CN109100402A - A kind of monoatomic method of deposition platinum, compound and application - Google Patents
A kind of monoatomic method of deposition platinum, compound and application Download PDFInfo
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Abstract
The invention discloses a kind of monoatomic method of deposition platinum, compound and applications, wherein the deposition monoatomic method of platinum is comprising steps of in a solvent by the dispersion of metal phosphide nanometer sheet, be prepared dispersion liquid；By the dispersant liquid drop on carbon paper, it is used as working electrode after dry, using saturated calomel electrode as reference electrode, platinum electrode is used as to electrode；Electrolyte is prepared, electrolytic cell has been set up, certain voltage and certain circulating ring number is set, deposits to obtain platinum on metal phosphide nanometer sheet surface monatomic.The method of the invention is not necessarily to complex device, easy to operate, applied widely, is suitable for various metals phosphide material, and the catalytic performance of prepared compound is promoted significantly, while also providing a kind of new thinking to study monatomic catalysis.
Description
Technical field
The present invention relates to catalyst field more particularly to a kind of monoatomic methods of deposition platinum, compound and application.
Background technique
Currently, developing a kind of efficient catalyst is one of main research of catalyst field.Load type metal
Catalyst has an excellent catalytic performance, and the catalytic performance of loaded catalyst and its ruler of movable metallic component on carrier
It is very little closely related.In order to reach the catalytic effect of load type metal catalyst most preferably, the size of active metal constantly becomes smaller.It is single
Catalyst atom is that a kind of metal is evenly distributed on supported catalyst in the form of monoatomic.
Since Dalian materialization Zhang Tao seminar prepared monatomic Pt/FeO earliest in 2011xCatalyst
(Nature chemistry, 2011,3 (8): 634-641), the catalyst obtain in CO oxidation and CO selective oxidation reaction
Very high catalytic activity and stability, and thus propose the concept of monatomic catalysis.2012, E. Charles H.
Sykes seminar is dispersed in the surface Cu using monatomic Pd, and the catalyst of atom dispersion is characterized using means such as STM, should
Catalyst has selectivity (Science, 2012,335 (6073): 1209-1212) well for hydrogenation reaction.2014,
The Fe/SiO of the packet letter atom level dispersion standby with project team system2It makes important progress in methane anaerobic ethylene and anti-structure
(Sciense, 2014,334 (6184): 616-619.2016, the peak Zheng Nan seminar was synthesized with simple photochemical method
Pd/TiO2The catalyst of single atomic dispersion in olefin hydrogenation with splendid activity (Science, 2016,352
(6287): 797-800).The fast development of monatomic catalyst causes the extensive concern of numerous researchers, however, existing skill
For the preparation method of monatomic catalyst in the presence of the device is complicated, experimental implementation difficulty is big, and the scope of application is small, and prepared in art
The low problem of the catalytic performance of monatomic catalyst.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of monoatomic methods of deposition platinum, multiple
Close object and application, it is intended to solve the preparation method of monatomic catalyst in the prior art in the presence of the device is complicated, operation difficulty is big, fits
It is small with range, the low problem of the catalytic performance of prepared monatomic catalyst.
Technical scheme is as follows:
One kind depositing the monoatomic method of platinum on metal phosphide nanometer sheet surface, wherein the following steps are included:
In a solvent by the dispersion of metal phosphide nanometer sheet, dispersion liquid is prepared；
By the dispersant liquid drop on carbon paper, it is used as working electrode after dry, using saturated calomel electrode as reference electrode, platinum electricity
Pole is used as to electrode；
Electrolyte is prepared, electrolytic cell has been set up, certain voltage and certain circulating ring number is set, in metal phosphide nanometer sheet
Surface deposits to obtain platinum monatomic.
Described deposits the monoatomic method of platinum on metal phosphide nanometer sheet surface, wherein the metal phosphide is received
Rice piece in metallic element be group VIII metal element, Group IVB metallic element, VB race metallic element, group vib metallic element,
One of VIIB race metallic element and Group IIB metal element are a variety of.
