CN111118524A - A kind of preparation method of two-dimensional amorphous Pt nanosieve - Google Patents
A kind of preparation method of two-dimensional amorphous Pt nanosieve Download PDFInfo
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- CN111118524A CN111118524A CN202010093273.0A CN202010093273A CN111118524A CN 111118524 A CN111118524 A CN 111118524A CN 202010093273 A CN202010093273 A CN 202010093273A CN 111118524 A CN111118524 A CN 111118524A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 239000012265 solid product Substances 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- VEJOYRPGKZZTJW-FDGPNNRMSA-N (z)-4-hydroxypent-3-en-2-one;platinum Chemical compound [Pt].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O VEJOYRPGKZZTJW-FDGPNNRMSA-N 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 2
- 239000012498 ultrapure water Substances 0.000 claims description 2
- FJDJVBXSSLDNJB-LNTINUHCSA-N cobalt;(z)-4-hydroxypent-3-en-2-one Chemical compound [Co].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FJDJVBXSSLDNJB-LNTINUHCSA-N 0.000 claims 2
- 239000002086 nanomaterial Substances 0.000 abstract description 19
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 abstract description 9
- 238000011160 research Methods 0.000 abstract description 4
- 239000010411 electrocatalyst Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000005518 electrochemistry Effects 0.000 abstract description 2
- 239000000446 fuel Substances 0.000 abstract description 2
- 239000010970 precious metal Substances 0.000 abstract 2
- 229910000510 noble metal Inorganic materials 0.000 description 12
- 235000019441 ethanol Nutrition 0.000 description 11
- 230000000694 effects Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 230000007547 defect Effects 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000002178 crystalline material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000005300 metallic glass Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
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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
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
- C25B11/081—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the element being a noble metal
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
- H01M4/905—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC
- H01M4/9058—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC of noble metals or noble-metal based alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
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Abstract
本发明涉及二维贵金属纳米材料技术领域，公开了一种二维非晶Pt纳米筛的制备方法；具体是将摩尔比为1:0.01‑1:1‑100的Pt(acac)2、Co(acac)3与NaBr加入到乙醇溶液中形成溶液，搅拌均匀后烘干，然后将烘干所得产物研磨后经过热处理后，置于浓硝酸中腐蚀得到a‑Pt NMs，可用于燃料电池与电化学分解水过程中的高效电催化剂；本发明超薄的多孔纳米结构具有大比表面积，同时还具有优异的电荷传输能力和大量的活性位点，从而使得制备的二维非晶Pt纳米筛具有极佳的电催化应用前景；本发明方法产量高，易操作，有利于对二维非晶贵金属纳米材料进一步科学研究和推广应用。
The invention relates to the technical field of two-dimensional precious metal nanomaterials, and discloses a preparation method of a two -dimensional amorphous Pt nanosieve; acac) 3 and NaBr are added to the ethanol solution to form a solution, dried after stirring, and then the product obtained by drying is ground and subjected to heat treatment, and then placed in concentrated nitric acid to corrode to obtain a-Pt NMs, which can be used for fuel cells and electrochemistry. High-efficiency electrocatalyst in the process of water splitting; the ultrathin porous nanostructure of the present invention has a large specific surface area, and also has excellent charge transport ability and a large number of active sites, so that the prepared two-dimensional amorphous Pt nanosieve has extremely high performance. Good electrocatalytic application prospect; the method of the invention has high yield and easy operation, which is beneficial to further scientific research and popularization and application of two-dimensional amorphous precious metal nanomaterials.
Description
Technical Field
The invention belongs to the technical field of preparation of two-dimensional metal materials, and particularly relates to a preparation method of a two-dimensional amorphous Pt nano-sieve.
Background
In recent years, two-dimensional nanomaterials have attracted extensive attention of researchers because they exhibit many unique physicochemical properties due to their quantum effects, small-size effects, surface effects, and macroscopic quantum tunneling effects. The noble metal nano material has potential application value in the fields of catalysis, electrochemistry, new energy, medicine, optics and the like due to the surface plasma effect, the quantum effect and the biocompatibility of the noble metal nano material. However, the scarcity of noble metals and their expensive price greatly hinders their widespread use. The performance of the noble metal nano material is closely related to the shape, the size and the shape of the noble metal nano material, so that the size and the shape of the noble metal nano material can be controlled to synthesize the noble metal nano material and the performance research of the noble metal nano material is a research hotspot in the field of the nano material at present. For non-layered materials represented by metals, the non-directionality of metal bonds causes metal atoms to be closely packed in three dimensions in space, and the intrinsic driving force of two-dimensional anisotropic growth is lacked. Thus, efficient, controllable preparation of two-dimensional metal nanomaterials is currently still a challenging topic.
