CN114950411A - Noble metal single-atom catalyst, preparation method thereof and application thereof in ascorbic acid detection - Google Patents
Noble metal single-atom catalyst, preparation method thereof and application thereof in ascorbic acid detection Download PDFInfo
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Abstract
The invention provides a noble metal single-atom catalyst which consists of a carbon carrier and noble metal elements, wherein noble metal atoms are dispersed on the surface of the carbon carrier in an atomic scale in the form of cation species. The noble metal monatomic catalyst provided by the invention has a monatomic active center, has an obvious improvement on the detection effect of ascorbic acid compared with commercial conductive carbon black, has the advantages of high sensitivity, low detection limit, good selectivity and the like, and can meet the requirements of direct or indirect quantitative monitoring in biosensing.
Description
Technical Field
The invention belongs to the technical field of electrochemical sensing, and particularly relates to a noble metal monatomic catalyst, a preparation method thereof and application thereof in ascorbic acid detection.
Background
Ascorbic acid is a compound essential for normal operation of the body, and can be ingested by diet, and when the content is insufficient, various diseases such as scurvy, osteoporosis, anorexia and the like can be caused, so that the detection of the content of the ascorbic acid in food, medicines and even human physiological environment is particularly important. At present, many effective means for detecting ascorbic acid have been reported, and commonly used methods include spectrophotometry, fluorescence, capillary electrophoresis, high performance liquid chromatography, amperometric detection, and the like, wherein electrochemical methods are widely used due to advantages of sensitive detection, simple equipment, strong portability, mild conditions, and the like.
Under the condition of not depending on biomolecules such as enzyme, the problems of narrow detection range, poor selectivity and the like still exist in the electrochemical sensing technology, and the targeted design and development of the high-efficiency catalyst is an important way for meeting the challenges. The monatomic catalyst has high activity, high selectivity and 100 percent of metal atom utilization rate, and shows great application potential in the aspect of improving the biosensing performance. Meanwhile, with the gradual and deep research of the monatomic catalyst, a universal synthesis method and a macro preparation process are reported, and support is provided for the development of the practical application of the monatomic catalyst.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a noble metal monatomic catalyst, a preparation method thereof, and an application thereof in detecting ascorbic acid, wherein the noble metal monatomic catalyst provided by the present invention can be used for electrode modification, and exhibits excellent electrochemical sensing performance against ascorbic acid.
The invention provides a noble metal single-atom catalyst which consists of a carbon carrier and noble metal elements, wherein noble metal atoms are dispersed on the surface of the carbon carrier in an atomic scale in the form of cation species.
Preferably, the carbon support is selected from conductive carbon blacks.
Preferably, the conductive carbon black is one selected from KJ600, BP2000, XC72, and N326.
Preferably, the noble metal element is one selected from Ru, Pd, Au and Pt.
Preferably, the mass ratio of the noble metal element to the conductive carbon black is (1-1.5): 100.
The invention also provides a preparation method of the noble metal monatomic catalyst, which comprises the following steps:
dissolving a noble metal compound in a low-boiling-point low-polarity solvent to obtain a noble metal solution;
while grinding the conductive carbon black, dropwise adding a noble metal solution into the conductive carbon black, and after full grinding, volatilizing the solvent to obtain solid powder;
and carrying out heat treatment on the solid powder to obtain the noble metal monatomic catalyst.
Preferably, the noble metal compound is selected from one of ruthenium acetylacetonate, palladium acetylacetonate, chloroauric acid and platinum acetylacetonate;
the low-boiling point and low-polarity solvent is selected from one of acetone, tetrahydrofuran and 2-butanone;
the concentration of the noble metal compound when dissolved in a low-boiling point low-polarity solvent is 8-16 mg/mL.
Preferably, the heat treatment is carried out under the inert atmosphere condition, the temperature of the heat treatment is 5-10 ℃ higher than the boiling point of the low-boiling-point low-polarity solvent, and the time of the heat treatment is 12-16 h.
The invention also provides an application of the noble metal monatomic catalyst in ascorbic acid detection.
Compared with the prior art, the noble metal monatomic catalyst provided by the invention is composed of a carbon carrier and noble metal elements, wherein the noble metal atoms are atomically dispersed on the surface of the carbon carrier in the form of cation species. The noble metal monatomic catalyst provided by the invention has a monatomic active center, has an obvious improvement on the detection effect of ascorbic acid compared with commercial conductive carbon black, has the advantages of high sensitivity, low detection limit, good selectivity and the like, and can meet the requirements of direct or indirect quantitative monitoring in biosensing.