Described deposits the monoatomic method of platinum on metal phosphide nanometer sheet surface, wherein the metal phosphide is received
Metallic element in rice piece is one of iron, cobalt, nickel, manganese, zinc, chromium, tin, lead, molybdenum or a variety of.
Described deposits the monoatomic method of platinum on metal phosphide nanometer sheet surface, wherein the solvent is containing naphthols
Aqueous isopropanol.
It is described to deposit the monoatomic method of platinum on metal phosphide nanometer sheet surface, wherein the isopropanol with it is described
The volume ratio of naphthols is 10:1 ~ 1000:1.
Described deposits the monoatomic method of platinum on metal phosphide nanometer sheet surface, wherein the quality of the dispersion liquid
Concentration is 1 ~ 5 mg/mL.
Described deposits the monoatomic method of platinum on metal phosphide nanometer sheet surface, wherein the carbon paper is 1 square li
The carbon paper of rice；The volume that the dispersion liquid is added dropwise on the carbon paper is 50 ~ 500 μ L.
Described deposits the monoatomic method of platinum on metal phosphide nanometer sheet surface, wherein the electrolyte is that pH is 1
~ 3 acidic electrolysis bath, voltage are 0 ~ -1.3 V, and circulating ring number is 1000 ~ 15000 circles.
A kind of compound, wherein be prepared using method as described above；The compound includes that metal phosphide is received
Rice piece and the platinum for being grown on metal phosphide nanometer sheet surface are monatomic.
A kind of application of compound as described above, wherein the compound is applied to electro-catalysis water decomposition.
The utility model has the advantages that the present invention, which provides one kind, deposits the monoatomic method of platinum on metal phosphide nanometer sheet surface, pass through
Use the carbon paper of carried metal phosphide nanometer sheet for working electrode, saturated calomel electrode is reference electrode, and platinum electrode is to electricity
Certain voltage and circulating ring number are arranged in the electrolytic solution, and then deposits to obtain platinum list on metal phosphide nanometer sheet surface for pole
Atom.The method of the invention is not necessarily to complex device, easy to operate, applied widely, is suitable for various metals phosphide material,
And the catalytic performance of prepared compound is promoted significantly, while also providing a kind of new thinking to study monatomic catalysis.
Detailed description of the invention
Fig. 1 is that the embodiment of the present invention 1 deposits the monoatomic flow diagram of platinum.
Fig. 2 is the Co prepared in the embodiment of the present invention 10.5Ni0.5PxThe transmission plot of nanometer sheet.
Fig. 3 is the Pt-Co prepared in the embodiment of the present invention 10.5Ni0.5PxThe LSV of the OER of compound schemes.
Fig. 4 is the Pt-Co prepared in the embodiment of the present invention 20.25Ni0.75PxThe LSV of the HER of compound schemes.
Fig. 5 is the Pt-Co prepared in the embodiment of the present invention 30.25Ni0.75PxThe LSV of the HER of compound schemes.
Fig. 6 is the Pt-CoP prepared in the embodiment of the present invention 4xThe LSV of the HER of compound schemes.
Specific embodiment
The present invention provides a kind of monoatomic method of deposition platinum, compound and application, to make the purpose of the present invention, technical side
Case and effect are clearer, clear, and the present invention is described in more detail below.It should be appreciated that specific reality described herein
It applies example to be only used to explain the present invention, be not intended to limit the present invention.
The present invention provides a kind of in the metal phosphide nanometer sheet surface deposition monoatomic method of platinum, comprising:
Step A, dispersion liquid in a solvent by the dispersion of metal phosphide nanometer sheet, is prepared；
Step B, the dispersant liquid drop is regard as working electrode after dry on carbon paper, it is electric using saturated calomel electrode as reference
Pole, platinum electrode are used as to electrode；
Step C, electrolyte is prepared, electrolytic cell has been set up, certain voltage and certain circulating ring number is set, in metal phosphide
Nanometer sheet surface deposits to obtain platinum monatomic.
