CN115140743B - Two-dimensional metal boride and hydrothermal auxiliary alkali liquor etching preparation method and application - Google Patents
Two-dimensional metal boride and hydrothermal auxiliary alkali liquor etching preparation method and application Download PDFInfo
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Abstract
The invention discloses a two-dimensional metal boride, which is obtained by the following steps: dispersing MAB phase material in alkali solutionTransferring the suspension into a hydrothermal kettle, heating in an oven or a microwave hydrothermal box, preserving heat for proper reaction time, cooling, filtering, washing and drying to obtain the target product, namely the two-dimensional metal boride. MAB phase material comprises MoAlB, cr 2 AlB 2 、Ni 2 ZnB、WAlB、Ti 2 InB 2 、Fe 2 AlB 2 One or a mixture of two or more of the above; two-dimensional metal boride MoB, crB, ni 2 B. WB, tiB, feB. The invention also discloses a preparation method of the two-dimensional metal boride and application of the two-dimensional metal boride in preparation of lithium ion batteries. The method adopts the hydrothermal auxiliary alkali liquor etching method to prepare the MBene material, and is environment-friendly and safe. The prepared MBene material is used for a lithium ion battery, has excellent battery capacity and has wide application prospect.
Description
Technical Field
The present invention relates to a two-dimensional metal boride (MBene) material.
The invention also relates to a method for efficiently preparing the MBene material by adopting a hydrothermal auxiliary alkali liquor etching method.
The invention also relates to application of the MBene material in preparation of lithium ion batteries.
Background
In 2011, a graphene-like material, two-dimensional transition metal carbides, nitrogen and carbon-nitrogen compounds (MXene, M is a transition metal element, and X is carbon or nitrogen element), was reported by Yury Gogotsi et al (adv. Mater.2011, 23:4248-4253), of the university of Derexed, USA, the variety of which is two-dimensional transition metal carbides. Ternary ceramic MAX phase (e.g. Ti 3 AlC 2 etc.)areprecursorsforthepreparationofMXene,wheretheM-Abondstrengthisrelativelyweak,sothatthemetalbondcanberemovedbyetchingThe combined A element layer (such as Al layer) can obtain binary layered MXene (such as Ti 3 C 2 Etc.).
Recently, ade and Hillebrecht [ Inorg. Chem.2015,54:6122-6135 ] reported boron-containing element compounds similar to the MAX phase in which boron replaced the X element, this new precursor was named the MAB phase in which B represents the boron element and predicted that a new two-dimensional transition metal boride material (MBene) similar to MXene might be derived, potentially having a broad application prospect (e.g., lithium ion battery anode material) similar to MXene materials. MXene cannot be directly reacted from M and X elements due to its thermodynamic metastable nature; the property of MBene material is similar to that of the material, boron element and metal or metal chloride react to obtain metal boride particles only, so that the preparation of MXene is analogous to the strategy of etching from MAX phase, and MBene can be prepared by etching MAB phase.
As the structure is similar, the MXene etching method can be used as a reference, and although the current research of MXene materials is more, the method is limited by the fact that the etching method mostly adopts extremely toxic fluorine-containing compounds (such as the current common HCl mixed LiF etching method), and the defects of high treatment cost of wastewater generated by preparation and the like seriously limit the practical application of the MXene materials. Green fluorine-free synthesis strategies of MXene have also been reported, as reported by Wang Changda et al [ adv. Mater.2021,33,2101015 ] in which the hydrothermal method employs hydrochloric acid etching for 5 days, the reaction time is too long; the MXene is prepared by etching with alkali liquor at 270 ℃ by using a high-pressure reaction kettle, wherein the reaction temperature is too high, the equipment requirement is very high, and the method has dangerousness. The above methods have respective disadvantages and have not been used for the synthesis of MBene materials. It is not obvious whether the boride (MBene) and carbide (MXene) base properties are necessarily suitable for direct analogy or not, and no report is available, so further investigation is required. MBene synthesis has also been reported in literature, as in Wang Junjie et al [ Nat. Commun.2019,10,2284 ] using a metal alloy method, using Ti under vacuum 2 InB 2 The precursor mixed Mo powder is reacted at 1050 ℃ for 6 days to obtain the two-dimensional TiB, the method is time-consuming and has complex process, and can be seen from XRD patternsThe etching degree is low. Alameda et al [ J.am.chem.Soc.2018,140:8833-8840 ] etched aluminum molybdenum by sodium hydroxide solution only has microscopic etching effect, and the product molybdenum boride cannot be observed on XRD spectrogram, and two-dimensional metal molybdenum boride cannot be obtained macroscopically. Meanwhile, the boron element has the characteristics of easy oxidation and the like, and the oxidizing agent cannot be introduced in the etching method.
