CN114045517B - Ternary lamellar transition metal boride and preparation method and application thereof - Google Patents
Ternary lamellar transition metal boride and preparation method and application thereof Download PDFInfo
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- CN114045517B CN114045517B CN202111281669.9A CN202111281669A CN114045517B CN 114045517 B CN114045517 B CN 114045517B CN 202111281669 A CN202111281669 A CN 202111281669A CN 114045517 B CN114045517 B CN 114045517B
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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 description 7
- 238000005530 etching Methods 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 14
- 150000005622 tetraalkylammonium hydroxides Chemical class 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract 2
- 239000000463 material Substances 0.000 claims description 10
- 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
- 239000000047 product Substances 0.000 description 28
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 26
- RILZRCJGXSFXNE-UHFFFAOYSA-N 2-[4-(trifluoromethoxy)phenyl]ethanol Chemical compound OCCC1=CC=C(OC(F)(F)F)C=C1 RILZRCJGXSFXNE-UHFFFAOYSA-N 0.000 description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 12
- 239000000243 solution Substances 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910016569 AlF 3 Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000002244 precipitate 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
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 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
- 238000001035 drying Methods 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000011065 in-situ storage 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
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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Abstract
The invention discloses a ternary layered transition metal boride Mo 2 AlB 2 Is prepared fromThe method is characterized in that MoAlB particles are placed in a fluoboric acid aqueous solution to carry out 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 after washing, transition metal boride Mo is obtained 2 AlB 2 。
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a ternary layered transition metal boride, a preparation method and application thereof.
Background
With the continued growth of the global population and the increase in fossil fuel consumption, the development of renewable energy sources such as solar and wind energy has become increasingly important. H 2 The carbon-free fuel which stores energy in a chemical bond mode has the advantages of environmental protection, sustainability, good economy and the like, and has wide development prospect. Electrocatalytic hydrogen evolution is an important approach to making pure hydrogen fuels, and the key to hydrogen evolution technology is to increase the electrocatalyst activity of the catalyst, improving the reaction conversion efficiency by minimizing the overpotential required for the Hydrogen Evolution Reaction (HER). Catalysts currently studied are mainly transition metal sulfides, selenides, phosphides, carbides, nitrides, borides, and the like.
The hydrogen evolution catalytic activity of two-dimensional transition metal borides has attracted extensive attention by scholars. Kim et al (chem. Commun.,2019,55,9295) propose that the synthesis of two-dimensional transition metal borides (mbens) can be performed by etching of the MAB phase of moolb et al. However, alameda et Al have found that MBene cannot be etched directly from MoAlB due to the jagged double Al layer in the MoAlB phase. Although there have been attempts to etch the MoAlB phase to date, there have been no reports of successful preparation of two-dimensional MoB materials. Zhang and Bai et al (Acta materials, 2017, 132:69) consider Mo based on theoretical calculations 2 AlB 2 Is a precursor that is likely to etch the MBene phase. Most current etching methods inevitably involve the use of hydrofluoric acid or in situEtching MoAlB (JACS, 2019, 141:10852) with hydrofluoric acid, and removing one layer of the serrated double Al atomic layer to obtain Mo 2 AlB 2 . Hydrofluoric acid has strong corrosiveness in the etching process, and the use and the post-treatment of the hydrofluoric acid have large safety risks.
The invention adopts fluoboric acid to etch MoAlB and combines with tetraalkylammonium hydroxide treatment to prepare Mo 2 AlB 2 The material avoids the use of hydrofluoric acid or in-situ hydrofluoric acid in the MILD method in the experimental process, and improves the experimental safety; and Mo etched by fluoboric acid method 2 AlB 2 Has higher electrocatalytic activity.
Disclosure of Invention
In order to solve the problems, the invention provides a method for converting MoAlB into Mo based on the combination of fluoroboric acid etching and tetraalkylammonium hydroxide treatment 2 AlB 2 A method of material. The technical scheme is specifically as follows:
preparation of ternary layered transition metal boride Mo 2 AlB 2 Placing MoAlB in a fluoboric acid aqueous solution, and performing etching reaction at normal pressure to obtain an etching product; then the etching product is put into aqueous solution of tetraalkylammonium hydroxide for post-treatment, and transition metal boride Mo can be obtained after washing 2 AlB 2 ；
In one embodiment of the invention, the mass fraction of the aqueous fluoroboric acid solution is 5-70wt%.
