CN115140743A - 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 method: and dispersing the MAB phase material in an alkali solution, transferring the suspension into a hydrothermal kettle, heating in an oven or a microwave hydrothermal box, keeping the temperature for reacting for a proper time, cooling, filtering, washing and drying to obtain the target product, namely the two-dimensional metal boride. MAB phase material comprises MoAlB and 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 (a); the two-dimensional metal boride is MoB, crB and Ni 2 B. At least one of WB, tiB and 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 a lithium ion battery. The invention adopts the hydrothermal auxiliary alkali liquor etching method to prepare MBene materialGreen and safe. The prepared MBene material is used for lithium ion batteries, shows excellent battery capacity and has wide application prospect.
Description
Technical Field
The 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 a lithium ion battery.
Background
In 2011, yury gootsi et al [ adv. Mater.2011, 23. Ternary ceramic MAX phases (e.g. Ti) 3 AlC 2 Etc.) is a precursor for preparing MXene, wherein the bonding strength of M-A bond is relatively weak, so that the A element layer (such as Al layer) bonded by metal bond can be removed by etching to obtain binary layered MXene (such as Ti layer) 3 C 2 Etc.).
Recently, ade and Hillebrecht [ inorg. Chem.2015, 54. MXene cannot be directly formed by directly reacting M and X elements due to the thermodynamic metastable property of MXene; the properties of MBene material are similar to that of MBene material, only metal boride particles can be obtained by reacting boron with metal or metal chloride, so the MBene can be prepared by etching MAB phase compared with the strategy of preparing MXene by etching from MAX phase.
With similar structure, MXene etching method can be used as referenceAlthough many researches are carried out on the MXene material at present, the MXene material is limited by the defects that the etching method mostly adopts a highly toxic fluorine-containing compound (such as the existing common HCl mixed LiF etching method), the treatment cost of wastewater generated by preparation is high, and the like, and the practical application of the MXene material is severely restricted. MXene's green fluorine-free synthesis strategy is also reported, such as Wang Changda et al [ adv. Mater.2021,33,2101015 ] reported that the hydrothermal method adopts hydrochloric acid etching reaction for 5 days, and the reaction time is too long; li Tengfei et al (Angew. Chem. Int. Edit.2018,57, 6115-6119) use alkaline liquor to etch and prepare MXene under the condition of 270 ℃ of a high-pressure reaction kettle, and the method has too high reaction temperature, very high equipment requirement and danger. The above methods all have their own disadvantages and have not been used for the synthesis of MBene materials. Because of the great difference between the basic properties of boride (MBene) and carbide (MXene), it is not obvious and reported that the boride (MBene) and carbide (MXene) are suitable for direct analogy, and further exploration is needed. MBene synthesis has also been reported in the literature, for example, by Wang Junjie et al [ nat. Commun.2019,10,2284 ] using a metal alloy method with Ti under vacuum 2 InB 2 The precursor mixed Mo powder reacts for 6 days at 1050 ℃ to obtain the two-dimensional TiB, the method is time-consuming and complex in process, and the etching degree is low as can be seen from an XRD (X-ray diffraction) pattern. Alameda et al [ J.Am.chem.Soc.2018,140:8833-8840 ] adopt sodium hydroxide solution to etch boron-aluminum-molybdenum, only microscopic etching effect can be achieved, the product molybdenum boride cannot be observed on an XRD spectrogram, and two-dimensional metal molybdenum boride cannot be obtained macroscopically. Meanwhile, boron has the characteristics of easy oxidation and the like, and an oxidant cannot be introduced by an etching method.
Chinese patent (application No. 202110558638.7) also reports that a-site element in MAB phase material is removed by adopting dilute alkali solution etching reaction to obtain two-dimensional transition metal boride material, and like the defects of the above mentioned article, the dilute alkali solution etching effect is not good, only weak manganese boride peak can be observed from the XRD diagram, the etching degree of precursor phase is very 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 also can see main body etching from XRD patternThe corrosion effect is poor, the chromium boride is not a main phase, and meanwhile, the chromium boride is used as a lithium ion battery cathode, and the primary 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 too low specific capacity and has no battery application prospect.