The present invention deposits to obtain the monoatomic mechanism of platinum on metal phosphide nanometer sheet surface: electricity under certain condition follows
Platinum electrode generates the monoatomic decomposition of platinum during ring, and the platinum separated is monatomic to deposit to metal phosphorus under the action of potential
In compound nanometer sheet, deposit to obtain platinum on metal phosphide nanometer sheet surface monatomic.Deposition platinum of the present invention is monoatomic
Method is not necessarily to complex device, easy to operate, low in cost.Importantly, the present invention utilizes three-electrode system electrochemical deposition
The monoatomic method of platinum can be monatomic in various metals phosphide nanometer sheet surface deposition platinum, to enhance the monoatomic catalysis of platinum
Performance.
Step A of the present invention specifically includes the following steps:
A1, hard calcium silicate nanowire white powder is configured to hard calcium silicate nanowire dispersion liquid, by metal chloride be added to
In hard calcium silicate nanowire dispersion liquid, then magnetic agitation carries out water-bath until solution went clear, room temperature is cooling, will obtain
The product obtained wash repeatedly, then carries out ethyl alcohol and wash repeatedly, dry in vacuum oven, and unformed metallic hydrogen is prepared
Oxide nano-slice powder；
A2, it is separately added into sodium dihydrogen phosphite and unformed metal hydroxides nanometer sheet powder at the place end to end of small porcelain boat,
It at the uniform velocity heats up under inert gas (such as argon gas) atmosphere, high-temperature calcination under conditions of temperature is 200-400 DEG C is prepared after cooling
Obtain metal phosphide nanometer sheet；
A3, suitable metal phosphide nanometer sheet is weighed, be dispersed in solvent, carried out ultrasonic disperse, dispersion is prepared
Liquid.
Preferably, the metallic element in the metal phosphide nanometer sheet is group VIII metal element, Group IVB metal member
One of element, VB race metallic element, group vib metallic element, VIIB race metallic element and Group IIB metal element etc. are a variety of.
The present invention can be deposited using the monoatomic method of three-electrode system electrochemical deposition on above-mentioned metal phosphide nanometer sheet surface
Platinum is monatomic, and the monatomic catalyst of platinum is successfully prepared.It is furthermore preferred that metallic element in the metal phosphide be iron,
One of cobalt, nickel, manganese, zinc, chromium, tin, lead, molybdenum etc. are a variety of.Using prepared by above-mentioned preferred metal phosphide nanometer sheet
The monatomic catalyst of obtained platinum has more excellent catalytic performance.
Metal phosphide nanometer sheet of the present invention has the characteristics that specific surface area is high, thus can provide more active sites
Point can utmostly improve the utilization rate of pt atom after load is monatomic, and then improve its catalytic activity.Gold of the present invention
Belong to the lamellar structure that phosphide nanometer sheet has two-dimensional ultrathin, while better stability and electricity can be kept to urge in acid condition
Change performance.Three-electrode system electrochemical deposition method of the invention is a used time longer preparation method, the metal phosphide
The stability of nanometer sheet facilitates going on smoothly for electrodeposition process, and the lamellar structure of two-dimensional ultrathin is also beneficial to the heavy of pt atom
Product.
Preferably, the solvent is the aqueous isopropanol containing naphthols.The present invention is added to suitable naphthols in isopropanol,
Suitable naphthols facilitates metal phosphide and is adhered to electrode surface, and the excessively high catalyst that will lead to of naphthol content is contacted with electrode
Resistance increases severely, and is unfavorable for the progress of electrochemical deposition process.Preferably, the volume ratio of the isopropanol and the naphthols is 10:1
~1000:1.Most preferably, the volume ratio of the isopropanol and the naphthols is 1000:7, in optimal proportion containing the different of naphthols
Propanol solution can significantly improve metal phosphide nanometer sheet in the adhesion amount of carbon paper surface, and then improve and utilize in subsequent step
Three-electrode system deposits the effect of pt atom catalyst in metal phosphide nanometer sheet.