In one embodiment of the present invention, the reaction temperature of the etching reaction is 60-110 ℃.
In one embodiment of the invention, the reaction time of the etching reaction is 4-72h.
In one embodiment of the present invention, the mass concentration of the tetraalkylammonium hydroxide in the aqueous solution of tetraalkylammonium hydroxide is 5 to 80wt%.
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 invention, the alkyl group of the tetraalkylammonium hydroxide is methyl, ethyl, propyl, butyl, or a combination thereof.
Transition metal boride Mo prepared by using method 2 AlB 2 Has better application in the field of electrocatalytic.
The invention has the beneficial effects that:
the invention prepares the ternary layered transition metal boride Mo with a single aluminum atomic layer through the etching of the fluoroboric acid to the MoAlB and the post-treatment of the tetraalkylammonium hydroxide 2 AlB 2 The method comprises the steps of carrying out a first treatment on the surface of the The obtained material is subjected to hydrogen evolution test to reach a current density of 10mA cm -2 Having a lower overpotential; the material has good hydrogen evolution performance.
Drawings
FIG. 1 shows XRD patterns of the fluoroboric acid etching product (80-H-MAB), TMAH treated product (80-HT-MAB) and starting material MoAlB obtained in example 1.
FIG. 2 is a linear voltammogram (LSV) of the product 80-HT-MAB obtained in example 1.
FIG. 3 is an XRD spectrum of the fluoroboric acid etching product (90-H-MAB) and TMAH treated product (90-HT-MAB) obtained in example 2.
FIG. 4 is an XRD pattern of sample 50-HT-MAB obtained after intercalation of fluoroboric acid etch product 50-H-MAB and TMAH in comparative example 1.
FIG. 5 XRD pattern of 35-M-MAB of the product obtained in comparative example 2.
FIG. 6 is a linear voltammogram (LSV) of the product obtained in comparative example 2.
Detailed Description
The technical scheme of the invention is described in detail through specific examples.
Example 1
1g of MoAlB powder was slowly added to a 40wt% strength fluoroboric acid solution, wherein the mass ratio of fluoroboric acid solution to MoAlB powder was 60:1. The mixture was then reacted at 80℃for 48h. After the reaction is finished, the product is thoroughly cooled, the precipitate is centrifugally washed by deionized water until the pH value of the supernatant is more than 5, the supernatant is filtered, and a filter cake is placed in a vacuum oven at 60 ℃ for drying for 12 hours for later use, and is marked as 80-H-MAB.
The product obtained above was added to a tetramethylammonium hydroxide solution (TMAH) having a concentration of 25% by weight 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 adopted in the whole reaction process, and deionized water is used for centrifugal washing until the pH value is neutral after the reaction is finished. The product was dried in a vacuum oven at 60℃for 12h, labeled 80-HT-MAB.
MoAlB and HBF 4 XRD spectra of the intermediate etching product (80-H-MAB), TMAH treated product (80-HT-MAB) and raw material MoAlB obtained by the reaction are shown in figure 1. The characteristic peak of the MoAlB raw material of the 80-H-MAB sample disappeared, shifted from 2θ=12.61° to 13.61 ° based on the 020 diffraction peak corresponding to the intermediate layer, and the product contained AlF 3 (2θ=25.3°) impurity, the peak at 2θ is 13.6 °,28.6 °,38.6 °,41.6 °,43.0 ° is attributed to Mo 2 AlB 2 The characteristic peaks of (2) prove that the zigzag double Al layers in MoAlB are etched to form one layer, and the MoAlB is successfully converted into Mo 2 AlB 2 . The diffraction peak of the impurity fluoride of the 80-HT-MAB sample after TMAH treatment disappeared, demonstrating that the fluoride on the sample surface was successfully removed by TMAH treatment.
To study 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, when the current density is 10mA cm -2 The over potential required for 80-HT-MAB was 241mV, indicating good HER electrocatalytic activity.
