CN112974832A - Preparation method of Pt concave cubic nanocrystal, and nanocrystal and application thereof - Google Patents
Preparation method of Pt concave cubic nanocrystal, and nanocrystal and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
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- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 31
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 31
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 claims abstract description 25
- 235000003704 aspartic acid Nutrition 0.000 claims abstract description 22
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000013078 crystal Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 46
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 35
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 17
- 239000000725 suspension Substances 0.000 claims description 17
- -1 polytetrafluoroethylene Polymers 0.000 claims description 9
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- 239000002244 precipitate Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000001035 drying Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 7
- 238000006722 reduction reaction Methods 0.000 abstract description 7
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- 229910002621 H2PtCl6 Inorganic materials 0.000 abstract description 5
- 238000005580 one pot reaction Methods 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
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- 230000003197 catalytic effect Effects 0.000 description 10
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- 238000001228 spectrum Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
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- 229910003609 H2PtCl4 Inorganic materials 0.000 description 1
- CKLJMWTZIZZHCS-UWTATZPHSA-N L-Aspartic acid Natural products OC(=O)[C@H](N)CC(O)=O CKLJMWTZIZZHCS-UWTATZPHSA-N 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
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- 239000012670 alkaline solution Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of a Pt concave cubic nanocrystal, the nanocrystal and application thereof, and the Pt concave cubic nanocrystalThe preparation method comprises the following steps: adding polyvinylpyrrolidone (PVP) and aspartic acid into deionized water, and stirring for dissolving; addition of H2PtCl6·6H2Continuously stirring O, and adjusting the pH value of the solution; and carrying out high-temperature hydrothermal reaction on the solution, carrying out centrifugal washing on the solution after the reaction to obtain a sample, and drying to obtain the Pt concave nanocube. The Pt concave cubic nanocrystal is obtained by controlling and synthesizing by using a simple one-pot hydrothermal reduction method and using micromolecular aspartic acid as a morphology regulator and polyvinylpyrrolidone as a dispersing agent under a specific pH condition, has a smooth surface, a concave structure in the Pt concave cubic nanocrystal, a high-index crystal face, a high dispersity, a stable morphology and a uniform size, and shows excellent electrocatalytic activity and stability for an alkaline Oxygen Reduction Reaction (ORR).
Description
Technical Field
The invention belongs to a nano inorganic material, and particularly relates to a preparation method of a Pt concave cubic nanocrystal, the nanocrystal and application thereof.
Background
ORR is one of typical electrochemical reactions in energy conversion and storage devices such as fuel cells and metal-air batteries, and has been widely studied in recent years. Designing high performance electrocatalysts for ORR is of great importance for electrochemical energy conversion and storage devices such as fuel cells, metal-air batteries, and the like. Precious metal Pt is the most commonly used ORR catalyst at present, and based on the close correlation between the geometric shape and the ORR performance, people are dedicated to regulating and controlling the shape, the composition and the structure of the Pt-based nano material so as to reduce the high cost and improve the electrocatalytic activity and the stability of the Pt-based nano material.
A large number of researches show that due to the fact that the Pt nanocrystals have different crystal face indexes and different shapes, the number of catalytic active sites exposed on the surface of the Pt nanocrystals is different, and therefore the catalytic activity shows larger difference when the Pt nanocrystals catalyze the ORR reaction. Among them, HIF, a High index facets (High index facets) having a large number of atomic steps, edges and kinks, plays an important role in increasing catalytic activity and catalytic reaction selectivity. Compared with the crystal face with low index, the nano catalyst with the crystal face with high index is thermodynamically unstable, and the synthesis difficulty is higher. There are many Pt nanocrystals with high index prepared using electrochemical reduction and heat treatment methods. Although these Pt nanocrystals have been demonstrated to have high catalytic activity, their size is still relatively large and the preparation method is rather limited in throughput. Therefore, it remains a challenge to prepare Pt nanocrystals with high index crystal planes using a simple, scalable process based on wet chemical reduction.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides a preparation method of a Pt concave cubic nanocrystal, and the prepared nanomaterial is that the Pt concave cubic nanocrystal presents extremely excellent ORR catalytic activity and stability under an alkaline condition, so that a new material is provided for improving the application of the Pt nanomaterial in electro-catalysis ORR.