Drawings
FIG. 1 is a scanning and transmission electron microscope image of Ru monatomic, Pd monatomic, Au monatomic, Pt monatomic catalysts prepared in examples 1-4 of the present invention;
FIG. 2 is an X-ray diffraction pattern of the Ru monatomic and Pd monatomic catalysts prepared in examples 1-2 of the present invention;
FIG. 3 is a spherical aberration corrected high angle annular dark field scanning transmission electron microscope image of the Ru monatomic catalyst of example 1 according to the present invention;
FIG. 4 shows X-ray near-edge absorption structure spectra and extended-edge X-ray absorption fine structure spectra of Ru monatomic and Pd monatomic catalysts prepared in examples 1-2 of the present invention;
FIG. 5 is a comparison graph of the performance of Ru monatomic and Pd monatomic catalysts prepared in examples 1-2 of the present invention and the ascorbic acid detection performance of the original commercial conductive carbon black;
FIG. 6 shows the selectivity of Ru monatomic and Pd monatomic catalysts prepared in examples 1-2 of the present invention against ascorbic acid and interfering substances.
Detailed Description
The invention provides a noble metal single-atom catalyst which consists of a carbon carrier and noble metal elements, wherein noble metal atoms are dispersed on the surface of the carbon carrier in an atomic scale in the form of cation species.
Wherein the carbon support is selected from conductive carbon blacks. The conductive carbon black is a commercial conductive carbon black. In some embodiments of the invention, the conductive carbon black is selected from one of KJ600, BP2000, XC72, and N326.
The noble metal element is selected from one of Ru, Pd, Au and Pt, preferably one of Ru and Pd.
The mass ratio of the noble metal element to the conductive carbon black is (1-1.5): 100, preferably 1:100, 1.1:100, 1.2:100, 1.3:100, 1.4:100, 1.5:100, or any value between (1-1.5): 100.
The invention also provides a preparation method of the noble metal monatomic catalyst, which comprises the following steps:
dissolving a noble metal compound in a low-boiling-point low-polarity solvent to obtain a noble metal solution;
while grinding the conductive carbon black, dropwise adding a noble metal solution into the conductive carbon black, and after full grinding, volatilizing the solvent to obtain solid powder;
and carrying out heat treatment on the solid powder to obtain the noble metal monatomic catalyst.
Specifically, the noble metal compound is dissolved in a low-boiling point low-polarity solvent to obtain a noble metal solution.
The noble metal compound is selected from one of ruthenium acetylacetonate, palladium acetylacetonate, chloroauric acid and platinum acetylacetonate, and is preferably ruthenium acetylacetonate or palladium acetylacetonate;
the low-boiling point and low-polarity solvent is selected from one of acetone, tetrahydrofuran and 2-butanone, and is preferably acetone;
the concentration of the noble metal compound when dissolved in a low-boiling point low-polarity solvent is 8-16 mg/mL, preferably 8, 10, 12, 14, 16, or any value between 8-16 mg/mL.
Then, while grinding the conductive carbon black, a small amount of noble metal solution is dripped into the conductive carbon black, and after full grinding, the solvent is basically volatilized to obtain solid powder. Wherein the mass ratio of the noble metal element in the noble metal compound to the conductive carbon black is (1-1.5): 100, preferably any value between 1:100, 1.1:100, 1.2:100, 1.3:100, 1.4:100, 1.5:100, or (1-1.5): 100.
And finally, carrying out heat treatment on the solid powder to obtain the noble metal monatomic catalyst. The heat treatment is carried out under the condition of inert atmosphere, the temperature of the heat treatment is 5-10 ℃ higher than the boiling point of the low-boiling-point low-polarity solvent, and the time of the heat treatment is 12-16 h, preferably 12, 13, 14, 15, 16 or any value between 12-16 h.
In the present invention, the inert atmosphere condition is preferably argon gas. In a specific embodiment, the solid powder is heat treated in a tube furnace to remove the solvent sufficiently that mild drying conditions are effective to prevent aggregation of the metal atoms.
The noble metal monatomic catalyst provided by the invention is obtained by impregnating and adsorbing a noble metal precursor with commercial conductive carbon black and drying the precursor, wherein the wettability of an impregnation solution on a carbon carrier is increased, and the effective anchoring of monatomic dispersed metal species is promoted by combining mild drying conditions. The method utilizes an impregnation method and the action of a low-boiling-point and low-polarity solvent to ensure that the noble metal atoms are atomically dispersed on the surface of the carbon carrier in the form of cationic species.
The invention also provides an application of the noble metal monatomic catalyst in ascorbic acid detection.
