CN107170998A - 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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- CN107170998A CN107170998A CN201710339066.7A CN201710339066A CN107170998A CN 107170998 A CN107170998 A CN 107170998A CN 201710339066 A CN201710339066 A CN 201710339066A CN 107170998 A CN107170998 A CN 107170998A
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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 invention provides a kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle, including one the step of prepare black phosphorus graphene composite material：After black phosphorus nanoscale twins material and graphene nano sheet layer material are carried out into ball milling under argon gas protection, washed respectively with ethanol and water, suction filtration obtains black phosphorus graphene composite material, vacuum drying is collected；Black phosphorus graphene composite material is scattered in ethanol again, ultrasonically treated rear addition stabilizer and metal precursor, continual ultrasonic stirring, it is 9 11 to adjust pH, reducing agent is added, lasting stirring produces 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 more preferably, effectively raises the electro-chemical activity and stability of fuel-cell catalyst in the present invention, and preparation technology is easy to operate, is adapted to large-scale production.
Description
Technical field
The invention belongs to materialogy field, it is related to a kind of fuel battery anode catalyst material, it is specifically a kind of black
The preparation method of phosphorus graphene composite material supported precious metal nano-particle.
Background technology
Due to the increasingly depleted of global fossil energy resources and increasingly sharpening for problem of environmental pollution, it is badly in need of people and looks for
Cleaning, the efficient novel environment friendly energy.Wherein, fuel cell is due to energy density is high, fuel source is extensive and is employed
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 reserves of the noble metal in nature are limited and expensive, are vulnerable to poisoning for intermediate product.So, it is expensive
Metal needs will be combined with other materials, wherein, black phosphorus graphene composite material has larger specific surface area, suitable band
Gap, good heat endurance 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.
The content of the invention
The above-mentioned technical problem existed for catalyst in the prior art, it is compound the invention provides a kind of black phosphorus graphene
The preparation method of material load noble metal nano particles, described 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 invention provides a kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle, including such as
Lower step：
1) one the step of prepare black phosphorus graphene composite material, by black phosphorus nanoscale twins material and graphene nano sheet layer material
Mechanical ball mill 24-48h, described black phosphorus nanoscale twins material and the mass ratio of graphene nano sheet layer material under argon gas protection
For 1:1.5 ~ 2.5, obtained precursor ethanol and deionized water are distinguished into centrifuge washing 2 ~ 6 times, collected by suction is carried out, then will
Above-mentioned product vacuum obtains black phosphorus graphene composite material after drying；
2) one the step of prepare black phosphorus graphene composite material supported precious metal nano-particle, by black phosphorus graphene composite material
Be scattered in ethanol, it is ultrasonically treated after add stabilizer and metal precursor, described black phosphorus graphene composite material and stably
The mass ratio of agent is 1:1 ~ 10, during the metal in described metal precursor is platinum, palladium, gold or silver, described metal precursor
The quality of metal is the 10 ~ 30% of black phosphorus graphene composite material and metal quality sum, persistently stirs 8-12h, and regulation pH is
9-11, adds reducing agent, and described reducing agent is potassium borohydride, sodium borohydride or hydrazine hydrate, metal precursor and reducing agent
Mass ratio be 1:1 ~ 100,1-5h is persistently stirred, obtaining black phosphorus graphene composite material carried noble metal after vacuum drying receives
Rice corpuscles.
Further, described stabilizer is CTAB.
Further, step 1）In, the mass ratio of black phosphorus and graphene is 1:1~3.
Further, in described black phosphorus graphene composite material supported precious metal nano-particle, the content of noble metal
For 1-90wt%.
Further, based on red phosphorus, the mechanical ball mill under argon gas protection is obtained described black phosphorus material.
Further, described grapheme material is prepared based on graphene activation.
Further, its composite construction is black by applying external force mechanical ball mill in described black phosphorus graphene composite material
What phosphorus was obtained with graphene.
After black phosphorus nanoscale twins material and graphene nano sheet layer material are carried out ball milling by the present invention under argon gas protection, use
Ethanol and water are washed respectively, and last suction filtration obtains black phosphorus graphene composite material, and vacuum drying is collected；Black phosphorus graphene is answered again
Condensation material is scattered in ethanol, the ultrasonically treated rear metal added in stabilizer and metal precursor, described metal precursor
For platinum, palladium, gold or silver, continual ultrasonic stirring, regulation pH is 9-11, adds reducing agent, lasting stirring, after vacuum drying i.e.
Obtain black phosphorus graphene composite material supported precious metal nano-particle.
Obtained by testing sign, black phosphorus and graphene effectively forms composite construction, and realize multiple element
Co-doped, the electronic structure that the present invention is combined between 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, its technological progress is significant to the present invention.The present invention is with answering that black phosphorus and graphene are formed
Close structure, more preferably, shape characteristic is into sheet, platinum, palladium, gold or silver for the combination of black phosphorus graphene composite material carrier and noble metal
Nano-particle is evenly distributed and in alkaline alcohols with good electro catalytic activity.Effective raising fuel cell of the invention
The electro-chemical activity and stability of catalyst, and preparation technology is simple and clear, is adapted to large-scale production, with certain use valency
Value.