The two-dimensional amorphous metal nanosheets have unique properties due to asymmetry of long-range rotation and translation and disorder of atomic arrangement. For example, the surface of the two-dimensional amorphous material has a large number of randomly oriented bonds, so that the two-dimensional amorphous material has abundant defects and coordination unsaturated sites, and has better catalytic performance than a crystalline material. In addition, the method for manufacturing the nanometer-sized holes in the two-dimensional metal material can effectively improve the specific surface area and the number of active sites of the material, so that the material has a good mass transfer effect, and the excellent electrocatalysis performance is shown. However, the noble metal nanomaterials synthesized by the conventional methods are generally crystalline due to the strong isotropy of the metal bonds. Therefore, the synthesis of two-dimensional amorphous noble metal nanomaterials with precisely controllable elemental composition, material size and morphology remains a significant challenge.
Disclosure of Invention
The invention overcomes the defects of the prior art, successfully prepares the two-dimensional amorphous Pt nano-sieve, overcomes the defects of the element composition, the size and the shape of the noble metal nano-material synthesized by the traditional method, and aims to improve the performance of the electrocatalyst of the two-dimensional amorphous metal nano-plate.
The invention is realized by the following technical scheme.
A preparation method of a two-dimensional amorphous Pt nano-sieve specifically comprises the following steps:
a) mixing Pt (acac)2、Co(acac)3Adding NaBr and the mixture into an ethanol solution, and stirring the mixture at room temperature until the mixture is fully mixed and dissolved;
b) drying the mixed solution to obtain a light yellow solid product;
c) grinding the light yellow solid product into powder, and carrying out heating annealing in a tube furnace;
d) cleaning and drying the heat-treated product to obtain a product expressed as Pt/Co NSs;
e) and (3) putting the Pt/Co NSs into concentrated nitric acid for soaking and corroding, and then cleaning and drying to obtain the a-Pt NMs.
Preferably, the volume ratio of the absolute ethyl alcohol to the ultrapure water in the ethanol solution used in the step a is 6: 1.
Preferably, Pt (acac)2、Co(acac)3The molar weight x/y/z ratio of the NaBr to the NaBr is 1:0.01-1: 1-100.
Preferably, the stirring and mixing time of the step a is 8-12 h.
Preferably, the step b is to dry the mixed solution in an oven, wherein the oven temperature is 40-80 ℃.
Preferably, the grinding time in the step c is 0.5 to 1 hour.
Preferably, the heating annealing in the step c is carried out at the temperature of 150 ℃ and 300 ℃ for 1-3 h in an air atmosphere, and the temperature rise rate is 5 ℃/h.
Preferably, the water used for washing in steps d and e is deionized water, and the drying manner is freeze drying.
Preferably, the soaking corrosion time in the step e is 0.5 to 12 hours.
Compared with the prior art, the invention has the following beneficial effects:
the a-Pt NMs synthesized by the method can be used for fuel cells and high-efficiency electrocatalysts in the electrochemical water decomposition process. Compared with the prior art, the amorphous structure in the ultrathin two-dimensional amorphous porous nano structure enables the material to have rich defects and coordinated unsaturated positions, so that the local electronic environment can be adjusted, and the catalytic performance superior to that of a crystalline material is provided. On the other hand, the unique porous structure of the two-dimensional nanosieve allows the material to have a large specific surface area, which can provide more "space" for charge transport and mass transfer, while having many defect atoms (i.e., edge sites) around the pores with high reactivity, which can improve electrocatalytic activity. In conclusion, the advantages of the two are combined, so that the prepared two-dimensional amorphous Pt nano-sieve has excellent electrocatalysis application prospect. The method has high yield and easy operation, and is favorable for further scientific research, popularization and application of the two-dimensional amorphous noble metal nano material.
Drawings
FIG. 1 is a scanning electron microscope image of the Pt/Co NSs prepared in example 1.
FIG. 2 is a transmission electron microscope image of the Pt/Co NSs prepared in example 1.
FIG. 3 is a selected area diffraction pattern of the Pt/Co NSs prepared in example 1.
FIG. 4 is a transmission electron microscope image of a-Pt NMs prepared in example 1.
FIG. 5 is a selected area diffraction pattern of a-Pt NMs prepared in example 1.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solution of the present invention is described in detail below with reference to the embodiments and the drawings, but the scope of protection is not limited thereto.
Example 1
A two-dimensional amorphous Pt nano-sieve: the preparation method of the a-Pt NMs comprises the following steps:
first 8 mg Pt (acac)2、0.5mg Co(acac)3The resulting solution was stirred with 10 mg NaBr in 7 mL of ethanol at room temperature for 12 hours. In the ethanol solution, the volume ratio of ethanol to deionized water is 6: 1.
Then, the above solution was transferred to an oven to be dried at 60 ℃ to obtain a pale yellow solid product. And grinding the dried product into powder, heating to 230 ℃ in a tube furnace at the speed of 5 ℃/min, preserving heat for 1.5 h, and naturally cooling to room temperature. Wherein the gas atmosphere is air. The product Pt/Co NSs is obtained. And (3) immersing Pt/Co NSs into concentrated nitric acid to corrode for 3 h, washing a sample by using deionized water, and freeze-drying to obtain a product a-Pt NMs.