Chinese patent (application No. 202110558638.7) also reports that the removal of the A-site element in MAB phase material by a dilute alkali etching reaction results in a two-dimensional transition metal boride material, and as with the disadvantages of the above-mentioned articles, the dilute alkali etching effect is poor, only a weak manganese boride peak can be observed from the XRD pattern, and the etching degree in the precursor phase is low, which indicates that the method is not a better strategy for preparing MBene.
Chinese patent (application number 201810140682.4) adopts dilute hydrochloric acid to etch boron aluminum chromium to prepare two-dimensional chromium boride, and the XRD pattern shows that the main body etching effect is poor, the chromium boride is not the main phase, meanwhile, the chromium boride is used as the negative electrode of the lithium ion battery, and the initial specific capacity is 115mAh g -1 The specific capacity of the second circle is attenuated to 70mAh g -1 The electrode material prepared by the method has low specific capacity and has no application prospect of batteries.
In order to overcome the defects, the method for efficiently preparing the MBene material by using the MAB phase is researched in a green, fluorine-free, simple and convenient way, has very important research significance, and provides a material foundation for wide application research of the two-dimensional metal boride.
Disclosure of Invention
The invention aims to provide a two-dimensional metal boride (MBene) material.
It is still another object of the present invention to provide a method for preparing the above MBene material, i.e., a method for efficiently preparing the above MBene material by using a hydrothermal-assisted alkali etching method.
In order to achieve the above object, the two-dimensional metal boride provided by the present invention is obtained by the following method:
dispersing MAB phase material in alkali solution, transferring the suspension into a hydrothermal kettle, heating in an oven, preserving heat for proper reaction time, cooling, filtering, washing and drying to obtain the target product, namely the two-dimensional metal boride.
In the two-dimensional metal boride, the two-dimensional metal boride is MoB, crB, ni 2 B. WB, tiB, feB; MAB phase material comprises MoAlB, cr 2 AlB 2 、Ni 2 ZnB、WAlB、Ti 2 InB 2 、Fe 2 AlB 2 One or a mixture of two or more of the above.
The method for preparing the two-dimensional metal boride provided by the invention comprises the following steps:
dispersing MAB phase material in alkali solution, transferring the suspension into a hydrothermal kettle, heating in an oven or a microwave oven, performing heat preservation reaction, cooling, filtering, washing and drying to obtain the target product, namely the two-dimensional metal boride.
In the method, the two-dimensional metal boride is MoB, crB, ni 2 B. WB, tiB, feB; MAB phase material comprises MoAlB, cr 2 AlB 2 、Ni 2 ZnB、WAlB、Ti 2 InB 2 、Fe 2 AlB 2 One or a mixture of two or more of the above.
In the method, the molar ratio of the MAB phase material to the alkali in the alkali solution is 1:0.01-0.8, and the alkali is one or more than two of sodium hydroxide, potassium hydroxide, lithium hydroxide, calcium hydroxide, barium hydroxide, tetramethyl ammonium hydroxide and ammonia water.
In the method, the solvent of the alkali solution is at least one of water, ethanol and methanol.
In the method, the concentration mass ratio of the alkali solution is 15-30wt.%.
In the method, the temperature of the heat preservation reaction is 110-150 ℃; the reaction time is 2-24 hours.
In the method, the hydrothermal reaction heating mode is an oven or a microwave hydrothermal box.
The two-dimensional metal boride provided by the invention can be applied to lithium ion batteries.
The hydrothermal auxiliary alkali etching method provided by the invention is mild and green in process, does not use high-risk etchants such as hydrofluoric acid, is high in safety, and realizes green preparation of MBene materials. The novel two-dimensional material prepared by the method is used as a lithium ion battery cathode material, shows excellent specific capacity of the battery, and has wide application prospect.
