CN107170998B - A kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle - Google Patents
A kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle Download PDFInfo
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- CN107170998B CN107170998B CN201710339066.7A CN201710339066A CN107170998B CN 107170998 B CN107170998 B CN 107170998B CN 201710339066 A CN201710339066 A CN 201710339066A CN 107170998 B CN107170998 B CN 107170998B
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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
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
- H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
- H01M8/1013—Other direct alcohol fuel cells [DAFC]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The present invention provides a kind of preparation methods of black phosphorus graphene composite material supported precious metal nano-particle; include the steps for preparing a black phosphorus graphene composite material: after black phosphorus nanoscale twins material and graphene nano sheet layer material are carried out ball milling under protection of argon gas; it is washed respectively with ethyl alcohol and water; suction filtration obtains black phosphorus graphene composite material, and vacuum drying is collected；It again disperses black phosphorus graphene composite material in ethyl alcohol, stabilizer and metal precursor, continual ultrasonic stirring is added after ultrasonic treatment, adjusting pH is 9-11, reducing agent is added, it is lasting to stir, up to black phosphorus graphene composite material supported precious metal nano-particle after vacuum drying.The combination of black phosphorus graphene composite material carrier and noble metal is more preferable in the present invention, effectively raises the electro-chemical activity and stability of fuel-cell catalyst, and preparation process is easy to operate, is suitble to large-scale production.
Description
Technical field
The invention belongs to materialogy fields, are related to a kind of fuel battery anode catalyst material, specifically a kind of black
The preparation method of phosphorus graphene composite material supported precious metal nano-particle.
Background technique
Since the increasingly depleted and problem of environmental pollution of global fossil energy resources increasingly sharpens, it is badly in need of people and looks for
Cleaning, the efficient novel environment friendly energy.Wherein, fuel cell is since with energy density, high, fuel source is applied extensively
In every field, the key of fuel cell power conversion efficiency is catalyst.Direct alcohol fuel cell elctro-catalyst is with your gold
Based on category, but the reserves of noble metal in nature are limited and expensive, vulnerable to poisoning for intermediate product.So expensive
Metal needs will carry out compound with other materials, wherein black phosphorus graphene composite material has biggish specific surface area, suitable band
Gap, good thermal stability and chemical stability etc., black phosphorus graphene composite material can change the structure of black phosphate material, make
The chemical active sites for obtaining material surface increase, and therefore, black phosphorus graphene composite material has preferable development prospect.
Summary of the invention
For above-mentioned technical problem existing for catalyst in the prior art, the present invention provides a kind of black phosphorus graphene is compound
The preparation method of material load noble metal nano particles, this new black phosphorus graphene composite material carried noble metal nanometer
The catalytic activity that the preparation method of particle will solve direct alcohol fuel cell catalyst in the prior art is not high, expensive
Technical problem.
The present invention provides a kind of preparation methods of black phosphorus graphene composite material supported precious metal nano-particle, including such as
Lower step:
1) prepare black phosphorus graphene composite material the step of, by black phosphorus nanoscale twins material and graphene nano lamella
Material mechanical ball mill 24-48h under protection of argon gas, the matter of the black phosphorus nanoscale twins material and graphene nano sheet layer material
Amount, by obtained precursor ethyl alcohol and deionized water difference centrifuge washing 2 ~ 6 times, carries out collected by suction than being 1:1.5 ~ 2.5,
Again black phosphorus graphene composite material will be obtained after above-mentioned product vacuum drying；
2) prepare black phosphorus graphene composite material supported precious metal nano-particle the step of, black phosphorus graphene is compound
Material is scattered in ethyl alcohol, is added stabilizer and metal precursor after ultrasonic treatment, the black phosphorus graphene composite material and
The mass ratio of stabilizer is 1:1 ~ 10, and the metal in the metal precursor is platinum, palladium, gold or silver, the metal front
The quality of metal is the 10 ~ 30% of the sum of black phosphorus graphene composite material and metal quality in body, persistently stirs 8-12h, adjusts pH
For 9-11, reducing agent is added, the reducing agent is potassium borohydride, sodium borohydride or hydrazine hydrate, metal precursor and reduction
The mass ratio of agent is 1:1 ~ 100, persistently stirs 1-5h, and black phosphorus graphene composite material carried noble metal is obtained after vacuum drying
Nanoparticle.