The application of the noble metal monatomic catalyst means that the catalyst has a catalytic effect on the oxidation of ascorbic acid under a certain potential after an electrode is modified, and a current signal generated by the catalyst is linearly related to the concentration of ascorbic acid molecules. Electrochemical biosensors based on this have the promise of meeting the need for analytical monitoring of ascorbic acid content in vitro and in vivo. In the specific embodiment of the application, compared with commercial conductive carbon black, the detection effect of the noble metal monatomic catalyst on ascorbic acid is obviously improved, and the noble metal monatomic catalyst has the advantages of high sensitivity, low detection limit, good selectivity and the like.
The preparation method of the noble metal monatomic catalyst provided by the invention is simple and feasible, has universality, has the potential of macroscopic synthesis and further application in the fields of electrode printing, electrochemical test paper production, microelectrode modification and the like, and provides support for developing more efficient and practical sensing devices and detection products.
For further understanding of the present invention, the noble metal monatomic catalyst provided by the present invention, the preparation method thereof and the application thereof in detecting ascorbic acid are described below with reference to the following examples, and the scope of the present invention is not limited by the following examples.
Example 1
Preparation of Ru monatomic catalyst:
(1) preparing 270 mu L of acetone solution of 16mg/mL ruthenium acetylacetonate, grinding while dropwise adding the acetone solution into 100mg of conductive carbon black, continuously grinding for 30min after the dropwise adding is finished, and obtaining solid powder after the solvent is basically volatilized;
(2) putting the obtained solid powder into a porcelain boat, then putting the porcelain boat into a tube furnace, sealing and introducing argon, heating to 65 ℃ under the argon atmosphere, keeping the temperature for 16h, naturally cooling to room temperature, and taking out the Ru monatomic catalyst, wherein the morphology of the material is shown in the attached drawing 1, in the drawing 1, a is a scanning and transmission electron microscope image of the Ru monatomic catalyst in the embodiment 1, b is a scanning and transmission electron microscope image of the Pd monatomic catalyst in the embodiment 2, c is a scanning and transmission electron microscope image of the Au monatomic catalyst in the embodiment 3, and d is a scanning and transmission electron microscope image of the Pt monatomic catalyst in the embodiment 4; as shown in fig. 2, a is an X-ray diffraction pattern of the Ru monoatomic catalyst and a standard pattern of the Ru metal, and b is an X-ray diffraction pattern of the Pd monoatomic catalyst and a standard pattern of the Pd metal, and it can be seen that no diffraction peak of Ru is shown in the X-ray diffraction pattern; as shown in the attached FIG. 3, in FIG. 3, the spherical aberration correction high angle annular dark field scanning transmission electron microscope image of Ru monatomic catalyst with a low power and b high power shows that Ru monatomic is uniformly distributed on the carbon carrier under the spherical aberration correction transmission electron microscope, and meanwhile, the Ru-Ru bond does not exist in the material, which further illustrates that the Ru-Ru bond is a monatomic dispersed catalyst, as shown in FIG. 4. In fig. 4, a and b are X-ray near-edge absorption structure spectrum and extended-edge X-ray absorption fine structure spectrum of Ru single-atom catalyst, respectively, and c and d are X-ray near-edge absorption structure spectrum and extended-edge X-ray absorption fine structure spectrum of Pd single-atom catalyst, respectively.
Example 2
Preparation of Pd monatomic catalyst:
(1) preparing 270 mu L of 16mg/mL acetylacetone palladium solution, adding the acetone solution into 100mg conductive carbon black while grinding, continuing to grind for 30min after finishing the adding, and obtaining solid powder after the solvent is basically volatilized;
(2) putting the obtained solid powder into a porcelain boat, then putting the porcelain boat into a tube furnace, sealing, introducing argon, heating to 65 ℃ under the argon atmosphere, keeping for 16h, naturally cooling to room temperature, taking out to obtain the Pd monatomic catalyst, wherein the shape of the material is shown in figure 1; as shown in FIG. 2, no diffraction peak of Pd is shown in the X-ray diffraction pattern; as shown in fig. 4, the absence of Pd — Pd bonds in the material further illustrates that it is a monoatomic dispersion catalyst.
Example 3
Preparation of Au monatomic catalyst:
(1) preparing 270 mu L of 8mg/mL chloroauric acid acetone solution, adding the solution into 100mg of conductive carbon black while grinding, continuing grinding for 30min after finishing the adding, and obtaining solid powder after the solvent is basically volatilized;
(2) and putting the obtained solid powder into a porcelain boat, then putting the porcelain boat into a tube furnace, sealing, introducing argon, heating to 65 ℃ under the argon atmosphere, keeping for 16h, naturally cooling to room temperature, and taking out to obtain the Au monatomic catalyst, wherein the shape of the material is shown in the attached figure 1.