The invention also provides a Pt concave cubic nanocrystal and application.
The technical scheme is as follows: in order to achieve the above purpose, the preparation method of the Pt concave cubic nanocrystal comprises the following steps:
(1) adding polyvinylpyrrolidone (PVP) and aspartic acid into deionized water, and stirring for dissolving;
(2) adding H into the mixed solution2PtCl6·6H2Continuously stirring, and adjusting the pH value of the solution to 9-14;
(3) and carrying out high-temperature hydrothermal reaction on the solution, carrying out centrifugal washing on the solution after the reaction to obtain a sample, and drying to obtain the Pt concave nanocube.
Wherein the ratio of polyvinylpyrrolidone PVP to aspartic acid in the step (1) is 7: 1-13: 1
Preferably, the mass ratio of polyvinylpyrrolidone PVP to aspartic acid is 10: 1.
Wherein, in the step (2), H2PtCl6·6H2The mass ratio of O to aspartic acid is 0.4-0.6.
Preferably, H in step (2)2PtCl6·6H2The mass ratio of O to aspartic acid was 0.52.
Wherein, KOH or NaOH solution is used for adjusting the pH value of the solution to 10 in the step (2).
Preferably, the pH of the solution is adjusted to 10 using a 1M KOH solution.
Wherein the temperature of the high-temperature hydrothermal reaction in the step (3) is 180-220 ℃, and the time is 3.5-4.5 h.
Preferably, in the step (3), the high-temperature hydrothermal reaction is carried out by transferring the solution into an autoclave with a polytetrafluoroethylene lining, obtaining a dark brown suspension through the high-temperature hydrothermal reaction, centrifuging the suspension at a high speed, and washing the precipitate with a mixed solution of ethanol and acetone.
Preferably, the sample obtained in the step (3) is dried in a vacuum oven at 60-80 ℃ for 4-5h, and the Pt concave nanocubes can be obtained.
The Pt concave cubic nanocrystal prepared by the preparation method of the Pt concave cubic nanocrystal is provided by the invention.
The Pt nanocrystal is a Pt concave nanocube, a concave structure is arranged in the Pt nanocrystal, the Pt nanocrystal has a high-index crystal face, and the particle size is 16-21 nm.
Furthermore, the prepared Pt concave cubic nanocrystal has the characteristics of high crystal face index, uniform size and high dispersity.
The Pt concave cubic nanocrystal prepared by the preparation method of the Pt concave cubic nanocrystal disclosed by the invention is applied to the field of electrocatalysis. In particular, the catalyst can be used as a catalyst in the field of electrocatalysis.
The invention uses a simple one-pot hydrothermal reduction method with H2PtCl6·6H2O is a metal precursor, micromolecular aspartic acid (L-aspartic acid) is a morphology regulator, polyvinylpyrrolidone (PVP) is a dispersant, the Pt concave nano-cube is obtained by controlled synthesis under the condition that the pH value of the solution is 10, and the prepared Pt concave nano-cube has extremely excellent ORR catalytic activity and stability under the alkaline condition.
The Pt concave nanocrystallines with high-index crystal faces are synthesized by adopting a specific morphology regulator and a specific dispersant and regulating a specific pH (pH is 10) of a solution. The nano material obtained by the invention has a high-index crystal face, more active sites and larger specific surface area, and meanwhile, a large number of atomic steps, edges and kinks caused by the concave structure of the Pt concave nanocube increase the specific surface area of the nanocrystal and increase the number of active sites exposed on the surface.
