CN114045517A - Ternary layered transition metal boride and preparation method and application thereof - Google Patents
Ternary layered transition metal boride and preparation method and application thereof Download PDFInfo
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- CN114045517A CN114045517A CN202111281669.9A CN202111281669A CN114045517A CN 114045517 A CN114045517 A CN 114045517A CN 202111281669 A CN202111281669 A CN 202111281669A CN 114045517 A CN114045517 A CN 114045517A
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- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 15
- 150000003624 transition metals Chemical class 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000005530 etching Methods 0.000 claims abstract description 30
- 229910016459 AlB2 Inorganic materials 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 150000005622 tetraalkylammonium hydroxides Chemical class 0.000 claims abstract description 13
- 239000007864 aqueous solution Substances 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 17
- RILZRCJGXSFXNE-UHFFFAOYSA-N 2-[4-(trifluoromethoxy)phenyl]ethanol Chemical compound OCCC1=CC=C(OC(F)(F)F)C=C1 RILZRCJGXSFXNE-UHFFFAOYSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 32
- 239000000047 product Substances 0.000 description 29
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 12
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 4
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910004039 HBF4 Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- -1 transition metal sulfides Chemical class 0.000 description 2
- 238000004832 voltammetry Methods 0.000 description 2
- 238000001075 voltammogram Methods 0.000 description 2
- 229910015278 MoF3 Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 238000001212 derivatisation Methods 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- FASQHUUAEIASQS-UHFFFAOYSA-K molybdenum trifluoride Chemical compound F[Mo](F)F FASQHUUAEIASQS-UHFFFAOYSA-K 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 125000005207 tetraalkylammonium group Chemical group 0.000 description 1
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- 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
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
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Abstract
The invention discloses a ternary layered transition metal boride Mo2AlB2The preparation method is characterized in that MoAlB particles are placed in a fluoboric acid aqueous solution and are subjected to an etching reaction under normal pressure to obtain an etching product; then the etching product is put into aqueous solution of tetraalkylammonium hydroxide for post-treatment, and the transition metal boride Mo is obtained after washing2AlB2。
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a ternary layered transition metal boride and a preparation method and application thereof.
Background
With the continuous growth of the global population and the increase of fossil fuel consumption, the development of renewable energy sources such as solar energy and wind energy becomes more and more important. H2The carbon-free fuel is a carbon-free fuel which stores energy in the form of chemical bonds, has the advantages of environmental protection, sustainability, good economy and the like, and has wide development prospect.The key of the hydrogen evolution technology is to improve the electrocatalyst activity of the catalyst and improve the reaction conversion efficiency by minimizing the overpotential required by the Hydrogen Evolution Reaction (HER). The catalysts studied at present mainly comprise transition metal sulfides, selenides, phosphides, carbides, nitrides, borides and the like.
The hydrogen evolution catalytic activity of two-dimensional transition metal borides has attracted a great deal of attention from scholars. Kim et al (chem. commun.,2019,55,9295) proposed that the synthesis of two-dimensional transition metal borides (MBene) can be performed by etching of MAB phase such as MoAlB. However, Alameda et Al found that MBene could not be etched directly from MoAlB due to the MoAlB phase having a jagged double Al layer. So far, despite attempts to etch MoAlB phases with a number of sets of issues, no successful preparation of two-dimensional MoB materials has been reported. Zhang and Bai et al (Acta Materialia,2017,132:69) consider Mo based on theoretical calculations2AlB2Is a precursor that is likely to etch MBene phase. Most current etching methods inevitably involve etching MoAlB (JACS,2019,141:10852) with hydrofluoric acid or in situ generated hydrofluoric acid, removing one layer of the double Al atomic layer with saw-tooth shape, resulting in Mo2AlB2. Hydrofluoric acid has strong corrosivity in the etching process, and the use and the post-treatment of the hydrofluoric acid have greater safety risks.
The invention adopts fluoboric acid to etch MoAlB, combines with tetraalkylammonium hydroxide treatment to prepare Mo2AlB2The material avoids the use of hydrofluoric acid or in-situ hydrofluoric acid in a MILD method in the experimental process, and improves the experimental safety; and Mo etched by fluoroboric acid method2AlB2Has higher electrocatalytic activity.
Disclosure of Invention
In order to solve the problems, the invention provides a method for converting MoAlB into Mo based on fluoroboric acid etching and tetraalkylammonium hydroxide treatment2AlB2A method of making a material. The technical scheme is as follows:
preparation of ternary layered transition metal boride Mo2AlB2The method of (1), the method isPlacing MoAlB in a fluoboric acid aqueous solution, and carrying out an etching reaction under normal pressure to obtain an etching product; then the etching product is put into aqueous solution of tetraalkylammonium hydroxide for post-treatment, and the transition metal boride Mo can be obtained by washing2AlB2;
In one embodiment of the present invention, the mass fraction of the aqueous fluoroboric acid solution is 5 to 70 wt%.
