CN112717924A - Method for rapidly synthesizing monatomic catalyst by plasma sputtering method and application thereof - Google Patents
Method for rapidly synthesizing monatomic catalyst by plasma sputtering method and application thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000002294 plasma sputter deposition Methods 0.000 title claims abstract description 14
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 5
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 14
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 14
- 238000000151 deposition Methods 0.000 claims abstract description 11
- 230000008021 deposition Effects 0.000 claims abstract description 10
- 238000004544 sputter deposition Methods 0.000 claims abstract description 8
- 229910003087 TiOx Inorganic materials 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 238000003487 electrochemical reaction Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 claims description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 32
- 229910052751 metal Inorganic materials 0.000 abstract description 14
- 239000002184 metal Substances 0.000 abstract description 14
- 239000000758 substrate Substances 0.000 abstract description 12
- 229910021397 glassy carbon Inorganic materials 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 238000011068 loading method Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 2
- 239000010935 stainless steel Substances 0.000 abstract description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 229910052697 platinum Inorganic materials 0.000 description 5
- 239000013077 target material Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001308 synthesis method Methods 0.000 description 3
- 239000011149 active material Substances 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000012937 correction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012612 commercial material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
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Abstract
本发明公布等离子溅射法快速合成一种单原子催化剂的方法及其应用，催化剂载体和活性金属均由等离子溅射方法合成，合成的Pt1/TiOx单原子催化剂催化性能优异。以玻碳片、钛网、不锈钢片、碳纸等作为基板，以载体靶材和活性金属靶材为原料；将基板置于载物台，采用三靶材等离子溅射仪将载体和活性金属交替溅射沉积在基板上，交替沉积若干次即可得到催化剂样品。本发明具有活性金属负载量可控、合成速度快、工艺简单、能耗低等优点，例子中制备的催化剂在过电位50mv时，质量比活性和转换效率(TOF)分别是20％商业铂炭的11.05倍和3.5倍。
The invention discloses a method for rapidly synthesizing a single-atom catalyst by plasma sputtering and its application. The catalyst carrier and active metal are both synthesized by the plasma sputtering method, and the synthesized Pt 1 /TiO x single-atom catalyst has excellent catalytic performance. The glassy carbon sheet, titanium mesh, stainless steel sheet, carbon paper, etc. are used as the substrate, and the carrier target and active metal target are used as raw materials; the substrate is placed on the stage, and the carrier and active metal are separated by a three-target plasma sputtering instrument Alternate sputter deposition on the substrate, alternate deposition several times to obtain catalyst samples. The invention has the advantages of controllable active metal loading, fast synthesis speed, simple process, low energy consumption, etc. When the overpotential of the catalyst prepared in the example is 50mv, the mass specific activity and conversion efficiency (TOF) are respectively 20% of commercial platinum carbon 11.05 times and 3.5 times.
Description
Technical Field
The invention belongs to the field of catalysis, and particularly relates to rapid synthesis of a monatomic catalyst by combining a plasma sputtering method with a catalyst preparation technology, namely, synthesis of a monatomic catalyst material by applying a plasma sputtering technology.
Background
With the gradual depletion of fossil fuels, one potential solution is to convert solar energy, wind energy and other energy sources into electric energy for temporary storage and then discharge the electric energy when needed (peak clipping and valley filling). In view of the scale of clean energy utilization, such energy storage systems must be inexpensive and efficient, and easy to store and transport. Water is converted into hydrogen energy through electrochemical reaction, so that high-efficiency conversion and storage of electric energy generated by renewable clean energy to chemical energy can be realized, and sustainable development and utilization of clean energy such as solar energy, wind energy and the like are facilitated.
The electrochemical reaction converts water into hydrogen energy, and the use of a high-efficiency electro-catalytic Hydrogen Evolution (HER) catalyst is not available. But the scarcity of resources, high price and the like limit the industrial application of platinum. Therefore, the low load and high quality specific activity of the monatomic catalysis fully makes up the defect of insufficient resources and promotes the industrial application of the platinum. The traditional metal nano catalyst, particularly the monatomic catalyst, has the disadvantages of high synthesis difficulty, complex process flow, high energy consumption, long time consumption and difficult control of the size of the active metal.
In order to overcome the defects of the prior art, the invention mainly aims to solve the technical problems of finding a catalyst synthesis method which has the advantages of short synthesis period, simple process, low production cost, environmental friendliness and the like, improving the utilization rate of active metals, reducing the use amount of resources such as noble metals and the like, simplifying the synthesis complexity of a monatomic catalyst, synthesizing the catalyst rapidly on a large scale, and making up for the defect of difficult synthesis of common catalysts, particularly monatomic catalysts.