Further, the stabilizer is CTAB.
Further, in step 1), the mass ratio of black phosphorus and graphene is 1:1 ~ 3.
Further, in the black phosphorus graphene composite material supported precious metal nano-particle, the content of noble metal
For 1-90wt%.
Further, based on red phosphorus, mechanical ball mill obtains the black phosphorus material under protection of argon gas.
Further, the grapheme material is prepared based on graphene activation.
Further, its composite construction is black by applying external force mechanical ball mill in the black phosphorus graphene composite material
What phosphorus and graphene obtained.
After black phosphorus nanoscale twins material and graphene nano sheet layer material are carried out ball milling under protection of argon gas by the present invention, use
Ethyl alcohol and water wash respectively, finally filter and obtain black phosphorus graphene composite material, and vacuum drying is collected；Black phosphorus graphene is answered again
Condensation material is scattered in ethyl alcohol, and stabilizer and metal precursor, the metal in the metal precursor are added after ultrasonic treatment
For platinum, palladium, gold or silver, continual ultrasonic stirring, adjusting pH is 9-11, adds reducing agent, lasting to stir, after vacuum drying i.e.
Obtain black phosphorus graphene composite material supported precious metal nano-particle.
It is obtained by testing characterization, black phosphorus and graphene effectively form composite construction, and realize multiple element
Co-doped, electronic structure between present invention combination composite construction carrier and noble metal influences, so that its catalyst is in alkali
Property alcohols in have preferable electro catalytic activity and electrochemical stability.
Compared with prior art, the present invention its technological progress is significant.The present invention is answered with what black phosphorus and graphene were formed
Structure is closed, the combination of black phosphorus graphene composite material carrier and noble metal is more preferable, and shape characteristic is at sheet, platinum, palladium, gold or silver
Nanoparticle is evenly distributed and has good electro catalytic activity in alkaline alcohols.The present invention effectively improves fuel cell
The electro-chemical activity and stability of catalyst, and preparation process is simple and clear, is suitble to large-scale production, uses valence with certain
Value.
Detailed description of the invention
Fig. 1 is the XRD diagram that the resulting black phosphorus graphene composite material of embodiment 1 loads Pd nano particle.
Fig. 2 is the TEM figure and EDS-mapping figure of the resulting black phosphorus graphene composite material of embodiment 1.
Fig. 3 is the XPS figure that the resulting black phosphorus graphene composite material of embodiment 1 loads Pd nano particle.
Fig. 4 is that the resulting black phosphorus graphene composite material of embodiment 1 loads Pd nano particle in 1M NaOH+1M
CH3CH2Cyclic voltammogram in OH.
Fig. 5 is that the composite material of the resulting different black phosphorus graphene ratios of embodiment 1 loads Pd nano particle in 1M NaOH
+1M CH3CH2Cyclic voltammogram in OH.
Fig. 6 is that the resulting black phosphorus graphene composite material of embodiment 1 loads Pd nano particle in 1M NaOH+1M
CH3CH2Time current curve in OH.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle, specifically includes the following steps:
(1) preparation of black phosphorus graphene composite material
1. the preparation of black phosphorus: taking 2g red phosphorus and 15mL ultrapure water to be added in the water heating kettle of 25mL together at room temperature, 200
Heat steams 12h at DEG C, for removing the oxide layer on red phosphorus surface.After then taking out and drying, 0.5-1h is ground with agate mortar, so
By multilayer black phosphorus presoma, argon filling gas shielded carries out mechanical ball mill, ball milling 24-48h at normal temperatures and pressures afterwards, and revolving speed is maintained at
500r/min.Black phosphorus is obtained after the completion of mechanical ball mill.
2. the activation method of graphene: graphene is impregnated 12 h, sample obtained in 6 M potassium hydroxide solutions
Using deionized water and dehydrated alcohol eccentric cleaning, then sample is put in in 60 DEG C of baking oven dry 12 h, in nitrogen
800 DEG C of 2 h of calcining, heating rate are 5 DEG C/min.Activated graphene is obtained after naturally cool to collecting after room temperature.