In one embodiment of the present invention, the reaction temperature of the etching reaction is 60 to 110 ℃.
In one embodiment of the present invention, the reaction time of the etching reaction is 4 to 72 hours.
In one embodiment of the present invention, the concentration of tetraalkylammonium hydroxide in the aqueous solution of tetraalkylammonium hydroxide is from 5 to 80 wt%.
In one embodiment of the present invention, the tetraalkylammonium hydroxide is used in an amount of 0.5 times or more the mass of the MoAlB material.
In one embodiment of the present invention, the alkyl group of the tetraalkylammonium hydroxide is methyl, ethyl, propyl, butyl, or a combination thereof.
Transition metal boride Mo prepared by using method2AlB2Has good application in the field of electrocatalysis.
The invention has the beneficial effects that:
the invention prepares the ternary layered transition metal boride Mo with a single aluminum atomic layer by etching MoAlB with fluoboric acid and post-treating tetraalkylammonium hydroxide2AlB2(ii) a The obtained material was subjected to a hydrogen evolution test to a current density of 10mA cm-2The potential is lower; the material has good hydrogen evolution performance.
Drawings
FIG. 1 shows XRD spectra of the etching product of fluoroboric acid (80-H-MAB), TMAOH treated product (80-HT-MAB) and raw material MoAlB obtained in example 1.
FIG. 2 is a linear voltammogram (LSV curve) of the product 80-HT-MAB obtained in example 1.
FIG. 3 is the XRD spectra of the etching product of fluoroboric acid (90-H-MAB) and the TMAOH treated product (90-HT-MAB) obtained in example 2.
FIG. 4 is an XRD pattern of a sample 50-HT-MAB prepared by intercalating a fluoroboric acid etching product 50-H-MAB and TMAOH in comparative example 1.
FIG. 5 XRD pattern of product 35-M-MAB obtained in comparative example 2.
FIG. 6 is a linear voltammogram (LSV curve) of the product obtained in comparative example 2.
Detailed Description
The technical solution of the present invention will be described in detail by specific examples.
Example 1
1g of MoAlB powder was slowly added to a 40 wt% solution of the fluoroboric acid in a mass ratio of 60: 1. The mixture was then reacted at 80 ℃ for 48 h. And after the reaction is finished, completely cooling the product, centrifugally washing the precipitate by using deionized water until the pH value of the supernatant is more than 5, filtering, and drying the filter cake in a vacuum oven at 60 ℃ for 12 hours for later use, wherein the label is 80-H-MAB.
The product obtained above was added to a 25 wt% tetramethylammonium hydroxide solution (TMAOH) and reacted at 35 ℃ for 48 hours. Wherein the mass ratio of the tetramethylammonium hydroxide solution to the product is 20:1, magnetic stirring is used in the whole reaction process, and deionized water is used for centrifugal washing after the reaction is finished until the pH value is neutral. The product was dried in a vacuum oven at 60 ℃ for 12h and labeled 80-HT-MAB.
MoAlB and HBF4XRD spectra of intermediate etching product (80-H-MAB) obtained by reaction, TMAOH treated product (80-HT-MAB) and raw material MoAlB are shown in figure 1. The MoAlB raw material characteristic peak of the 80-H-MAB sample disappeared, and shifted from 2 θ of 12.61 ° to 13.61 ° based on the 020 diffraction peak corresponding to the intermediate layer, and the product contained AlF3(25.3 °) impurities, peaks at 13.6 °, 28.6 °, 38.6 °, 41.6 °, and 43.0 ° of 2 θ were assigned to Mo2AlB2The characteristic peak proves that one layer of the sawtooth-shaped double Al layer in the MoAlB is etched, and the MoAlB is successfully converted into Mo2AlB2. Derivatization of impurity fluorides of 80-HT-MAB samples after TMAOH treatmentThe peak was eliminated, demonstrating that the fluoride on the sample surface was successfully removed by treatment with TMAOH.
To investigate the HER electrocatalytic activity of the samples, 80-HT-MAB was tested using linear voltammetry (LSV) with a sample mass loading of 0.5mg cm-2. The test results are shown in FIG. 2, at a current density of 10mA cm-2The overpotential 241mV required by 80-HT-MAB indicates that it has good HER electrocatalytic activity.
Example 2
Same as example 1, but HBF4The aqueous solution treatment temperature was changed to 90 ℃ and the other steps were the same. And after the etching by the fluoboric acid, adding the obtained product into a tetramethylammonium hydroxide solution (TMAOH) with the concentration of 25 wt%, reacting for 48 hours at 35 ℃, magnetically stirring in the whole reaction process, and centrifugally washing with deionized water until the pH is neutral. The product was dried in a vacuum oven at 60 ℃ for 12 h.