Disclosure of Invention
The invention aims to mainly find a catalyst synthesis method with the advantages of simple synthesis method, good process control, low production cost, environmental friendliness and the like and a high-quality catalyst with high catalytic activity by combining a plasma sputtering technology and a catalyst synthesis technology. Makes up for some of the disadvantages of the traditional catalyst synthesis process.
Synthesis of monatomic Pt1/TiOxCatalyst, Pt being dispersed in monoatomic formThe conditions are that the absolute pressure is 20pa, and the gas environment is Ar: N2The volume ratio is 9:1, the sputtering working current is 5mA, and the duration is 1 second; TiO 2xThe carrier deposition condition is 20pa absolute pressure, and the gas environment is Ar: N2The volume ratio is 9:1, the working current of sputtering deposition is 19mA, and the duration is 60 seconds;
pt and TiOxThe catalyst was obtained by alternately depositing 15 times each.
The prepared catalyst is used as a catalyst when water is converted into hydrogen energy through an electrochemical reaction.
The carrier target material used in the invention is a black titanium oxide target material with the purity of 99.99 percent, the active material target material is a platinum (Pt) target material with the purity of 99.99 percent, and the substrate is a glassy carbon sheet. Simultaneously mounting two targets on a three-target plasma sputtering instrument; the substrate is placed at a specified absolute pressure of 20pa and Ar: N2After setting the working time of the plasma sputtering apparatus on a stage in a gas atmosphere of 9:1 (volume ratio), the sputtering deposition of the carrier and the active metal is started, and the stage alternately deposits black titanium oxide in the platinum target for several times to obtain the 'sandwich-like' catalyst film. The invention finally obtains the ultralow-load Pt with high catalytic activity1/TiOxA monatomic catalyst (see figures 2-3).
The substrate with the catalyst attached to a specific area was subjected to electrochemical testing. The activity of the catalyst is tested by using a traditional three-electrode system, and specifically the test environment is 0.5M sulfuric acid, the reference electrode is a saturated calomel electrode, the counter electrode is a carbon rod, and the working electrode is a glassy carbon sheet. The electrochemistry of commercial platinum carbon (Pt/C) was tested under the same conditions and compared (see FIG. 4).
The Pt content in the obtained catalyst can be calculated after an inductively coupled plasma mass spectrometry (ICP-MS) test to obtain the Pt loading capacity of the prepared monatomic catalyst. The aggregation state of the active metal Pt can be determined by a high-resolution electron microscope (HR-TEM), a spherical aberration correction electron microscope (AC-TEM) and the like.
The invention has the advantages that:
1. according to the analysis of the current catalyst material development condition, the catalyst development inertia thinking place is limited in the complex time-consuming chemical reaction synthesis field, the invention develops the combination of the plasma sputtering technology and the catalyst synthesis technology, and widens the research field and the research direction of the catalyst material development.
2. The method has the advantages of simple process flow, low energy consumption, short time consumption, low comprehensive cost and the like, and has the capability and space of large-scale development.
3. The catalyst developed by the invention can be attached to any conductor (such as a glass carbon sheet, stainless steel, carbon paper and the like) or even a semiconductor substrate without using an adhesive, and is more energy-saving and environment-friendly in synthesis and more convenient to use.
5. The catalyst developed by the invention has the advantages that the loading capacity of the active metal can be regulated and controlled, the particle size of the active metal can also be controlled, and the use amount of the noble metal or other active metals can be effectively controlled.
6. Pt developed by the present invention1/TiOxThe catalyst has high catalytic activity, and the specific activity of the catalyst is obviously superior to that of a commercial material.
Description of the drawings:
fig. 1 is a diagram of a single-atom high-angle annular dark field (HAADF) for each layer of catalyst Pt after debugging.
FIG. 2 shows the monoatomic Pt1/TiOxHigh Resolution Transmission Electron Microscopy (HRTEM) images of the catalyst.
FIG. 3 shows the monoatomic Pt1/TiOxCatalyst High Angle Annular Dark Field (HAADF) diagram.
Figure 4 is a graph comparing catalytic performance (HER) of the as-synthesized monatomic catalyst with 20% commercial platinum carbon (20%. Pt/C).