Example 4
Preparation of Pt monatomic catalyst:
(1) preparing 270 mu L of 10mg/mL acetylacetone platinum acetone solution, adding the solution into 100mg conductive carbon black while grinding, continuing to grind for 30min after finishing the adding, and obtaining solid powder after the solvent is basically volatilized;
(2) and putting the obtained solid powder into a porcelain boat, putting the porcelain boat into a tube furnace, sealing, introducing argon, heating to 65 ℃ under the argon atmosphere, keeping for 16 hours, naturally cooling to room temperature, and taking out to obtain the Pt monatomic catalyst, wherein the material morphology is shown in figure 1.
Example 5
The Ru and Pd monatomic catalysts prepared in preparation examples 1-2 were subjected to ascorbic acid sensing performance test:
10 mul of catalyst dispersion consisting of 2mg of noble metal monatomic catalyst, 1mL of ethanol/water (v/v ═ 1:1), and 10 mul of Nafion D-521 dispersion was added dropwise to a clean glassy carbon electrode as a working electrode.
The test is carried out by utilizing a three-electrode system, wherein the reference electrode is an Ag/AgCl electrode, the counter electrode is a Pt wire, and the electrolyte is 1 multiplied by PBS buffer solution.
The three-electrode system was placed in a 1 XPBS buffer solution and ascorbic acid was added to the solution continuously such that the concentration of ascorbic acid in the solution was 1. mu.M, 3. mu.M, 10. mu.M, 30. mu.M, 0.1mM, 0.3mM, 1mM, 3mM, 10mM, 30mM in this order, giving continuous amperometric-time response curves as shown in FIG. 5 a. Corresponding current vs. ascorbic acid concentration curves were also obtained, as shown in fig. 5 b. As can be seen from FIG. 5c, the detection limit of ascorbic acid by the Pd monatomic catalyst was 1. mu.M, while that by the commercial conductive carbon black was 3. mu.M. From the results, the noble metal monatomic catalyst shows good detection effect, and has obvious advantages over commercial conductive carbon black in sensitivity and detection limit due to the high activity and high selectivity of the monatomic metal center. The three-electrode system was placed in 1 x PBS buffer solution and ascorbic acid, glucose, glycine, L-glutamic acid were added to the solution in order to evaluate the selectivity of Ru monoatomic, Pd monoatomic catalysts for ascorbic acid and interfering substances, as shown in fig. 6. Both the Ru monatomic and Pd monatomic catalysts have substantially no response to interfering substances, and exhibit excellent selectivity.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A noble metal monatomic catalyst characterized by consisting of a carbon support and a noble metal element, wherein the noble metal atom is atomically dispersed on the surface of the carbon support in the form of a cationic species.
2. The noble metal monatomic catalyst of claim 1 wherein said carbon support is selected from the group consisting of conductive carbon blacks.
3. The noble metal monatomic catalyst of claim 2 wherein said conductive carbon black is selected from one of KJ600, BP2000, XC72, and N326.
4. The noble metal monatomic catalyst of claim 1 wherein the noble metal element is selected from one of Ru, Pd, Au, and Pt.
5. The noble metal monatomic catalyst according to claim 1, wherein the mass ratio of the noble metal element to the conductive carbon black is (1 to 1.5): 100.
6. A method for preparing a noble metal monoatomic catalyst according to any one of claims 1 to 5, comprising the steps of:
dissolving a noble metal compound in a low-boiling-point low-polarity solvent to obtain a noble metal solution;
while grinding the conductive carbon black, dropwise adding a noble metal solution into the conductive carbon black, and after full grinding, volatilizing the solvent to obtain solid powder;
and carrying out heat treatment on the solid powder to obtain the noble metal monatomic catalyst.
7. The production method according to claim 6, wherein the noble metal compound is one selected from the group consisting of ruthenium acetylacetonate, palladium acetylacetonate, chloroauric acid, and platinum acetylacetonate;
the low-boiling point and low-polarity solvent is selected from one of acetone, tetrahydrofuran and 2-butanone;
the concentration of the noble metal compound when dissolved in a low-boiling point low-polarity solvent is 8-16 mg/mL.
8. The preparation method according to claim 6, wherein the heat treatment is carried out under an inert atmosphere, the temperature of the heat treatment is 5-10 ℃ higher than the boiling point of the low-boiling-point low-polarity solvent, and the time of the heat treatment is 12-16 h.
9. Use of the noble metal monatomic catalyst according to any one of claims 1 to 5 in ascorbic acid detection.
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