3. the preparation of black phosphorus graphene composite material: by black phosphorus nanoscale twins material and graphene nano sheet layer material in argon
Under gas shielded, by 500r/min mechanical ball mill 24-48h, obtained precursor ethyl alcohol and deionized water is centrifuged respectively and washed
It washs three times, then carries out collected by suction, then will obtain black phosphorus graphene composite material after 40 DEG C of product above-mentioned vacuum drying.
(2) preparation of black phosphorus graphene composite material supported precious metal nano-particle
It disperses black phosphorus graphene composite material in ethyl alcohol, stabilizer and metal precursor, institute is added after ultrasonic treatment
The ratio of the black phosphorus graphene composite material and stabilizer stated is 1:1 ~ 10, and the metal in the metal precursor is platinum, palladium, gold
Or silver, persistently stir 8-12h.Adjusting pH is 9-11, adds reducing agent, and the reducing agent is potassium borohydride, sodium borohydride
Or hydrazine hydrate, the mass ratio of metal precursor and reducing agent are 1:1 ~ 100, the quality of the metal is in Heteroatom doping
The 10 ~ 30% of the sum of empty carbon ball and metal quality, persistently stir 1-5h, and black phosphorus graphene composite material is obtained after vacuum drying
Supported precious metal nano-particle.
The XRD diagram of black phosphorus graphene composite material supported precious metal nano-particle obtained above, as shown in Figure 1.From figure
In find out (020), (040), (060) three peak of black phosphorus, (002) characteristic peak and metal Pd of C element in graphene
(111), (200), (220), (311) four characteristic diffraction peaks, it was confirmed that black phosphorus graphene composite material supported precious metal palladium is received
Rice corpuscles.
The TEM of above-mentioned resulting black phosphorus graphene composite material schemes and EDS-mapping figure, as shown in Figure 2.It can from figure
To find out, there are two kinds of elements of P, C, and be evenly distributed.
By above-mentioned resulting black phosphorus graphene composite material supported precious metal nano-particle, elemental analysis is carried out using XPS,
As a result as shown in figure 3, after as can be seen from the figure BP-G loads Pd nanoparticle, the peak 3d of Pd exists, and thus proves, success
Load Pd nano particle.
Fig. 4 corresponding is black phosphorus graphene composite material supported precious metal nano-particle in 1M NaOH+1M CH3CH2OH
In cyclic voltammogram.It can be seen from the figure that the initial oxidation potential of black phosphorus graphene composite material load Pd nano particle
It is apparently higher than activated carbon-carried palladium；Black phosphorus graphene composite material load Pd nano particle the oxidate current for just sweeping ethyl alcohol be
1592mA mg-1Compared to the 600 mA mg of oxidate current for just sweeping ethyl alcohol of activated carbon-carried palladium-1, it is its 2.65 times, from
And proving black phosphorus graphene composite material load Pd nano particle has higher oxidation activity to ethyl alcohol.
Fig. 5 is corresponding be different black phosphorus graphene ratios composite material supported precious metal nano-particle 1M NaOH+
1M CH3CH2The cyclic voltammogram for carrying out electro-chemical activity test in OH to it, when black phosphorus and graphene ratio are 1:2, just
The oxidate current for sweeping ethyl alcohol is 1592mA mg-1, ethyl alcohol is just swept compared to black phosphorus and graphene ratio for 1:1 and 1:3
Oxidate current is respectively 747 mA mg-1With 610 mA mg-1, it is their 2.13 times and 2.61 times, to prove black phosphorus
Graphene composite material, which loads Pd nano particle, has higher oxidation activity to ethyl alcohol.
Fig. 6 corresponding is time current curve of the black phosphorus graphene composite material load Pd nano particle in ethanol solution
It is higher.After 3600s, the electric current of black phosphorus graphene composite material load Pd nano particle remains 391 mA mg-1, compare
In 12.3 mA mg of activated carbon-carried palladium-1It is higher by 30 times.To demonstrate black phosphorus graphene composite material load Pd nano particle
There is better electrochemical stability in ethanol.