Detailed Description
The present invention will be described in further detail with reference to the practice of experimental facts, but the embodiments of the present invention are not limited thereto, and the carrier target, the active material target, and the substrate to be used are not limited thereto.
Example 1
Polishing the glassy carbon sheet substrate by using polishing powder, cleaning and placing the polished glassy carbon sheet substrate in a vacuum drying oven for drying for later use. The two used target materials are simultaneously arranged on a three-target plasma sputtering instrument; placing the glassy carbon sheet substrate at an absolute pressure of 20pa and Ar: N29:1 (volume ratio)) On a stage in a gas atmosphere, black titanium oxide (TiO)x) The single sputtering deposition working current is 19mA and the time length is 60 seconds, the working current is 5mA and the time length is 1 second when the platinum (Pt) is deposited by single sputtering, and 15 times of deposition are alternately carried out, thus obtaining the monatomic Pt1/TiOxA catalyst film. In particular, the parameters of vacuum degree, gas environment, time, current and the like of the deposition of the carrier and the active metal are conclusion values of the test that Pt is dispersed in a titanium oxide film carrier in a monoatomic form, which is explored in advance. The dispersed state of Pt in the monolayer catalyst is clearly a monoatomic level dispersion (see fig. 1).
The substrate with the catalyst attached to a specific area was subjected to electrochemical testing. The activity of the catalyst is tested by using a traditional three-electrode system, and specifically the test environment is 0.5M sulfuric acid, the reference electrode is a saturated calomel electrode, the counter electrode is a carbon rod, and the working electrode is a catalyst/glassy carbon sheet. Electrochemical measurements were made on 20% commercial platinum carbon (20%. Pt/C) under the same conditions, and the catalytic activity was compared with each other, and the results showed that the specific activity of the catalyst according to the present invention was 11.05 times that of the 20% commercial platinum carbon (see FIG. 4).
According to calculation after inductively coupled plasma mass spectrometry (ICP-MS) test, the Pt loading capacity of the monatomic catalyst prepared by the method is 1.6%. The aggregation state of the active metal Pt is determined to be monoatomic dispersion by means of a high-resolution electron microscope (HR-TEM), a spherical aberration correction electron microscope (AC-TEM) and the like, namely, the supported monoatomic Pt is successfully synthesized by means of a plasma sputtering method in the invention1A TiOx catalyst.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4046712A (en) * | 1972-11-30 | 1977-09-06 | United Kingdom Atomic Energy Authority | Catalysts sputtered on substantially nonporous low surface area particulate supports |
| WO2002057508A2 (en) * | 2001-01-17 | 2002-07-25 | N.V. Bekaert S.A. | Method for the production of sputtering targets |
| WO2017135136A1 (en) * | 2016-02-01 | 2017-08-10 | 国立大学法人北海道大学 | Structure in which single atoms are dispersed on support, method for manufacturing structure in which single atoms are dispersed on support, and sputtering device |
| CN111411386A (en) * | 2020-05-15 | 2020-07-14 | 北京工业大学 | A method for preparing platinum/titania nanotube composite electrode by atomic layer deposition |
-
2021
- 2021-01-07 CN CN202110018820.3A patent/CN112717924B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4046712A (en) * | 1972-11-30 | 1977-09-06 | United Kingdom Atomic Energy Authority | Catalysts sputtered on substantially nonporous low surface area particulate supports |
| WO2002057508A2 (en) * | 2001-01-17 | 2002-07-25 | N.V. Bekaert S.A. | Method for the production of sputtering targets |
| WO2017135136A1 (en) * | 2016-02-01 | 2017-08-10 | 国立大学法人北海道大学 | Structure in which single atoms are dispersed on support, method for manufacturing structure in which single atoms are dispersed on support, and sputtering device |
| CN111411386A (en) * | 2020-05-15 | 2020-07-14 | 北京工业大学 | A method for preparing platinum/titania nanotube composite electrode by atomic layer deposition |
Non-Patent Citations (1)
| Title |
|---|
| CHAO MA ET AL.: "Synthesis of TiO2/Pt/TiO2 multilayer films via radio frequency magnetron sputtering and their enhanced photocatalytic activity" * |
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Effective date of registration: 20231204 Address after: 610093 No. 5, Gaopeng Avenue, high tech Zone, Chengdu, Sichuan Patentee after: Sichuan Yalian Hydrogen Energy Technology Co.,Ltd. Address before: 100124 No. 100 Chaoyang District Ping Tian Park, Beijing Patentee before: Beijing University of Technology |