As can be seen from an observation of fig. 3, the 020 diffraction peak of the fluoroboric acid etching product 90-H-MAB sample was shifted from 2 θ ═ 12.61 ° to 13.24 °, and the product initially contained MoF3(2 θ ═ 23.2 °) and AlF3(2 θ 25.3 °). After TMAOH treatment, the diffraction peak of impurity fluoride of the 90-HT-MAB sample disappears, and the XRD pattern accords with Mo2AlB2And (5) characterizing.
Comparative example 1
Same as example 1, but HBF4The aqueous solution treatment temperature was changed to 50 ℃ and the other steps were the same. And after the etching by the fluoboric acid, adding the obtained product into a tetramethylammonium hydroxide solution (TMAOH) with the concentration of 25 wt%, reacting for 48 hours at 35 ℃, magnetically stirring in the whole reaction process, and centrifugally washing with deionized water until the pH is neutral. The product was dried in a vacuum oven at 60 ℃ for 12 h.
As can be seen from FIG. 4, the 020 diffraction peaks of the sample 50-HT-MAB prepared by the fluoroboric acid etching product 50-H-MAB and TMAOH intercalation do not obviously shift, the intensity of the characteristic peak of the raw material is still strong, which indicates that Mo is not prepared2AlB2A material.
Comparative example 2
1.5gLiF is added to 30mL of 9mol L-1In the hydrochloric acid solution, after stirring for 10min by a magnetic stirring device, the MoAlB powder is slowly added into the mixed solution of the lithium fluoride and the hydrochloric acid, and then the reaction is carried out for 48h at 35 ℃. And after the reaction is finished, completely cooling the product, centrifugally washing the precipitate by using deionized water until the pH value of the supernatant is neutral, finally drying the product in a vacuum oven at 60 ℃ for 12 hours to obtain the product, and naming the product as 35-M-MAB, wherein M represents the reaction product and is prepared by etching by using a MILD method (HCl/LiF). The XRD pattern from the product (FIG. 5) corresponds to Mo2AlB2The characteristics of (1).
To study the HER electrocatalytic activity of the samples, they were tested using linear voltammetry (LSV) with a sample mass loading of 0.5mg cm-2. The test results are shown in FIG. 6 at a current density of 10mA cm-2The overpotential required for 35-M-MAB was 246mV higher than that for the sample 80-HT-MAB prepared in example 1. The overpotential (241mV) of 80-HT-MAB is 5mV lower than that of 35-M-MAB (246mV), which indicates that the sample prepared by the fluoboric acid etching method has higher HER electrocatalytic activity, and should be because the formed laminated structure is more obvious after the fluoboric acid etching and the TMAOH intercalation, and has larger contact area with the electrolyte.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. Ternary layered transition metal boride Mo2AlB2The preparation method is characterized in that MoAlB particles are placed in a fluoboric acid aqueous solution and subjected to etching reaction under normal pressure to obtain an etching product; then the etching product is put into aqueous solution of tetraalkylammonium hydroxide for post-treatment, and the ternary layered transition metal boride Mo is obtained after washing2AlB2。
2. The method according to claim 1, wherein the mass fraction of the aqueous fluoroboric acid solution is 5 to 70 wt%.
3. The method according to claim 1, wherein the reaction temperature of the etching reaction is 60-110 ℃.
4. The method of claim 1, wherein the etching reaction has a reaction time of 4 to 72 hours.
5. The method according to claim 1, wherein the aqueous solution of tetraalkylammonium hydroxide has a tetraalkylammonium hydroxide concentration of from 5 to 80 wt% based on the mass of the aqueous solution.
6. The method according to claim 1, wherein the tetraalkylammonium hydroxide is used in an amount of 0.5 times or more the mass of the MoAlB material.
7. The process of claim 1, wherein the alkyl group of the tetraalkylammonium hydroxide is methyl, ethyl, propyl, butyl, or a combination thereof.
8. The transition metal boride Mo of claim 12AlB2Application in the field of electrocatalysis.
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CN115140743A (en) * | 2022-05-29 | 2022-10-04 | 深圳信息职业技术学院 | Two-dimensional metal boride and hydrothermal auxiliary alkali liquor etching preparation method and application |
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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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114590817A (en) * | 2022-04-12 | 2022-06-07 | 郑州航空工业管理学院 | Two-dimensional layered boride material, preparation method thereof and application of two-dimensional layered boride material as electromagnetic wave absorption material |
CN115140743A (en) * | 2022-05-29 | 2022-10-04 | 深圳信息职业技术学院 | Two-dimensional metal boride and hydrothermal auxiliary alkali liquor etching preparation method and application |
CN115140743B (en) * | 2022-05-29 | 2023-09-19 | 深圳信息职业技术学院 | Two-dimensional metal boride and hydrothermal auxiliary alkali liquor etching preparation method and application |
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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