Drawings
FIG. 1 is a view of an MBene scanning electron microscope prepared by the preparation method of example 1 of the present invention.
FIG. 2 shows the XRD pattern of two-dimensional molybdenum boride MBene prepared by the preparation method of example 1 of the present invention.
Fig. 3 is a charge-discharge curve diagram of two-dimensional molybdenum boride MBene prepared by the preparation method of example 1 of the present invention as a negative electrode in a lithium ion battery.
Fig. 4 is a graph showing the number of cycles of two-dimensional molybdenum boride MBene prepared by the preparation method of example 1 of the present invention as a negative electrode in a lithium ion battery.
Detailed Description
The technical scheme of the invention is as follows:
dispersing MAB phase material in alkali solution, transferring the suspension into a hydrothermal kettle, heating in an oven, preserving heat for proper reaction time, cooling, filtering, washing and drying to obtain the target product, namely the two-dimensional metal boride (MBene). And coating the two-dimensional metal boride MBene to be used as a lithium ion battery anode material. Because the etching effect of the alkali liquor is poor at normal temperature and normal pressure, the etching effect of hydroxide ions on an aluminum atomic layer in the MAB phase material can be enhanced under the high pressure effect in the hydrothermal kettle, and the ideal etching effect is achieved. The invention uses a hydrothermal auxiliary alkali liquor etching method for preparing a two-dimensional metal boride (MBene) material for the first time, and the prepared boride has excellent specific capacity in a lithium ion battery.
Alternatively, the MAB phase material comprises MoAlB, cr 2 AlB 2 、Ni 2 ZnB、WAlB、Ti 2 InB 2 、Fe 2 AlB 2 One or a mixture of two or more of the above.
Alternatively, the MBene is MoB, crB, ni 2 B. WB, tiB, feB.
Optionally, the molar ratio of the MAB phase material to the alkali in the alkali solution is 1:0.01-0.8, and the alkali is one or more than two of sodium hydroxide, potassium hydroxide, lithium hydroxide, calcium hydroxide, barium hydroxide, tetramethyl ammonium hydroxide and ammonia water.
Optionally, the solvent in the alkali solution is at least one of water, ethanol and methanol.
Optionally, the concentration mass ratio of the alkali solution is 15-30wt.%.
Optionally, the temperature of the thermal insulation reaction is 110-150 ℃; the heat preservation time is 2-24 hours.
The two-dimensional metal boride MBene can be used for preparing a negative electrode material to be applied to an ion battery, such as a lithium ion battery negative electrode.
Aiming at the defects in the prior etching technology at present, for example, the hydrofluoric acid which is a common etchant has high risk; the effect is not obvious by directly etching with alkali liquor; and the introduction of an etchant with oxidizing property is easy to oxidize boron element. The invention provides a method for preparing MBene material by MBene green hydrothermal auxiliary alkali liquor etching.
The present invention will be described in further detail below in order to make the objects, technical solutions and effects of the present invention more clear and distinct. It should be understood that the specific examples described herein are intended to illustrate the invention and are not intended to limit the invention.
Based on the above, the embodiment of the invention provides a method for preparing MBene material by green hydrothermal auxiliary alkali etching, which comprises the following steps:
s1, S1; dispersing MAB phase material in alkali solution for etching;
s2, transferring the suspension into a hydrothermal kettle, and heating in an oven or a microwave hydrothermal box;
s3, carrying out heat preservation reaction for a proper time, cooling, filtering, washing and drying to obtain a target product, namely the two-dimensional metal boride MBene;
and S4, coating the two-dimensional metal boride MBene to be used as a lithium ion battery anode material.
In the embodiment, MAB phase material is adopted as a precursor, alkali liquor is used as an etchant, MAB is dispersed in the alkali liquor, and is transferred into a hydrothermal kettle, so that the etching effect of the alkali liquor is enhanced under the auxiliary effect of hydrothermal, and finally the two-dimensional metal boride MBene material is obtained. The coating is used as a negative electrode material of a lithium ion battery, and shows excellent battery capacity.
