be prepared by soaking and stirring AlC powder in 49 percent HF solution for 120h2C two-dimensional crystal; after soaking for 40h at 70 ℃, a small amount of Al gradually appears2O3And V2O5And a small number of two-dimensional transparent sheet structures were observed, predicted to be V2C two-dimensional crystal, and analysis of the result shows that V cannot be successfully prepared2C, but the experimental exploration shows the relationship between HF concentration and etching temperature and time to V2The influence of the C preparation process is particularly important. In 2020, ZhangYajuan et al general V2The AlC powder is immersed into HF solution, the reaction temperature is fixed to 35 ℃, the reaction time is strictly controlled to 120h, and the generation of a multilayer structure can be observed through SEM images of the AlC powder, however, the multilayer V prepared by the method2C, in XRD pattern, V2Characteristic peak of C and V2The characteristic peak of AlC is very weak, indicating that the purity is not high, by mixing the multilayer V2C, the electrical property of the electrode is tested, and the result shows that the capacity after the circulation stabilization is 241mAh/g under the current density of 0.1A/g, because the purity is not high and V is not completely embodied2And electrical properties of the C electrode. V2C has the advantages of stable structure, good conductivity, excellent lithium storage capacity and capability of being compounded with a plurality of materials.
Disclosure of Invention
The object of the invention is to solve the problem of the prior art of etching a multilayer V with HF solutions2The C purity is low, the synthesis method is complicated, and the high-purity phase multilayer V which has high purity and simple synthesis method can be prepared2And C, a method for preparing the material.
The invention relates to a high-purity phase multilayer V2The preparation method of the material C is realized according to the following steps:
firstly, mixing 0.6-1 g V2Placing the AlC powder into 40-60 mL of HF aqueous solution with the mass concentration of 30% -50%, and stirring and reacting at room temperature for 240-288 hours to obtain a reaction solution;
repeatedly centrifuging the reaction liquid obtained in the step one at 5000-12000 r/min by using a centrifugal machine, adding deionized water for cleaning, repeating for many times, centrifuging and cleaning until the pH value of the supernatant is 5-7, and collecting solid-phase precipitate;
thirdly, drying the solid-phase precipitate obtained in the second step to obtain a high-purity-phase multilayer V2And C, material.
The invention relates to a high-purity phase multilayer V2Application of C material as negative electrode material in lithium ion batteryIn (1).
The invention adopts HF solution to etch high-purity multi-layer V for the first time2And during preparation of the material C, the dosage of the HF aqueous solution is increased to 40-60 ml, the chemical reaction time is increased to 240-288 h, and the reaction temperature is room temperature. Moderate increases in reaction time and acid levels allow the chemical reaction to proceed more actively and completely. Laminating high purity phases V2When C is used as the cathode of the lithium ion battery, the multilayer V is tested2C, the specific capacity of the negative electrode material is kept at 333.8mAh/g after circulating for 65 circles under the current density of 0.1A/g, and is kept at 109.1mAh/g after circulating for 650 circles under the current density of 2A/g, so that the negative electrode material has a series of advantages of high specific capacity, stable circulation, long service life and the like. Compared with the prior art, the invention has reasonable process, simple and convenient operation and excellent performance, and is a lithium ion battery cathode material with application prospect.
Drawings
FIG. 1 shows the high-purity phase multilayer V obtained in example I2XRD pattern of material C;
FIG. 2 shows the high-purity phase multilayer V obtained in example one2EDX plot of material C;
FIG. 3 shows the high-purity phase multilayer V obtained in example one2SEM image of material C;
FIG. 4 shows the high-purity phase multilayer V obtained in example one2C material under the current density of 0.1A/g charge-discharge cycle test chart, wherein 1-cycle efficiency, 2-specific discharge capacity, 3-specific charge capacity;
FIG. 5 shows the high-purity multi-layer V obtained in example one2C, a charge-discharge cycle test chart of the material under different current densities, wherein 1 is discharge specific capacity, and 2 is charge specific capacity;
FIG. 6 shows the high-purity multi-layer V obtained in example one2C, a charge-discharge cycle test chart of the material under the current density of 2A/g, wherein an upper curve represents cycle efficiency, and a lower curve represents discharge specific capacity;
FIG. 7 shows the high-purity multi-layer V obtained in example one2CV curve test chart of C material, wherein 1 represents 5.0mVs-1And 2 represents 2.0mVs-1And 3 represents 1.0mVs-1And 4 represents 0.5mVs -15 th generationTABLE 0.1mVs-1；
FIG. 8 shows the high purity phase multilayer V obtained in example one2EIS map of material C.