The invention uses molecular aspartic acid (L-aspartic acid) and polyvinylpyrrolidone (PVP) as a morphology regulator and a dispersant respectively, wherein the morphology regulator can reduce the reduction rate of Pt ions, and the dispersant can disperse products, has uniform size and regular morphology. In addition, the pH value has great influence on the formation of the final shape in the preparation process, and the Pt concave nanocube structure can be obtained by adding a potassium hydroxide solution to adjust the pH value of the solution to be 10, so that the Pt concave nanocube structure has excellent electrocatalytic activity and stability on ORR, and only irregular Pt nanospheres or Pt nanocubes can be obtained when the pH value is improper.
Has the advantages that: compared with the prior art, the invention has the following advantages:
1. the Pt concave cubic nanocrystal is prepared by a one-pot hydrothermal reduction method, and the preparation method is simple, mild in condition and environment-friendly.
2. The invention skillfully uses micromolecular aspartic acid as a morphology regulator and PVP as a dispersant, thus having high experimental controllability on the aspects of the morphology and the dispersity of a final product. The Pt concave cubic nanocrystal prepared by the method has wide raw material source, and can realize large-scale production.
3. The Pt nano material prepared by the invention is a specific concave cube, has a smooth surface, a concave structure in the Pt nano material, a high-index crystal face, high crystallinity, high dispersity, stable appearance and uniform size, and shows excellent electrocatalytic activity and stability to ORR in an alkaline solution.
Drawings
FIG. 1 is a TEM spectrum of a Pt concave cubic nanocrystal prepared by the method of the present invention;
FIG. 2 is an XRD pattern of Pt concave cubic nanocrystals prepared by the method of the present invention;
FIG. 3 is a CV plot and an ORR polarization plot of Pt concave cubic nanocrystals prepared by the method of the present invention;
FIG. 4 is the result of accelerated durability test of Pt concave cubic nanocrystals prepared by the method of the present invention;
fig. 5 is a TEM spectrum of Pt nanocrystals at different pH conditions.
Detailed Description
The present invention is further illustrated by the following examples.
The experimental methods described in the examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Wherein the L-aspartic acid is obtained from the national pharmaceutical group chemical reagents, Inc. (Shanghai, China)
Polyvinylpyrrolidone PVP (PVP-K30, cat # 30154481) was purchased from national pharmaceutical group Chemicals Co., Ltd (Shanghai, China)
H2PtCl6·6H2O from national medicine group chemical reagent Co., Ltd (Shanghai, China)
Example 1
A preparation method of Pt concave cubic nanocrystals comprises the following steps:
400mg PVP and 40mg aspartic acid are weighed and added into 9.2mL deionized water, stirred for 2H under water bath at 30 ℃ to be fully dissolved, and 0.8mL of 0.05M H is added into the mixed solution2PtCl6·6H2And O, continuously stirring for 30 min. And (3) adjusting the pH value of the solution to 9 by using a 1M KOH solution, then transferring the solution into a 20mL stainless steel autoclave with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at the high temperature of 200 ℃ for 4 hours to obtain a dark brown suspension. Centrifuging the suspension at 20000rpm for 10min, washing the precipitate with ethanol and acetone mixed solution (volume ratio of 1: 1) for 5 times, and drying the obtained sample in a vacuum oven at 60 deg.C for 5h to obtain Pt concave nanocubes.
Example 2
A preparation method of Pt concave cubic nanocrystals comprises the following steps:
400mg PVP and 40mg aspartic acid are weighed and added into 9.2mL deionized water, stirred for 2H under water bath at 30 ℃ to be fully dissolved, and 0.8mL of 0.05M H is added into the mixed solution2PtCl6·6H2And O, continuously stirring for 30 min. Adjusting the pH value of the solution to 10 by using a 1M KOH solution, transferring the solution into a 20mL stainless steel autoclave with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at the high temperature of 200 ℃ for 4 hours to obtain a black brown suspensionAnd (4) liquid. Centrifuging the suspension at 20000rpm for 10min, washing the precipitate with ethanol and acetone mixed solution (volume ratio of 1: 1) for 5 times, and drying the obtained sample in a vacuum oven at 60 deg.C for 5h to obtain Pt concave nanocubes.