In addition, the method for preparing the MBene material by green hydrothermal auxiliary alkali liquor etching is simple to operate, has no potential safety hazard, is suitable for large-scale industrial production, and has universality.
In step S1, in one embodiment, the MAB phase material comprises MoAlB, cr 2 AlB 2 、Ni 2 ZnB、WAlB、Ti 2 InB 2 、Fe 2 AlB 2 One or a mixture of two or more of the above.
In step S2, in one embodiment, the molar ratio of the MAB phase material to the etching base is 1:0.01-0.8, and the etching base is one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide, calcium hydroxide, barium hydroxide, tetramethylammonium hydroxide, and ammonia water.
In one embodiment, the MBene is MoB, crB, ni 2 B. WB, tiB, feB.
In one embodiment, the reaction solvent is at least one of water, ethanol, and methanol.
In one embodiment, the aqueous base has a concentration to mass ratio of 15 to 30wt.%.
In step S3, in one embodiment, the hydrothermal reaction temperature is 110-150 ℃.
In one embodiment, the etch reaction soak time is 2 to 24 hours.
In step S4, in one embodiment, the prepared two-dimensional metal boride MBene is used as a negative electrode material of a lithium ion battery.
The embodiment of the invention provides a method for preparing two-dimensional metal boride MBene in a green manner, wherein the method comprises the step of using the MBene in a lithium ion battery anode material.
In order to further explain the technical scheme of the present invention and the effects thereof, the following is further described with reference to specific examples and comparative examples.
Example 1
1. MBene (MoB) was prepared as follows:
1g of MoAlB powder and 35 ml of 25wt% sodium hydroxide solution were mixed uniformly and transferred to a 100 ml reaction vessel which was placed in an oven and incubated at 120℃for 24 hours. After cooling, the suspension was filtered, washed three times with 1 mol/liter sodium hydroxide solution, washed five times with deionized water, and the obtained powder was dried at 80 ℃ for 10 hours to obtain two-dimensional molybdenum boride MBene having an accordion-like structure, the scanning electron microscope of which is shown in fig. 1, and fig. 2 is an XRD pattern of the two-dimensional molybdenum boride MBene of the present example.
2. The MBene lithium ion battery cathode is prepared according to the following steps:
and uniformly mixing the MBene powder prepared by the steps, acetylene black and sodium alginate, wherein the mass ratio is 80:10:10, water is used as a dispersing agent, the dispersing agent is magnetically stirred for 8 hours, the slurry is coated on a copper foil on a coating machine, the copper foil is dried for 12 hours at 70 ℃, and then the copper foil is dried for 12 hours at 80 ℃ in vacuum, so that a battery cathode can be prepared and can be used for a lithium ion battery. The lithium ion CR2032 button cell is assembled in an inert atmosphere glove box, a metal lithium sheet is a counter electrode, lithium hexafluorophosphate is electrolyte, and a cell diaphragm is Celgard 2400. Charge and discharge test was performed on a blue cell test system at 50mAg -1 The first charge specific capacity and the discharge specific capacity of the battery are 645.7mAhg respectively under the current density -1 And 666.0mAhg -1 The capacity fade is not great for three cycles, as shown in fig. 3. At 2Ag -1 The capacity is still 144.2mAhg after 1000 circles of current density -1 While the unetched boron aluminum molybdenum has little capacity, as shown in fig. 4.
Comparative example 1
1g of MoAlB powder and 35 ml of 25wt% sodium hydroxide solution were mixed uniformly and transferred to a 100 ml reaction vessel which was placed in an oven and incubated at 160℃for 24 hours. The prepared MoB particles are not of a two-dimensional lamellar structure, so that the hydrothermal temperature cannot be too high.