Detailed Description
The first embodiment is as follows: the high purity phase multilayer V of the present embodiment2The preparation method of the material C is implemented according to the following steps:
firstly, mixing 0.6-1 g V2Placing the AlC powder into 40-60 mL of HF aqueous solution with the mass concentration of 30% -50%, and stirring and reacting at room temperature for 240-288 hours to obtain a reaction solution;
repeatedly centrifuging the reaction solution obtained in the step one at 6000-12000 r/min by using a centrifugal machine, adding deionized water for cleaning, repeating for many times, centrifuging and cleaning until the pH value of the supernatant is 5-7, and collecting solid-phase precipitate;
thirdly, drying the solid-phase precipitate obtained in the second step to obtain a high-purity-phase multilayer V2And C, material.
The high purity phase multilayer V of the present embodiment2The C material is a high-purity phase multilayer V formed by etching with HF solution2C。
The second embodiment is as follows: the difference between the first embodiment and the second embodiment is that V is described in the first step2The grain size of AlC powder is 200 meshes.
The third concrete implementation mode: the difference between this embodiment and the first or second embodiment is that V is the first step2The volume ratio of the mass of the AlC powder to the HF aqueous solution is 1 g: 52-58 mL.
The fourth concrete implementation mode: this embodiment differs from one of the first to third embodiments in that 0.8gV is added in the first step2Placing the AlC powder into 40-50 mL of HF aqueous solution with the mass concentration of 30% -50%.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is that in the first step, the reaction is performed at room temperature for 250 to 270 hours with stirring.
The sixth specific implementation mode: the present embodiment is different from the first to fifth embodiments in that the repeated centrifugation is performed at 7000r/min to 9000r/min by using a centrifuge in the second step.
The seventh embodiment: this embodiment differs from one of the first to sixth embodiments in that the time for each centrifugation in step two is 5 minutes.
The specific implementation mode is eight: the present embodiment is different from the first to seventh embodiments in that the second step is repeated 6 to 8 times.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is that the solid phase precipitate is vacuum dried in step three, the vacuum drying temperature is 60 ℃, and the drying time is 12 h.
The detailed implementation mode is ten: this embodiment combines high purity phases into a multilayer V2The C material is used as a negative electrode material and applied to the lithium ion battery.
The first embodiment is as follows: this example high purity phase multilayer V2The preparation method of the material C is implemented according to the following steps:
firstly, 0.8g V2Placing AlC powder (200 meshes) into 45mL of HF aqueous solution with the mass concentration of 40%, and stirring and reacting for 264 hours at room temperature to obtain reaction liquid;
repeatedly centrifuging the reaction liquid obtained in the step one at 8000r/min by adopting a centrifuge, adding deionized water for cleaning, wherein the centrifuging time is 5 minutes each time, separating supernate from precipitate in each cleaning process, adding deionized water into the precipitate, shaking up, centrifuging again for multiple times, centrifugally cleaning until the pH value of the supernate is 6, and collecting solid-phase precipitate;
thirdly, carrying out vacuum drying treatment on the solid-phase precipitate obtained in the second step, wherein the vacuum drying temperature is 60 ℃, and the drying time is 12 hours, so as to obtain the high-purity-phase multilayer V2And C, material.
The high purity phase multilayer V obtained in this example2XRD of C material is shown in figure 1, from which Nb can be seen2The diffraction peak of the AlC powder at 41.3 degrees basically disappears completely after corrosion, and the 002 peak is advanced to 9.1 degrees from the original 13.5 degrees. To this end, it can be shown that V was successfully synthesized2And C, material.
FIG. 2 is V2EDX spectrum of C with V, C, O, F and Al atomic ratio of 2.03:106:0.79:0.06, it can be seen that the Al content is very small, indicating that the high-purity-phase multilayer V was successfully synthesized2And C, material.