Brief description of the drawings
Fig. 1 is that the black phosphorus graphene composite material of the gained of embodiment 1 loads the XRD of Pd nano particle.
Fig. 2 is the TEM figures and EDS-mapping figures of the black phosphorus graphene composite material of the gained of embodiment 1.
Fig. 3 is the XPS figures of the black phosphorus graphene composite material load Pd nano particle of the gained of embodiment 1.
Fig. 4 is that the black phosphorus graphene composite material of the gained of embodiment 1 loads Pd nano particle in 1M NaOH+1M
CH3CH2Cyclic voltammogram in OH.
Fig. 5 is that the composite of the different black phosphorus graphene ratios of the gained of embodiment 1 loads Pd nano particle in 1M NaOH
+1M CH3CH2Cyclic voltammogram in OH.
Fig. 6 is that the black phosphorus graphene composite material of the gained of embodiment 1 loads Pd nano particle in 1M NaOH+1M
CH3CH2Time current curve in OH.
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 following steps：
(1) preparation of black phosphorus graphene composite material
1. the preparation of black phosphorus：2g red phosphorus and 15mL ultra-pure waters is taken to be added to together in 25mL water heating kettle at room temperature, at 200 DEG C
Heat steams 12h, for removing the oxide layer on red phosphorus surface.After then taking out and drying, 0.5-1h is ground with agate mortar, then will
Argon filling gas shielded carries out mechanical ball mill to multilayer black phosphorus presoma at normal temperatures and pressures, and ball milling 24-48h, rotating 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 soaked into 12 h in 6 M potassium hydroxide solutions, the sample obtained
Using deionized water and absolute ethyl alcohol eccentric cleaning, then sample is put in 60 DEG C of baking oven and dries 12 h, in nitrogen
800 DEG C of 2 h of calcining, heating rate is 5 DEG C/min.Activated graphene is obtained after naturally cool to being collected 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 is centrifuged respectively with ethanol and deionized water and washed
Wash three times, then carry out collected by suction, then will obtain black phosphorus graphene composite material after above-mentioned 40 DEG C of vacuum drying of product.
(2) preparation of black phosphorus graphene composite material supported precious metal nano-particle
Black phosphorus graphene composite material is scattered in ethanol, ultrasonically treated rear addition stabilizer and metal precursor are described
The ratio of black phosphorus graphene composite material and stabilizer is 1:1 ~ 10, the metal in described metal precursor is platinum, palladium, Jin Huo
Silver, persistently stirs 8-12h.Regulation pH is 9-11, adds reducing agent, described reducing agent is potassium borohydride, sodium borohydride or
The mass ratio of hydrazine hydrate, metal precursor and reducing agent is 1:1 ~ 100, the quality of described metal is the hollow of Heteroatom doping
Carbon ball and the 10 ~ 30% of metal quality sum, persistently stirs 1-5h, and black phosphorus graphene composite material is obtained after vacuum drying and is born
Supported noble metal nano-particle.
The XRD of black phosphorus graphene composite material supported precious metal nano-particle obtained above, as shown in Figure 1.From figure
In find out black phosphorus (020),（040）、（060）C element in three peaks, graphene（002）Characteristic peak and metal Pd
(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 figures and EDS-mapping figures of the black phosphorus graphene composite material of above-mentioned gained, as shown in Figure 2.Can from figure
To find out, there are two kinds of elements of P, C, and be evenly distributed.
By the black phosphorus graphene composite material supported precious metal nano-particle of above-mentioned gained, elementary analysis is carried out using XPS,
As a result as shown in figure 3, as can be seen from the figure after BP-G loads Pd nano-particles, Pd 3d peaks are present, and thus prove, success
Load Pd nano particle.
It is black phosphorus graphene composite material supported precious metal nano-particle in 1M NaOH+1M CH that Fig. 4 is corresponding3CH2OH
In cyclic voltammogram.It can be seen that black phosphorus graphene composite material loads the initial oxidation current potential of Pd nano particle
Apparently higher than activated carbon-carried palladium；Black phosphorus graphene composite material load Pd nano particle the oxidate current for just sweeping ethanol be
1592mA mg-1Compared to the mA mg of oxidate current 600 for just sweeping ethanol of activated carbon-carried palladium-1, it is its 2.65 times, from
And prove black phosphorus graphene composite material load Pd nano particle has higher oxidation activity to ethanol.
Fig. 5 is corresponding be different black phosphorus graphene ratios composite supported precious metal nano-particle 1M NaOH+
1M CH3CH2The cyclic voltammogram of electro-chemical activity test is carried out in OH to it, when black phosphorus and graphene ratio are 1:When 2, it is just
The oxidate current for sweeping ethanol is 1592mA mg-1, it is 1 compared to black phosphorus and graphene ratio:1 and 1:3 just sweep ethanol
Oxidate current is respectively 747 mA mg-1With 610 mA mg-1, it is their 2.13 times and 2.61 times, so as to prove black phosphorus
Graphene composite material loads Pd nano particle has higher oxidation activity to ethanol.