Comparative example 2
1g of WAlB powder and 35 ml of 25wt% sodium hydroxide solution were mixed homogeneously and transferred to a 100 ml reaction vessel which was placed in an oven and incubated at 120℃for 24 hours. After cooling, the suspension is filtered, washed three times by 1 mol/liter sodium hydroxide solution, washed five times by deionized water, and the obtained powder is dried for 10 hours at 80 ℃ to obtain the two-dimensional tungsten boride MBene with the accordion structure. Under the same lithium ion battery assembly process, the lithium ion battery is assembled at 50mAg -1 The first charge specific capacity and the discharge specific capacity of the battery are 595.6mAhg respectively under the current density -1 And 603.2mAhg -1 ,. At 2Ag -1 The specific capacity is 134.5mAhg after 1000 circles of circulation under the current density -1 。
According to the embodiment, the method for preparing the two-dimensional metal boride (MBene) in a green manner is provided, wherein ternary metal boride precursors (MAB) are dispersed in alkaline solution in boride, the suspension is transferred into a hydrothermal kettle, the etching effect of the alkaline solution is enhanced under the action of hydrothermal auxiliary enhancement, and after the reaction is finished, the dispersion containing the MBene is filtered and washed to prepare the MBene material. The method adopts a hydrothermal auxiliary alkali liquor etching method for the first time to prepare the MBene material, does not adopt high-risk substances such as hydrofluoric acid in the preparation process, and is green and safe in the preparation process. The prepared MBene material is used for a lithium ion battery, has excellent battery capacity and has wide application prospect.
As can be seen from the two comparative examples, the method of the present invention is suitable for preparing MAB phase materials into two-dimensional metal borides (MBenes). Comparative example 1 the final product was granular due to the higher reaction temperature, rather than forming a two-dimensional layered structure. Comparative example 2 employed a material other than the MAB phase, and the secondary charge specific capacity and discharge specific capacity and cycle effect of the resulting product in a lithium ion battery were far less than those of example 1.
It is to be understood that the invention is not limited in its application to the examples described above, but is capable of modification and variation in light of the above teachings by those skilled in the art, and that all such modifications and variations are intended to be included within the scope of the appended claims.
Claims (4)
1. Use of a two-dimensional metal boride in a lithium ion battery, wherein the two-dimensional metal boride is obtained by:
dispersing MAB phase material in alkaline solution with concentration mass ratio of 15-30 wt%, transferring the suspension into a hydrothermal kettle, heating in an oven, reacting at 110-150deg.C for 2-24 hr, cooling, filtering, washing, and drying to obtain target product two-dimensional metal boride;
the molar ratio of the MAB phase material to the alkali in the alkali solution is 1:0.01-0.8.
2. The use according to claim 1, wherein the MAB phase material comprises MoAlB, cr 2 AlB 2 、Ni 2 ZnB、Ti 2 InB 2 、Fe 2 AlB 2 One or a mixture of two or more of the above; two-dimensional metal boride MoB, crB, ni 2 B. WB, tiB, feB.
3. The use according to claim 1, wherein the base is one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide, barium hydroxide, tetramethylammonium hydroxide, aqueous ammonia.
4. The use according to claim 1, wherein the solvent of the alkaline solution is at least one of water, ethanol, methanol.
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| DE69832073D1 (en) * | 1997-07-15 | 2005-12-01 | Silverbrook Res Pty Ltd | THERMALLY OPERATED INK JET |
| CN111204799A (en) * | 2018-11-22 | 2020-05-29 | 中国科学院金属研究所 | Preparation method of double-sided metal oxide or nitride hollow shell structure |
| CN113233470A (en) * | 2021-05-21 | 2021-08-10 | 中国科学院宁波材料技术与工程研究所 | Two-dimensional transition metal boride material, and preparation method and application thereof |
| CN114045517A (en) * | 2021-11-01 | 2022-02-15 | 无锡驭烯科技有限公司 | Ternary layered transition metal boride and preparation method and application thereof |
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| DE69832073D1 (en) * | 1997-07-15 | 2005-12-01 | Silverbrook Res Pty Ltd | THERMALLY OPERATED INK JET |
| CN111204799A (en) * | 2018-11-22 | 2020-05-29 | 中国科学院金属研究所 | Preparation method of double-sided metal oxide or nitride hollow shell structure |
| CN113233470A (en) * | 2021-05-21 | 2021-08-10 | 中国科学院宁波材料技术与工程研究所 | Two-dimensional transition metal boride material, and preparation method and application thereof |
| CN114045517A (en) * | 2021-11-01 | 2022-02-15 | 无锡驭烯科技有限公司 | Ternary layered transition metal boride and preparation method and application thereof |
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