Preferably, the concentration of the dispersion liquid is 1 ~ 5 mg/mL, and optimal is 2 mg/mL.The present invention controls dispersion liquid concentration
In appropriate range, it is ensured that metal phosphide nanometer sheet powder can be uniformly dispersed, convenient for catalyst in carbon paper surface
Dropwise addition.
Preferably, the ultrasonic disperse time is 10 ~ 100 min, and optimal is 60 min.The metal phosphide is described
Rapid dispersion in the ultrasonic disperse time obtains uniform, stable metal phosphide nanometer sheet solution.
In the step B, the carbon paper is 1 square centimeter of carbon paper, corresponding dispersion liquid be added dropwise volume be 50 ~
500 µL.The dropwise addition volume of metal phosphide nanometer sheet determines the load capacity of surface catalyst.The present invention passes through control metal
The dropwise addition volume of phosphide nanometer sheet, and then by load capacity control in suitable range, it can be when saving electrochemical deposition
Between while increase its catalytic performance to the maximum extent.
In the step C, electrolyte of the present invention can be neutral or acidic electrolysis bath.Preferably, the electrolysis
Liquid is acidic electrolysis bath, because the monoatomic transfer rate of platinum can be improved in deposition in acid condition, it is monatomic to facilitate platinum
Deposition efficiency in metal phosphide nanometer sheet.
Preferably, the pH of the acidic electrolysis bath is 1 ~ 3, and voltage is 0 ~ -1.3 V, and circulating ring number is 1000 ~ 15000 circles.
Acid pH, voltage and circulating ring number of the present invention guarantee the abundant progress of deposition process, avoid deposition process from carrying out insufficient
Caused by the monatomic catalyst of platinum catalytic performance reduce the problem of.
The present invention provides a kind of compound, is prepared using method as described above.The knot of compound of the present invention
Structure feature are as follows: the compound includes metal phosphide nanometer sheet and the platinum list for being grown on metal phosphide nanometer sheet surface
Atom.
The present invention also provides a kind of applications of compound, and the compound is applied to electro-catalysis water decomposition.Institute of the present invention
The compound of preparation has the characteristics that the utilization rate of catalytic activity height and pt atom is high, can be applied to electro-catalysis water decomposition.
Technical solution of the present invention is illustrated below by specific embodiment.
Embodiment 1
1、Co0.5Ni0.5PxThe synthesis of nanometer sheet
Hard calcium silicate nanowire white powder is configured to the hard calcium silicate nanowire dispersion liquid of 0.1 wt%, by the six of 3 mmol
Water cobalt chloride and six water nickel chlorides are added into the hard calcium silicate nanowire dispersion liquid of 50 mL, wherein cobalt ions and nickel ion
Total concentration is 0.06 mol/L, and 0.5 h of magnetic agitation is until solution went clear, the water-bath 3 under conditions of temperature is 80 DEG C
H, room temperature is cooling, and the product of acquisition is washed with water 3 times, and ethyl alcohol is washed 1 time, dry 6 in the vacuum oven that temperature is 60 DEG C
Co is prepared in h0.5Ni0.5(OH)2Nanometer sheet powder.
The sodium dihydrogen phosphite of 50 mg and the Co of 10 mg is added at the place end to end of small porcelain boat0.5Ni0.5(OH)2Nanometer sheet powder
End is warming up to 300 DEG C under an argon atmosphere with the heating rate of 5 DEG C/min, Co is obtained after high-temperature calcination0.5Ni0.5PxNanometer
Piece.