Example 2
As in example 1, but HBF 4 The aqueous solution treatment temperature was changed to 90℃and the other steps were the same. After the fluoboric acid etching, the obtained product is added into a tetramethyl ammonium hydroxide solution (TMAHH) with the concentration of 25 weight percent, the reaction is carried out for 48 hours at the temperature of 35 ℃, the magnetic stirring is adopted in the whole reaction process, and deionized water is used for centrifugal washing until the pH value is neutral after the reaction is finished. The product was dried in a vacuum oven at 60℃for 12h.
As can be seen from a review of fig. 3, the 020 diffraction peak of the 90-H-MAB sample of the fluoroboric acid etch product shifted from 2θ=12.61° to 13.24 °, product onInitially contains MoF 3 (2θ=23.2°) and AlF 3 Impurities of (2θ=25.3°). After TMAH treatment, diffraction peak of impurity fluoride of 90-HT-MAB sample is disappeared, XRD pattern is consistent with Mo 2 AlB 2 Features.
Comparative example 1
As in example 1, but HBF 4 The aqueous solution treatment temperature was changed to 50℃and the other steps were the same. After the fluoboric acid etching, the obtained product is added into a tetramethyl ammonium hydroxide solution (TMAHH) with the concentration of 25 weight percent, the reaction is carried out for 48 hours at the temperature of 35 ℃, the magnetic stirring is adopted in the whole reaction process, and deionized water is used for centrifugal washing until the pH value is neutral after the reaction is finished. The product was dried in a vacuum oven at 60℃for 12h.
As can be seen from FIG. 4, the 020 diffraction peaks of the sample 50-HT-MAB prepared by intercalation of the fluoroboric acid etching product 50-H-MAB and TMAH have no obvious deviation, and the characteristic peak intensity of the raw material is still strong, which indicates that Mo is not prepared 2 AlB 2 A material.
Comparative example 2
1.5g LiF was added to 30mL 9mol L -1 In the hydrochloric acid solution, after stirring for 10min by a magnetic stirring device, the MoAlB powder was slowly added to the mixed solution of lithium fluoride and hydrochloric acid, and then reacted at 35℃for 48 hours. After the reaction is finished, the product is thoroughly cooled, the precipitate is centrifugally washed by deionized water until the pH of the supernatant is neutral, finally, the supernatant is dried in a vacuum oven at 60 ℃ for 12 hours to obtain the product, and the product is named as 35-M-MAB, wherein M represents the reaction product and is prepared by etching by a MILD method (HCl/LiF). The XRD pattern (FIG. 5) from the product conforms to Mo 2 AlB 2 Is characterized by (3).
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, when the current density is 10mA cm -2 The overpotential required for 35-M-MAB was 246mV, which is higher than that of the sample 80-HT-MAB prepared in example 1. The 80-HT-MAB overpotential (241 mV) was 5mV lower than that of 35-M-MAB (246 mV), indicating that the sample prepared by the fluoroboric acid etching method had higher HER electrocatalytic activity, which was due to the etching by fluoroboric acid and TMAHO intercalationThe layered structure formed is then more pronounced, with a greater contact area with the electrolyte.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (4)
1. Ternary layered transition metal boride Mo 2 AlB 2 The preparation method is characterized in that MoAlB particles are placed in 5-70wt% fluoboric acid aqueous solution by mass percent, and etching reaction is carried out at normal pressure, wherein the reaction temperature of the etching reaction is 60-110 ℃ and the reaction time is 4-72h, so that an etching product is obtained; then placing the etching product in an aqueous solution of tetraalkylammonium hydroxide with the mass concentration of 5-80 and wt percent for post-treatment, and washing to obtain the ternary lamellar transition metal boride Mo 2 AlB 2 。
2. The method according to claim 1, wherein the amount of tetraalkylammonium hydroxide is more than 0.5 times the mass of the MoAlB material.
3. The method of claim 1, wherein the alkyl group of the tetraalkylammonium hydroxide is methyl, ethyl, propyl, butyl, or a combination thereof.
4. A transition metal boride Mo prepared by the preparation method of claim 1 2 AlB 2 Application in the field of HER electrocatalysis.
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