FIG. 3 is a high purity phase multilayer V2SEM photograph of material C, illustrating the structure of the multilayer.
FIGS. 4 to 8 are high purity phase multilayers V2C electrochemical performance test chart of material, a little V2Grinding the C material into powder as an active substance, mixing the active substance with acetylene black and polyvinylidene fluoride into slurry according to the mass ratio of 7:1.5:1.5, coating the slurry on copper foil to prepare an electrode sheet, drying the electrode sheet, pressing the electrode sheet into a 13mm electrode sheet by using a hand-press punching machine after drying, then preparing the electrode sheet into a button type lithium ion battery in a glove box, and then testing the electrochemical performance of the button type lithium ion battery, wherein as can be seen from figure 4, the current density of 0.1A/g circulates for 65 circles, the specific capacity is kept at 333.8mAh/g (reported by Michael Naguib, Yury Gogotsi and the like, and under the current density of 1C, the circulation stability can reach 210mAh/g, reported by ZhangYajuan and the like, and under the current density of 0.1A/g, V is used as an active substance2The capacity after C circulation stabilization is 241mAh/g), and the coulombic efficiency is close to 100%. Fig. 5 is a charge-discharge cycle test plot at different current densities showing good rate performance. As can be seen from FIG. 6, the high purity phase multilayer V2The C negative electrode material circulates 650 circles under the current density of 2A/g, the specific capacity is kept at 109.1mAh/g, and the coulombic efficiency is close to 100%. FIG. 7 is the drawing V2The CV curve of the C material illustrates the capacitive behavior at different sweep rates. FIG. 8 is the drawing V2The EIS map of the material C shows that the material has smaller charge transfer resistance and good particle diffusion capacity. Taken together, it is shown that the high purity phase multilayer V2The C material is a promising lithium ion battery cathode material.
Claims (10)
1. High purity phase multilayer V2The preparation method of the material C is characterized by comprising the following steps:
firstly, mixing 0.6-1 g V2Placing the AlC powder into 40-60 mL of HF aqueous solution with the mass concentration of 30% -50%, and stirring and reacting at room temperature for 240-288 hours to obtain a reaction solution;
repeatedly centrifuging the reaction liquid obtained in the step one at 5000-12000 r/min by using a centrifugal machine, adding deionized water for cleaning, repeating for many times, centrifuging and cleaning until the pH value of the supernatant is 5-7, and collecting solid-phase precipitate;
thirdly, drying the solid-phase precipitate obtained in the second step to obtain a high-purity-phase multilayer V2And C, material.
2. The high purity phase multilayer V of claim 12The preparation method of the material C is characterized in that the V in the step one2The grain size of AlC powder is 200 meshes.
3. The high purity phase multilayer V of claim 12The preparation method of the C material is characterized in that V in the step one2The volume ratio of the mass of the AlC powder to the HF aqueous solution is 1 g: 52-58 mL.
4. The high purity phase multilayer V of claim 12The preparation method of the material C is characterized in that 0.8g V is added in the step one2Placing the AlC powder into 40-50 mL of HF aqueous solution with the mass concentration of 30% -50%.
5. The high purity phase multilayer V of claim 12The preparation method of the material C is characterized in that in the step one, the material C is stirred and reacts for 250-270 hours at room temperature.
6. The high purity phase multilayer V of claim 12The preparation method of the material C is characterized in that a centrifuge is adopted in the second step to repeatedly centrifuge at 7000 r/min-9000 r/min.
7. The high purity phase multilayer V of claim 12And C, a preparation method of the material C, which is characterized in that the time of each centrifugation in the step two is 5 minutes.
8. The high purity phase multilayer V of claim 12The preparation method of the material C is characterized in that the step two is repeated for 6-8 times.
9. The high purity phase multilayer V of claim 12The preparation method of the material C is characterized in that the solid-phase precipitate in the step three is subjected to vacuum drying treatment, the vacuum drying temperature is 60 ℃, and the drying time is 12 hours.
10. High purity phase multilayer V2Use of C materials, characterised in that high-purity phases are laminated V2The C material is used as a negative electrode material and applied to the lithium ion battery.
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