FIG. 1 is a scanning electron microscope image of the Pt/Co NSs prepared in example 1, from which it can be seen that the sample prepared in example 1 is nanosheet in morphology.
FIG. 2 is a TEM image of the Pt/Co NSs prepared in example 1, and it can be seen that the sample morphology obtained in example 1 is nanosheet, consistent with the scanning results.
FIG. 3 is a selected area diffraction pattern of the Pt/Co NSs prepared in example 1, from which it can be seen that the resulting Pt/Co NSs are polycrystalline structures.
FIG. 4 is a TEM image of a-Pt NMs prepared in example 1, and it can be seen that the prepared sample has a porous structure.
FIG. 5 is a diffraction pattern of selected areas of a-Pt NMs prepared in example 1, from which it can be seen that the resulting sample is amorphous.
As can be clearly seen from the above graph, the ultrathin two-dimensional amorphous porous nanostructure of the present embodiment not only has a large specific surface area, but also has excellent charge transport capacity and a large number of active sites, so that the prepared two-dimensional amorphous Pt nanosieve has excellent electrocatalytic performance.
Example 2
The preparation of the a-Pt NMs comprises the following steps:
first 8 mg Pt (acac)2、4 mg Co(acac)3The resulting solution was stirred with 15 mg of NaBr in 14 mL of ethanol at room temperature for 12 hours. In the ethanol solution, the volume ratio of ethanol to deionized water is 6: 1.
Then, the above solution was transferred to an oven to be dried at 60 ℃ to obtain a pale yellow solid product. And grinding the dried product into powder, heating to 230 ℃ in a tube furnace at the speed of 5 ℃/min, preserving heat for 1.5 h, and naturally cooling to room temperature. Wherein the gas atmosphere is air. The product Pt/Co NSs is obtained. And (3) immersing Pt/Co NSs into concentrated nitric acid to corrode for 3 h, washing a sample by using deionized water, and freeze-drying to obtain a product a-Pt NMs.
Example 3
The preparation of the a-Pt NMs comprises the following steps:
first 8 mg Pt (acac)2、0.5 mg Co(acac)3The resulting solution was stirred with 10 mg NaBr in 7 mL of ethanol at room temperature for 12 hours. In the ethanol solution, the volume ratio of ethanol to deionized water is 6: 1.
Then, the above solution was transferred to an oven to be dried at 60 ℃ to obtain a pale yellow solid product. And grinding the dried product into powder, heating to 230 ℃ in a tube furnace at the speed of 5 ℃/min, preserving heat for 3 h, and naturally cooling to room temperature. Wherein the gas atmosphere is air. The product Pt/Co NSs is obtained. And (3) immersing Pt/Co NSs into concentrated nitric acid to corrode for 3 h, washing a sample by using deionized water, and freeze-drying to obtain a product a-Pt NMs.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104551000A (en) * | 2014-12-23 | 2015-04-29 | 国家纳米科学中心 | Platinum-cobalt nano-alloy mimic enzyme and preparing method and purpose thereof |
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| KR20190049276A (en) * | 2017-11-01 | 2019-05-09 | 부산대학교 산학협력단 | Pt-CoO NANO PARTICLE, MANUFACTURING METHOD OF THE SAME AND CATALYST COMPRISING THE SAME |
| CN109877342A (en) * | 2019-03-26 | 2019-06-14 | 中国科学技术大学 | Amorphous noble metal nanosheet and preparation method thereof |
| CN109904472A (en) * | 2017-12-11 | 2019-06-18 | 中国科学院大连化学物理研究所 | An amorphous PtSe electrocatalyst and its preparation and application |
-
2020
- 2020-02-14 CN CN202010093273.0A patent/CN111118524A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104551000A (en) * | 2014-12-23 | 2015-04-29 | 国家纳米科学中心 | Platinum-cobalt nano-alloy mimic enzyme and preparing method and purpose thereof |
| KR20190049276A (en) * | 2017-11-01 | 2019-05-09 | 부산대학교 산학협력단 | Pt-CoO NANO PARTICLE, MANUFACTURING METHOD OF THE SAME AND CATALYST COMPRISING THE SAME |
| CN109904472A (en) * | 2017-12-11 | 2019-06-18 | 中国科学院大连化学物理研究所 | An amorphous PtSe electrocatalyst and its preparation and application |
| CN109680224A (en) * | 2019-01-16 | 2019-04-26 | 南京理工大学 | A kind of preparation method of nano porous palladium base noncrystal alloy |
| CN109877342A (en) * | 2019-03-26 | 2019-06-14 | 中国科学技术大学 | Amorphous noble metal nanosheet and preparation method thereof |
Non-Patent Citations (4)
| Title |
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| MAZAL CARMIEL-KOSTAN ET.AL: "Composition−Reactivity Correlations in Platinum−Cobalt Nanoporous Network as Catalyst for Hydrodeoxygenation of 5‑Hydroxymethylfurfural", 《J. PHYS. CHEM. C》 * |
| 吕兰芬: "纳米多孔铂基金属材料的脱合金法制备及其工艺研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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