Example 3
A preparation method of Pt concave cubic nanocrystals comprises the following steps:
400mg PVP and 40mg aspartic acid are weighed and added into 9.2mL deionized water, stirred for 2H under water bath at 30 ℃ to be fully dissolved, and 0.8mL of 0.05M H is added into the mixed solution2PtCl6·6H2And O, continuously stirring for 30 min. And (3) adjusting the pH value of the solution to 11 by using a 1M KOH solution, then transferring the solution into a 20mL stainless steel autoclave with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at the high temperature of 200 ℃ for 4 hours to obtain a dark brown suspension. Centrifuging the suspension at 20000rpm for 10min, washing the precipitate with ethanol and acetone mixed solution (volume ratio of 1: 1) for 5 times, and drying the obtained sample in a vacuum oven at 60 deg.C for 5h to obtain Pt concave nanocubes.
Example 4
A preparation method of Pt concave cubic nanocrystals comprises the following steps:
400mg PVP and 40mg aspartic acid are weighed and added into 9.2mL deionized water, stirred for 2H under water bath at 30 ℃ to be fully dissolved, and 0.8mL of 0.05M H is added into the mixed solution2PtCl6·6H2And O, continuously stirring for 30 min. And (3) adjusting the pH value of the solution to 10 by using a 1M KOH solution, then transferring the solution to a 20mL stainless steel autoclave with a polytetrafluoroethylene lining, and carrying out a high-temperature hydrothermal reaction at 180 ℃ for 4 hours to obtain a dark brown suspension. Centrifuging the suspension at 20000rpm for 10min, washing the precipitate with ethanol and acetone mixed solution (volume ratio of 1: 1) for 5 times, and drying the obtained sample in a vacuum oven at 60 deg.C for 5h to obtain Pt concave nanocubes.
Example 5
A preparation method of Pt concave cubic nanocrystals comprises the following steps:
400mg of PVP and 40mg of aspartic acid are weighed into 9.2mL of deionized water and placed in a water bath at 30 DEG CStirring for 2 hr to dissolve completely, adding 0.8mL of 0.05M H2PtCl6·6H2And O, continuously stirring for 30 min. And (3) adjusting the pH value of the solution to 10 by using a 1M KOH solution, then transferring the solution to a 20mL stainless steel autoclave with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at the high temperature of 220 ℃ for 4 hours to obtain a dark brown suspension. Centrifuging the suspension at 20000rpm for 10min, washing the precipitate with ethanol and acetone mixed solution (volume ratio of 1: 1) for 5 times, and drying the obtained sample in a vacuum oven at 60 deg.C for 5h to obtain Pt concave nanocubes.
Example 6
A preparation method of Pt concave cubic nanocrystals comprises the following steps:
400mg PVP and 40mg aspartic acid are weighed and added into 9.2mL deionized water, stirred for 2H under water bath at 30 ℃ to be fully dissolved, and 0.8mL of 0.05M H is added into the mixed solution2PtCl6·6H2And O, continuously stirring for 30 min. And (3) adjusting the pH value of the solution to 10 by using a 1M KOH solution, then transferring the solution to a 20mL stainless steel autoclave with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at the high temperature of 200 ℃ for 3.5h to obtain a dark brown suspension. Centrifuging the suspension at 20000rpm for 10min, washing the precipitate with ethanol and acetone mixed solution (volume ratio of 1: 1) for 5 times, and drying the obtained sample in a vacuum oven at 60 deg.C for 5h to obtain Pt concave nanocubes.