In order to overcome the defects, the research on the method which is green, fluoride-free, simple and convenient and is suitable for etching the MAB phase to efficiently prepare the MBene material has very important research significance, and provides a material basis for the wide application research of the two-dimensional metal boride.
Disclosure of Invention
The invention aims to provide a two-dimensional metal boride (MBene) material.
The invention also aims to provide a method for preparing the MBene material, namely a method for efficiently preparing the MBene material by using a hydrothermal auxiliary alkali liquor etching method.
In order to achieve the purpose, the two-dimensional metal boride provided by the invention is obtained by the following method:
and dispersing the MAB phase material in an alkali solution, transferring the suspension into a hydrothermal kettle, heating in an oven, carrying out heat preservation reaction for a proper 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 and Ni 2 B. At least one of WB, tiB and FeB; MAB phase material comprises MoAlB and 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 them.
The invention provides a method for preparing the two-dimensional metal boride, which comprises the following steps:
and dispersing the MAB phase material in an alkali solution, transferring the suspension into a hydrothermal kettle, heating in an oven or a microwave oven, carrying out 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 and Ni 2 B. At least one of WB, tiB and FeB; MAB phase materialComprises MoAlB and 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 them.
In the method, the molar ratio of the MAB phase material to alkali in the alkali solution is 1.01-0.8, and the alkali is one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide, calcium hydroxide, barium hydroxide, tetramethylammonium 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 kept for 2 to 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 liquor etching method provided by the invention is used for etching the MAB phase material, the process is mild and green, a high-risk etching agent such as hydrofluoric acid is not used, the safety is high, and the green preparation of the MBene material is realized. 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 scanning electron micrograph of MBene prepared by the preparation method of example 1 of the present invention.
FIG. 2 is an XRD pattern of two-dimensional molybdenum boride MBene prepared by the preparation method of the embodiment 1 of the invention.
Fig. 3 is a charge-discharge curve diagram of the two-dimensional molybdenum boride MBene prepared by the preparation method of the embodiment 1 as the negative electrode in the lithium ion battery.
Fig. 4 is a cycle number diagram of the two-dimensional molybdenum boride MBene prepared by the preparation method of the embodiment 1 as the negative electrode in the lithium ion battery.
Detailed Description
The technical scheme of the invention is as follows:
and dispersing the MAB phase material in an alkali solution, transferring the suspension into a hydrothermal kettle, heating in an oven, 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 (3) coating the two-dimensional metal boride MBene to be used as a lithium ion battery negative electrode material. Because the etching effect of the alkali liquor is poor at normal temperature and normal pressure, the etching effect of hydroxyl ions on an aluminum atom layer in the MAB phase material can be enhanced under the action of high pressure in the hydrothermal kettle, and an ideal etching effect is achieved. The invention firstly uses the hydrothermal auxiliary alkali liquor etching method for preparing the two-dimensional metal boride (MBene) material, and the prepared boride has excellent specific capacity in the lithium ion battery.
Optionally, 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 them.
Optionally, MBene is MoB, crB, ni 2 B. At least one of WB, tiB and FeB.
Alternatively, the molar ratio of the MAB phase material to the alkali in the alkali solution is 1.01-0.8, and the alkali is one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide, calcium hydroxide, barium hydroxide, tetramethylammonium hydroxide and ammonia water.
Optionally, the solvent in the alkali solution is at least one of water, ethanol and methanol.
Alternatively, the concentration mass ratio of the alkali solution is 15-30wt.%.
Optionally, the temperature of the heat preservation 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 applied to an ion battery, such as a lithium ion battery negative electrode.