2, the monatomic deposition of platinum
Weigh the Co of 6 mg0.5Ni0.5PxNanometer sheet is dispersed in aqueous isopropanol (isopropanol and the naphthalene containing naphthols of 2 mL
The volume ratio of phenol is 1000:7) in, 1 h of ultrasonic disperse pipettes the dispersant liquid drop of 100 mL in 1 square centimeter of carbon with liquid-transfering gun
On paper, drying at room temperature is carried out；Preparing molar concentration is the sulfuric acid of 0.5 moL/L as electrolyte, to contain Co0.5Ni0.5PxIt receives
The carbon paper of rice piece is as working electrode, and as reference electrode, platinum electrode is used as to electrode saturated calomel electrode, and voltage range is arranged
For -0.2 ~ -1.0 V, it is 2500,5000,7500,10000 circles that circulating ring number, which is respectively set, and Pt-Co is prepared0.5Ni0.5Px
Compound.
It is the present embodiment deposition monoatomic flow diagram of platinum referring to Fig. 1, Fig. 1.The wherein structure of prepared compound
Feature: platinum is monatomic to be evenly distributed in super thin metal phosphide nanometer sheet, and the monoatomic super thin metal phosphide of Supported Pt Nanoparticles is received
Rice piece vertical-growth is on the surface of calcium silicate nanowire.
Referring to fig. 2, Fig. 2 is the Co prepared in the present embodiment0.5Ni0.5PxThe transmission plot of nanometer sheet.It can from Fig. 2
Out, Co prepared by the present embodiment0.5Ni0.5PxNanometer sheet has the nanometer chip architecture of two-dimensional ultrathin.
To Pt-Co prepared by the present embodiment of the present invention0.5Ni0.5PxCompound carries out OER electro-chemical test.
It is to 4 kinds of Pt-Co prepared by the present embodiment referring to Fig. 3, Fig. 30.5Ni0.5PxThe LSV of the OER of compound schemes.By
Figure it can be seen that with circulating ring number increase, OER chemical property is gradually increased, when circulating ring number is 2500 its
Chemical property is best, than circulating ring number to be promoted significantly when 0 circle, while it is also seen that being 5000 in circulating ring number
Its chemical property is essentially identical when circle, 7500 circle.Therefore, when circulating ring number is 2500 circle, the Pt-
Co0.5Ni0.5PxThe promotion of the OER chemical property of compound basically reaches best.
Embodiment 2
1、Co0.25Ni0.75PxThe synthesis of nanometer sheet
Hard calcium silicate nanowire white powder is configured to the hard calcium silicate nanowire dispersion liquid of 0.1 wt%, by the six of 3 mmol
Water cobalt chloride and six water nickel chlorides are added into the hard calcium silicate nanowire dispersion liquid of 50 mL, wherein cobalt ions and nickel ion
Total concentration is 0.06 mol/L, and 0.5 h of magnetic agitation is until solution went clear, the water-bath 3 under conditions of temperature is 80 DEG C
H, room temperature is cooling, and the product of acquisition is washed with water 3 times, and ethyl alcohol is washed 1 time, dry 6 in the vacuum oven that temperature is 60 DEG C
Co is prepared in h0.25Ni0.75(OH)2Nanometer sheet powder.
The sodium dihydrogen phosphite of 50 mg and the Co of 10 mg is added at the place end to end of small porcelain boat0.5Ni0.5(OH)2Nanometer sheet powder
End is warming up to 300 DEG C under an argon atmosphere with the heating rate of 5 DEG C/min, Co is obtained after high-temperature calcination0.25Ni0.75PxNanometer
Piece.
2, the monatomic deposition of platinum
Weigh the Co of 6mg0.25Ni0.75PxNanometer sheet is dispersed in aqueous isopropanol (isopropanol and the naphthols containing naphthols of 2mL
Volume ratio be 100:1) in, 1 h of ultrasonic disperse, pipetted respectively with liquid-transfering gun 25mL, 50mL, 75mL, 100mL, 200mL point
Dispersion liquid drop carries out drying at room temperature on 1 square centimeter of carbon paper；It prepares the sulfuric acid that molar concentration is 0.5moL/L and is used as electrolysis
Liquid, to contain Co0.25Ni0.75PxThe carbon paper of nanometer sheet is as working electrode, and saturated calomel electrode is as reference electrode, platinum electrode
As to electrode, setting voltage range is -0.2 ~ -1.0V, and setting circulating ring number is 2500, and Pt-Co is prepared0.25Ni0.75Px
Compound.