Example 7
A preparation method of Pt concave cubic nanocrystals comprises the following steps:
400mg PVP and 40mg aspartic acid are weighed and added into 9.2mL deionized water, stirred for 2H under water bath at 30 ℃ to be fully dissolved, and 0.8mL of 0.05M H is added into the mixed solution2PtCl6·6H2And O, continuously stirring for 30 min. The pH value of the solution is adjusted to 10 by using a 1M KOH solution, then the solution is transferred to a stainless steel autoclave with a 20mL polytetrafluoroethylene lining, and the black brown suspension is obtained after hydrothermal reaction at the high temperature of 200 ℃ for 4.5 h. Centrifuging the suspension at 20000rpm for 10min, washing the precipitate with ethanol and acetone mixed solution (volume ratio of 1: 1) for 5 times, drying the obtained sample in a vacuum oven at 60 deg.C for 5 hrAnd obtaining the Pt concave nanocubes.
Example 8
Example 8 was prepared identically to example 2, except that: the mass ratio of polyvinylpyrrolidone PVP to aspartic acid in the step (1) is 7:1, and H in the step (2)2PtCl6·6H2The mass ratio of O to aspartic acid is 0.4; the temperature of the high-temperature hydrothermal reaction in the step (3) is 180 ℃, and the time is 4.5 h.
Example 9
Example 9 was prepared identically to example 2, except that: the mass ratio of polyvinylpyrrolidone PVP to aspartic acid in the step (1) is 13:1, and H in the step (2)2PtCl6·6H2The mass ratio of O to aspartic acid is 0.6; the temperature of the high-temperature hydrothermal reaction in the step (3) is 220 ℃, and the time is 3.5 h.
Test example 1
Physical characterization of the Pt concave cubic nanocrystals prepared in example 2 above was performed using TEM, XRD, CV curve, accelerated durability test, and the like.
From the TEM spectrum (fig. 1a) of the Pt concave nanocubes, it can be seen that the product is a Pt concave nanocube with high dispersion degree and stable morphology, and the particle size distribution statistics (inset in fig. 1a) can obtain that the particle size of the prepared Pt nanocrystals is about between 16nm and 21nm, and the size is uniform. The prepared Pt concave nanocubes were observed to have smooth surfaces by enlarged TEM images (fig. 1b), and it can be clearly observed that the Pt concave nanocubes have a distinct inner concave structure. The XRD pattern of the Pt concave cube is shown in figure 2, the diffraction peak of the Pt concave cube corresponds to the diffraction peak of standard face-centered cubic Pt, and the smaller half-peak width shows that the synthesized Pt nanocrystal has high crystallinity.
FIG. 3a is a CV curve of Pt nanocubes and a control sample in a 0.1M KOH solution saturated with nitrogen, calculated to give an ECSA of 21.3M for the Pt nanocubes2 g-1Much larger than commercial Pt black (Johnson Matthey) at 16.8m2 g-1FIG. 3b shows Pt concave nanocubes and control samples in 0.1MKOH solution saturated with oxygenThe ORR polarization curve of (1) shows that the half-wave potential of the Pt concave nanocubes is 0.895V (vs. RHE), which is more commercial Pt black (E)1/20.853V (vs. rhe)) shifted positive by 42mV, indicating that Pt concave nanocubes have outstanding ORR catalytic activity.
In the Accelerated Durability Test (ADT), the stability of the samples was evaluated by CV curves and ORR polarization curves of Pt concave nanocubes and commercial Pt black cycling through 2000 cycles, 5000 cycles, and within a potential range of 0.6-1.1V (vs. The results are shown in FIG. 4. Calculations found that the electrochemical active area of the Pt concave nanocubes after 2000 cycles was as low as 83% of the initial value and 67% after 5000 cycles (fig. 4a), indicate that there is a performance degradation problem of the Pt concave nanocubes during the catalytic ORR process, which may be caused by the reduced thermodynamic stability due to the high surface energy of the high index crystal planes. Comparing CV curves before and after accelerated durability testing of the commercial Pt black catalyst (fig. 4d), it can be found that ECSA after 2000 and 5000 rounds is 58% and 47% of the initial value, respectively, indicating that the prepared Pt concave nanocubes still have higher stability compared to the commercial Pt black. Further comparing the ORR catalytic performance before and after accelerated durability testing of the two catalysts (fig. 4b, e), after cycling for 2000 cycles and 5000 cycles, the area activity at 0.95V (vs. rhe) potential was almost not significantly decreased for the Pt hollow cube, while the area activity at 0.9V (vs. rhe) potential was decreased by 8% and 19%, respectively (fig. 4 c); for the commercial Pt black catalyst (fig. 4f), the activity of the area at 0.9V (vs. rhe) potential decreased by 21% and 39%, respectively. The comparative results further show that the Pt concave nanocubes have higher stability than the commercial Pt black.