Aiming at the defects in the prior etching technology, such as high danger of hydrofluoric acid which is a common etchant; the effect is not obvious by directly etching with alkali liquor; and boron is easily oxidized by introducing an etchant with oxidizability. The invention provides a method for preparing an MBene material by MBene green hydrothermal auxiliary alkali liquor etching.
In order to make the objects, technical solutions and effects of the present invention clearer and clearer, the present invention is described in further detail below. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Based on this, the embodiment of the invention provides a method for preparing an MBene material by green hydrothermal auxiliary alkali liquor etching, wherein the method comprises the following steps:
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, keeping the temperature for reacting 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 the lithium ion battery negative electrode material.
In the embodiment, MAB phase material is used as a precursor, alkali liquor is used as an etching agent, MAB is dispersed in the alkali liquor, the MAB is transferred to a hydrothermal kettle, and the etching effect of the alkali liquor is enhanced under the auxiliary action of hydrothermal treatment, so that the two-dimensional metal boride MBene material is finally obtained. The coating is used as a negative electrode material of a lithium ion battery, and the excellent battery capacity is shown.
In addition, the method for preparing the MBene material by the green hydrothermal auxiliary alkali liquor etching is a preparation method which is simple to operate and free of potential safety hazards, is suitable for large-scale industrial production, and has universality.
In step S1, in one embodiment, the MAB phase material includes MoAlB and 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 them.
In step S2, in an embodiment, the molar ratio of the MAB phase material to the etching base is 1.01 to 0.8, and the etching base is one or a mixture of two 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. At least one of WB, tiB and FeB.
In one embodiment, the reaction solvent is at least one of water, ethanol, methanol.
In one embodiment, the concentration mass ratio of the aqueous alkali solution is 15-30wt.%.
In step S3, in one embodiment, the hydrothermal reaction temperature is 110 to 150 ℃.
In one embodiment, the etch reaction soak time is between 2 and 24 hours.
In step S4, in an 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 an environment-friendly manner, wherein the MBene is used for a lithium ion battery negative electrode material.
To further illustrate the technical solution and effects of the present invention, the following will be further described with reference to specific examples and comparative examples.
Example 1
1. MBene (MoB) was prepared according to the following procedure:
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 is filtered, washed with 1 mol/l sodium hydroxide solution three times, and then washed with deionized water five times, and the obtained powder is dried at 80 ℃ for 10 hours to obtain the two-dimensional molybdenum boride MBene with an accordion-like structure, wherein a scanning electron microscope of the powder is shown in figure 1, and figure 2 is an XRD (X-ray diffraction) pattern of the two-dimensional molybdenum boride MBene in the embodiment.
2. Preparing the cathode of the MBene lithium ion battery according to the following steps:
uniformly mixing MBene powder prepared in the steps with acetylene black and sodium alginate, wherein the mass ratio of the MBene powder to the acetylene black to the sodium alginate is 80And (3) powder, magnetically stirring for 8h, coating the slurry on a copper foil on a coating machine, drying at 70 ℃ for 12h, and then drying at 80 ℃ in vacuum for 12h to prepare the battery cathode, wherein the battery cathode can be used for a lithium ion battery. A lithium ion CR2032 button cell is assembled in an inert atmosphere glove box, a metal lithium sheet is taken as a counter electrode, lithium hexafluorophosphate is taken as electrolyte, and a cell diaphragm is Celgard 2400. Performing charge and discharge test on a blue battery test system at 50mAg -1 Under the current density, the first charging specific capacity and the first discharging specific capacity of the battery are 645.7mAhg respectively -1 And 666.0mAhg -1 The capacity fade was not large for three cycles, as shown in fig. 3. In 2Ag -1 The capacity of the capacitor still remains 144.2mAhg after 1000 cycles of circulation under the current density -1 While the unetched boroaluminomolybdenum has almost no capacity, as shown in fig. 4.
Comparative example 1
1g of MoAlB powder and 35 ml of 25% by weight sodium hydroxide solution were mixed homogeneously and transferred into a 100 ml reaction vessel, which was placed in an oven and incubated at 160 ℃ for 24 hours. The prepared MoB particles are not in a two-dimensional layered structure, so the hydrothermal temperature cannot be too high.