To Pt-Co prepared by the present embodiment0.25Ni0.75PxCompound carries out HER electro-chemical test.
Referring to fig. 4, Fig. 4 is respectively to 5 kinds of Pt-Co prepared by the present embodiment0.25Ni0.75PxThe HER's of compound test
LSV figure.As seen from the figure with the Co on carbon paper0.25Ni0.75PxThe increase of the load capacity of nanometer sheet, HER electro-chemical test
Performance gradually improves, but its test performance also starts to be deteriorated when load capacity reaches 200mL, illustrates that load capacity is excessively high to survey
Examination performance also can decrease.It can be learnt when load capacity is 100mL by figure, Pt-Co0.25Ni0.75PxCompound
HER electro-chemical test performance is best.
Embodiment 3
1、Co0.25Ni0.75PxThe synthesis of nanometer sheet
Hard calcium silicate nanowire white powder is configured to the hard calcium silicate nanowire dispersion liquid of 0.1 wt%, by the six of 3 mmol
Water cobalt chloride and six water nickel chlorides are added into the hard calcium silicate nanowire dispersion liquid of 50 mL, wherein cobalt ions and nickel ion
Total concentration is 0.06 mol/L, and 0.5 h of magnetic agitation is until solution went clear, the water-bath 3 under conditions of temperature is 80 DEG C
H, room temperature is cooling, and the product of acquisition is washed with water 3 times, and ethyl alcohol is washed 1 time, dry 6 in the vacuum oven that temperature is 60 DEG C
Co is prepared in h0.25Ni0.75(OH)2Nanometer sheet powder.
Locate that the sodium dihydrogen phosphite of 50 mg and the Co of 10 mg is added end to end in small porcelain boat0.5Ni0.5(OH)2Nanometer sheet powder
End is warming up to 300 DEG C under an argon atmosphere with the heating rate of 5 DEG C/min, Co is obtained after high-temperature calcination0.25Ni0.75PxNanometer
Piece.
2, the monatomic deposition of platinum
Weigh the Co of 6mg0.25Ni0.75PxNanometer sheet is dispersed in aqueous isopropanol (isopropanol and the naphthols containing naphthols of 2mL
Volume ratio be 100:1) in, ultrasonic disperse 1h pipettes the dispersant liquid drop of 100mL on 1 square centimeter of carbon paper with liquid-transfering gun,
Carry out drying at room temperature；Preparing molar concentration is the sulfuric acid of 0.5moL/L as electrolyte, to contain Co0.25Ni0.75PxNanometer sheet
Carbon paper is as working electrode, and as reference electrode, platinum electrode is used as to electrode saturated calomel electrode, and it is -0.2 that voltage range, which is arranged,
~ -1.0V, it is 2500,5000,7500,10000 that circulating ring number, which is respectively set, and Pt-Co is prepared0.25Ni0.75PxCompound.
To Pt-Co prepared by the embodiment of the present invention 30.25Ni0.75PxCompound carries out HER electro-chemical test.
It is 4 kinds of Pt-Co prepared by the present embodiment referring to Fig. 5, Fig. 50.25Ni0.75PxThe LSV of the HER of compound schemes.By scheming
It can be seen that HER performance is gradually increased with the increase of circulating ring number, its electrochemistry when circulating ring number is 7500
Can preferably, promotion is significant when circle than circulating ring number for 0,2500,5000, while it is also seen that being 7500 in circulating ring number
After circle, HER electro-chemical test degradation illustrates the activity of its monatomic deposition when circulating ring number is 7500 circle
Maximum, and the deposition of excessive pt atom can reduce its catalytic activity instead, this is identical as the rule of monatomic catalytic activity, from
It is a monoatomic deposition that side, which demonstrates deposition process,.