Comparative example 1
Comparative example 1 the preparation method of example 2 was used except that: addition of H2PtCl4Thereafter, the solution pH was adjusted to 1 or 8.5 using hydrochloric acid solution or KOH solution.
FIG. 5 shows TEM images of the products obtained when the pH of the solution was adjusted to 1 and 8.5, respectively. From fig. 5a it can be observed that when the pH of the solution is adjusted to 1, the product is Pt nanospheres, the particle size distribution statistics (fig. 5a inset) shows that the particle size of the Pt nanospheres is between 10nm and 20nm, and from the magnified TEM image (fig. 5b) it can be clearly seen that the Pt nanospheres prepared are irregularly shaped spheres. When the solution pH was adjusted to 8.5, the resulting product was Pt nanocubes (fig. 5c), and the particle size distribution statistics showed that the particle size of the Pt nanocubes was between 10nm and 17 nm. An enlarged TEM image (fig. 5d) shows that the Pt nanocubes have regular surfaces. The post ORR catalytic performance of both structures is significantly inferior to that of the Pt concave nanocubes prepared in example 2 of the present invention.
Claims (10)
1. A preparation method of a Pt concave cubic nanocrystal is characterized by comprising the following steps:
(1) adding polyvinylpyrrolidone (PVP) and aspartic acid into deionized water, and stirring for dissolving;
(2) adding H into the mixed solution2PtCl6·6H2Continuously stirring, and adjusting the pH value of the solution to 9-14;
(3) carrying out high-temperature hydrothermal reaction on the solution, and centrifugally washing the solution after the reaction to obtain a sample; the sample was dried to obtain Pt concave nanocubes.
2. The preparation method according to claim 1, wherein the mass ratio of polyvinylpyrrolidone PVP to aspartic acid in step (1) is 7: 1-13: 1.
3. The method according to claim 1, wherein H is used in the step (2)2PtCl6·6H2The mass ratio of O to aspartic acid is 0.4-0.6.
4. The method according to claim 1, wherein the solution pH is adjusted to 10 in step (2) using KOH or NaOH solution.
5. The preparation method as claimed in claim 1, wherein the temperature of the high temperature hydrothermal reaction in step (3) is 180-220 ℃ and the time is 3.5-4.5 h.
6. The preparation method according to claim 1, wherein the high-temperature hydrothermal reaction in step (3) is to transfer the solution into an autoclave with a polytetrafluoroethylene lining, the high-temperature hydrothermal reaction is to obtain a dark brown suspension, the suspension is centrifuged at a high speed, and the precipitate is washed with a mixed solution of ethanol and acetone.
7. The preparation method according to claim 1, wherein the sample obtained in step (3) is dried in a vacuum oven at 60-80 ℃ for 4-5h to obtain the Pt concave nanocubes.
8. A Pt concave cubic nanocrystal prepared by the method for preparing a Pt concave cubic nanocrystal of claim 1.
9. The Pt concave nanocube according to claim 8, wherein the Pt nanocrystallines are Pt concave nanocubes with a concave structure inside, a high index crystal face, and a particle size of between 16nm and 21 nm.
10. The use of the Pt concave cubic nanocrystal prepared by the method of claim 1 in the field of electrocatalysis.
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