Comparative example 2
1g of WAlB 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 kept at 120 ℃ for 24 hours. After cooling, the suspension is filtered, washed three times with 1 mol/l sodium hydroxide solution, then washed five times with deionized water, and the obtained powder is dried for 10 hours at 80 ℃ to obtain the two-dimensional tungsten boride MBene with the accordion-shaped structure. Under the same lithium ion battery assembling process, the lithium ion battery is assembled at 50mAg -1 The first charge specific capacity and the first discharge specific capacity of the battery are 595.6mAhg respectively under the current density -1 And 603.2mAhg -1 ,. In 2Ag -1 The specific capacity is 134.5mAhg after 1000 cycles of circulation under the current density -1 。
According to the embodiment, the method for preparing the two-dimensional metal boride (MBene) in an environment-friendly mode is characterized in that a ternary metal boride precursor (MAB) is dispersed in an alkali solution, a suspension is transferred into a hydrothermal kettle, the etching effect of the alkali solution is enhanced under the hydrothermal auxiliary enhancement effect, and after the reaction is finished, a dispersion liquid containing the MBene is filtered and washed to prepare the MBene material. The method adopts a hydrothermal auxiliary alkali liquor etching method for preparing the MBene material for the first time, 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 lithium ion batteries, shows excellent battery capacity and has wide application prospect.
From the two comparative examples, it can be seen that the process of the present invention is suitable for forming MAB phase materials into two-dimensional metal borides (MBene). Comparative example 1 the final product was granular, rather than forming a two-dimensional layered structure, due to the higher reaction temperature. The material of the MAB phase is not adopted in the comparative example 2, and the sub-charge specific capacity, the discharge specific capacity and the cycling effect of the prepared product in the lithium ion battery are far less ideal than those in the example 1.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A two-dimensional metal boride compound obtained by the following process:
and dispersing the MAB phase material in an alkali solution, transferring the suspension into a hydrothermal kettle, heating in an oven, carrying out heat preservation reaction for a proper time, cooling, filtering, washing and drying to obtain the target product, namely the two-dimensional metal boride.
2. The two-dimensional metal boride of claim 1 wherein said 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 them; the two-dimensional metal boride is MoB, crB and Ni 2 B. At least one of WB, tiB and FeB.
3. A method of preparing the two-dimensional metal boride of claim 1:
and dispersing the MAB phase material in an alkali solution, transferring the suspension into a hydrothermal kettle, heating in an oven, carrying out heat preservation reaction, cooling, filtering, washing and drying to obtain the target product, namely the two-dimensional metal boride.
4. The method of claim 3, wherein 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 them; the two-dimensional metal boride is MoB, crB and Ni 2 B. At least one of WB, tiB and FeB.
5. The method of claim 3, wherein the molar ratio of MAB phase material to base in the alkaline solution is 1.01-0.8, and the base is one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide, calcium hydroxide, barium hydroxide, tetramethylammonium hydroxide, and ammonia water.
6. A method according to claim 3, wherein the solvent of the alkali solution is at least one of water, ethanol, methanol.
7. A method according to claim 3, wherein the concentration mass ratio of the alkali solution is 1-30wt.%.
8. The method of claim 3, wherein the temperature of the incubation reaction is 100-200 ℃; the reaction time is kept between 0.1 and 30 hours.
9. The method according to claim 3, wherein the hydrothermal reaction equipment is an oven or microwave hydrothermal.
10. Use of a two-dimensional metal boride according to claim 1 in a lithium ion battery.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115532251A (en) * | 2022-10-09 | 2022-12-30 | 四川大学 | Layered transition metal boride material and preparation method and application thereof |
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| 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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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115532251A (en) * | 2022-10-09 | 2022-12-30 | 四川大学 | Layered transition metal boride material and preparation method and application thereof |
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