Embodiment 4
1、CoyPxThe synthesis of nanometer sheet
Hard calcium silicate nanowire white powder is configured to the hard calcium silicate nanowire dispersion liquid of 0.1 wt%, by the six of 3 mmol
Water cobalt chloride is added into the hard calcium silicate nanowire dispersion liquid of 50 mL, and wherein the concentration of cobalt ions is 0.06 mol/L, magnetic force
0.5 h is stirred until solution went clear, 3 h of water-bath under conditions of temperature is 80 DEG C, room temperature is cooling, by the production of acquisition
Object is washed with water 3 times, and ethyl alcohol is washed 1 time, and dry 6 h, are prepared Co(OH in the vacuum oven that temperature is 60 DEG C)2Nanometer
Piece powder.
Locate that the sodium dihydrogen phosphite of 50 mg and the Co(OH of 10 mg is added end to end in small porcelain boat)2Nanometer sheet powder, in argon
300 DEG C are warming up to the heating rate of 5 DEG C/min under gas atmosphere, Co is obtained after high-temperature calcinationyPxNanometer sheet.
2, the monatomic deposition of platinum
Weigh the Co of 6mgyPxNanometer sheet, being dispersed in the aqueous isopropanol containing naphthols of 2mL, (volume ratio of isopropanol and naphthols is
In 100:1), it is dry to carry out room temperature on 1 square centimeter of carbon paper for ultrasonic disperse 1h, the dispersant liquid drop for pipetting 100mL with liquid-transfering gun
It is dry；Preparing molar concentration is the sulfuric acid of 0.5moL/L as electrolyte, to contain CoyPxThe carbon paper of nanometer sheet as working electrode,
Saturated calomel electrode is as reference electrode, and platinum electrode is used as to electrode, and setting voltage range is -0.2 ~ -1.0V, and circulating ring is arranged
Number is 7500, and Pt-Co is preparedyPxCompound.
Pt-Co prepared by the embodiment of the present invention 4yPxCompound carries out HER electro-chemical test.
Referring to Fig. 6, Fig. 6 is Pt-Co manufactured in the present embodimentyPxThe LSV of the HER of compound schemes.It is following as seen from the figure
After ring 7500 encloses, HER chemical property is significantly increased, and illustrates that monatomic deposition is very aobvious to the promotion of electrocatalysis characteristic
It writes, while also it can be concluded that preparation method of the present invention can be applied to the metal composite of different proportion.
In conclusion the present invention, which provides one kind, deposits the monoatomic method of platinum on metal phosphide nanometer sheet surface, pass through
Use the carbon paper of carried metal phosphide nanometer sheet for working electrode, saturated calomel electrode is reference electrode, and platinum electrode is to electricity
Certain voltage and circulating ring number is arranged in pole in the electrolytic solution, and then deposition platinum is monatomic on metal phosphide nanometer sheet.
The method of the invention is not necessarily to complex device, easy to operate, applied widely, is suitable for various metals phosphide material, and
The catalytic performance of preparation-obtained compound is promoted significantly, while also providing a kind of new think of to study monatomic catalysis
Road.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of deposit the monoatomic method of platinum on metal phosphide nanometer sheet surface, which comprises the following steps:
In a solvent by the dispersion of metal phosphide nanometer sheet, dispersion liquid is prepared；
By the dispersant liquid drop on carbon paper, it is used as working electrode after dry, using saturated calomel electrode as reference electrode, platinum electricity
Pole is used as to electrode；
Electrolyte is prepared, electrolytic cell has been set up, certain voltage and certain circulating ring number is set, in metal phosphide nanometer sheet
Surface deposits to obtain platinum monatomic.
2. according to claim 1 deposit the monoatomic method of platinum on metal phosphide nanometer sheet surface, which is characterized in that
Metallic element in the metal phosphide nanometer sheet be group VIII metal element, Group IVB metallic element, VB race metallic element,
One of group vib metallic element, VIIB race metallic element and Group IIB metal element are a variety of.