Claims (7)
1. a kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle, it is characterised in that including walking as follows
It is rapid:
1) prepare black phosphorus graphene composite material the step of, by black phosphorus nanoscale twins material and graphene nano sheet layer material
Mechanical ball mill 24-48h under protection of argon gas, the mass ratio of the black phosphorus nanoscale twins material and graphene nano sheet layer material
For 1:1.5~2.5, obtained presoma ethyl alcohol and deionized water are distinguished centrifuge washing 2~6 times, carry out collected by suction, then
Black phosphorus graphene composite material will be obtained after presoma vacuum drying after collected by suction；
2) prepare black phosphorus graphene composite material supported precious metal nano-particle the step of, by black phosphorus graphene composite material
It is scattered in ethyl alcohol, stabilizer and metal precursor, the black phosphorus graphene composite material and stabilization is added after ultrasonic treatment
The mass ratio of agent is 1:1~10, and the metal in the metal precursor is platinum, palladium, gold or silver, in the metal precursor
The quality of metal is the 10~30% of the sum of black phosphorus graphene composite material and metal quality, persistently stirs 8-12h, adjusts pH and is
9-11, adds reducing agent, and the reducing agent is potassium borohydride, sodium borohydride or hydrazine hydrate, metal precursor and reducing agent
Mass ratio be 1:1~100, persistently stir 1-5h, obtain black phosphorus graphene composite material carried noble metal after vacuum drying
Nanoparticle.
2. a kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle according to claim 1,
It is characterized by: the stabilizer is CTAB.
3. a kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle according to claim 1,
It is characterized by: the mass ratio of black phosphorus and graphene is 1:2 in step 1).
4. a kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle according to claim 1,
It is characterized by: the content of noble metal is 1- in the black phosphorus graphene composite material supported precious metal nano-particle
90wt%.
5. a kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle according to claim 1,
It is characterized by: the black phosphorus material is based on red phosphorus, mechanical ball mill is obtained under protection of argon gas.
6. a kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle according to claim 1,
It is characterized by: the grapheme material is prepared based on graphene activation.
7. a kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle according to claim 1,
It is characterized by: its composite construction is by applying external force mechanical ball mill black phosphorus and stone in the black phosphorus graphene composite material
What black alkene obtained.
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| CN107802835B (en) * | 2017-12-04 | 2020-12-08 | 中南大学 | Black phosphorus nanosheet/platinum nanoparticle composite material and preparation method and application thereof |
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| CN108598510A (en) * | 2018-04-17 | 2018-09-28 | 上海电力学院 | A kind of preparation method of nickel oxide graphene composite material supported precious metal nano-particle |
| CN108483416A (en) * | 2018-05-08 | 2018-09-04 | 戚明海 | A kind of black phosphorus and preparation method thereof of boride modification |
| CN110327961A (en) * | 2019-07-12 | 2019-10-15 | 上海电力大学 | A kind of preparation method of black phosphorus-activated graphene hetero-junctions load nitridation nickel particle |
| CN111509241B (en) * | 2020-05-29 | 2021-07-13 | 贵州大学 | Black phosphorus @ titanium dioxide supported noble metal composite material and preparation method thereof |
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| CN113336206B (en) * | 2021-07-20 | 2022-05-17 | 哈尔滨工程大学 | Method for synthesizing porous black phosphorus nanosheet for negative electrode material of ion battery |
| CN113921835B (en) * | 2021-08-26 | 2023-06-06 | 上海空间电源研究所 | Preparation method of high-temperature proton exchange membrane fuel cell cathode catalyst |
| CN114015120B (en) * | 2021-12-03 | 2023-08-08 | 江苏万纳普新材料科技有限公司 | Antibacterial agent for plastic modification based on black phosphazene and preparation method thereof |
| CN115849316A (en) * | 2022-11-26 | 2023-03-28 | 昆明理工大学 | Preparation method of black phosphorus-based nano composite material |
| CN116443862A (en) * | 2023-03-14 | 2023-07-18 | 昆明理工大学 | High-performance sodium ion battery negative electrode material and preparation method thereof |
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| CN105217611B (en) * | 2015-09-21 | 2017-07-21 | 东南大学 | The preparation method of black phosphorus alkene quantum dot graphene nanometer sheet three-dimensional composite material |
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