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.So as to demonstrate black phosphorus graphene composite material load Pd nano particle
There is more preferable 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 following step
Suddenly：
1）One the step of prepare black phosphorus graphene composite material, by black phosphorus nanoscale twins material and graphene nano sheet layer material
Mechanical ball mill 24-48h, described black phosphorus nanoscale twins material and the mass ratio of graphene nano sheet layer material under argon gas protection
For 1:1.5 ~ 2.5, obtained precursor ethanol and deionized water are distinguished into centrifuge washing 2 ~ 6 times, collected by suction is carried out, then will
Above-mentioned product vacuum obtains black phosphorus graphene composite material after drying；
2）One the step of prepare black phosphorus graphene composite material supported precious metal nano-particle, by black phosphorus graphene composite material
Be scattered in ethanol, it is ultrasonically treated after add stabilizer and metal precursor, described black phosphorus graphene composite material and stably
The mass ratio of agent is 1:1 ~ 10, during the metal in described metal precursor is platinum, palladium, gold or silver, described metal precursor
The quality of metal is the 10 ~ 30% of black phosphorus graphene composite material and metal quality sum, persistently stirs 8-12h, and regulation pH is
9-11, adds reducing agent, and described reducing agent is potassium borohydride, sodium borohydride or hydrazine hydrate, metal precursor and reducing agent
Mass ratio be 1:1 ~ 100,1-5h is persistently stirred, obtaining black phosphorus graphene composite material carried noble metal after vacuum drying receives
Rice corpuscles.
2. a kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle according to claim 1,
It is characterized in that：Described 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 in that：Step 1）In, the mass ratio of black phosphorus and graphene is 1:2.
4. a kind of preparation method of black phosphorus graphene composite material supported precious metal nano-particle according to claim 1,
It is characterized in that：In described black phosphorus graphene composite material supported precious metal nano-particle, the content of noble metal is 1-
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 in that：Based on red phosphorus, the mechanical ball mill under argon gas protection is obtained described black phosphorus material.
6. a kind of preparation method of black phosphorus graphene composite material noble metal nano particles according to claim 1, it is special
Levy and be：Described 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 in that：Its composite construction is by applying external force mechanical ball mill black phosphorus and stone in described black phosphorus graphene composite material
What black alkene was obtained.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107658475A (en) * | 2017-09-25 | 2018-02-02 | 青岛大学 | A kind of platinum/black phosphorus@carbon ball methanol fuel cell anode catalyzers and preparation method thereof |
| CN107737947A (en) * | 2017-10-18 | 2018-02-27 | 武汉大学 | A kind of preparation method of grapheme platinum silver metal nano composite material |
| CN107802835A (en) * | 2017-12-04 | 2018-03-16 | 中南大学 | A kind of black phosphorus nanometer sheet/nano platinum particle composite and its preparation method and application |
| CN108483416A (en) * | 2018-05-08 | 2018-09-04 | 戚明海 | A kind of black phosphorus and preparation method thereof of boride modification |
| CN108492907A (en) * | 2018-03-26 | 2018-09-04 | 北京旭碳新材料科技有限公司 | The graphene conductive material and preparation method thereof of nano metal modification |
| 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 |
| 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 |
| CN111509241A (en) * | 2020-05-29 | 2020-08-07 | 贵州大学 | Black phosphorus @ titanium dioxide supported noble metal composite material and preparation method thereof |
| CN112366327A (en) * | 2020-11-04 | 2021-02-12 | 湖北大学 | GO-MOF (Al) -supported palladium-bismuth-phosphorus alloy nano catalyst and preparation method thereof |
| CN113270600A (en) * | 2021-04-21 | 2021-08-17 | 上海电力大学 | Pd/P-NCNS catalyst for high-activity direct formic acid fuel cell and preparation and application thereof |
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| 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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| CN107658475A (en) * | 2017-09-25 | 2018-02-02 | 青岛大学 | A kind of platinum/black phosphorus@carbon ball methanol fuel cell anode catalyzers and preparation method thereof |
| CN107737947A (en) * | 2017-10-18 | 2018-02-27 | 武汉大学 | A kind of preparation method of grapheme platinum silver metal nano composite material |
| CN107802835A (en) * | 2017-12-04 | 2018-03-16 | 中南大学 | A kind of black phosphorus nanometer sheet/nano platinum particle composite and its preparation method and application |
| 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 |
| CN108492907B (en) * | 2018-03-26 | 2020-08-21 | 北京旭碳新材料科技有限公司 | Nano-metal modified graphene conductive material and preparation method thereof |
| CN108492907A (en) * | 2018-03-26 | 2018-09-04 | 北京旭碳新材料科技有限公司 | The graphene conductive material and preparation method thereof of nano metal modification |
| 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 |
| CN111509241A (en) * | 2020-05-29 | 2020-08-07 | 贵州大学 | Black phosphorus @ titanium dioxide supported noble metal composite material and preparation method thereof |
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| CN113336206A (en) * | 2021-07-20 | 2021-09-03 | 哈尔滨工程大学 | Method for synthesizing porous black phosphorus nanosheet for negative electrode material of ion battery |
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| 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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