3. according to claim 2 deposit the monoatomic method of platinum on metal phosphide nanometer sheet surface, which is characterized in that
Metallic element in the metal phosphide nanometer sheet is one of iron, cobalt, nickel, manganese, zinc, chromium, tin, lead, molybdenum or a variety of.
4. according to claim 1 deposit the monoatomic method of platinum on metal phosphide nanometer sheet surface, which is characterized in that
The solvent is the aqueous isopropanol containing naphthols.
5. according to claim 4 deposit the monoatomic method of platinum on metal phosphide nanometer sheet surface, which is characterized in that
The volume ratio of the isopropanol and the naphthols is 10:1 ~ 1000:1.
6. according to claim 1 deposit the monoatomic method of platinum on metal phosphide nanometer sheet surface, which is characterized in that
The mass concentration of the dispersion liquid is 1 ~ 5 mg/mL.
7. according to claim 1 deposit the monoatomic method of platinum on metal phosphide nanometer sheet surface, which is characterized in that
The carbon paper that the carbon paper is 1 square centimeter；The volume that the dispersion liquid is added dropwise on the carbon paper is 50 ~ 500 μ L.
8. according to claim 1 deposit the monoatomic method of platinum on metal phosphide nanometer sheet surface, which is characterized in that
The electrolyte is the acidic electrolysis bath that pH is 1 ~ 3, and voltage is 0 ~ -1.3 V, and circulating ring number is 1000 ~ 15000 circles.
9. a kind of compound, which is characterized in that be prepared using method a method as claimed in any one of claims 1-8；It is described compound
Object include metal phosphide nanometer sheet and be grown on metal phosphide nanometer sheet surface platinum it is monatomic.
10. a kind of application of compound as claimed in claim 9, which is characterized in that the compound is applied to electro-catalysis water
It decomposes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810795400.4A CN109100402B (en) | 2018-07-19 | 2018-07-19 | Method for depositing platinum monoatomic compound and application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810795400.4A CN109100402B (en) | 2018-07-19 | 2018-07-19 | Method for depositing platinum monoatomic compound and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109100402A true CN109100402A (en) | 2018-12-28 |
| CN109100402B CN109100402B (en) | 2020-10-27 |
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Cited By (6)
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| CN111197173A (en) * | 2020-02-07 | 2020-05-26 | 复旦大学 | Electroplating preparation method of non-noble metal single-atom-doped two-dimensional material |
| CN112023922A (en) * | 2020-09-27 | 2020-12-04 | 广州大学 | Pt-MnO2Material, preparation method and application thereof |
| CN112774697A (en) * | 2020-09-07 | 2021-05-11 | 南京大学 | Monoatomic metal-molybdenum sulfide nano-composite and preparation method and application thereof |
| CN113249739A (en) * | 2021-06-04 | 2021-08-13 | 中国科学技术大学 | Metal phosphide-loaded monatomic catalyst, preparation method thereof and application of metal phosphide-loaded monatomic catalyst as hydrogen evolution reaction electrocatalyst |
| CN114318403A (en) * | 2021-12-31 | 2022-04-12 | 上海大学 | Method for preparing platinum monoatomic material by adopting alkyl imidazole ionic liquid |
| CN114807996A (en) * | 2022-04-13 | 2022-07-29 | 北京工业大学 | Preparation method of monatomic platinum-loaded transition metal phosphide hydrogen evolution catalyst |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111197173A (en) * | 2020-02-07 | 2020-05-26 | 复旦大学 | Electroplating preparation method of non-noble metal single-atom-doped two-dimensional material |
| CN112774697A (en) * | 2020-09-07 | 2021-05-11 | 南京大学 | Monoatomic metal-molybdenum sulfide nano-composite and preparation method and application thereof |
| CN112023922A (en) * | 2020-09-27 | 2020-12-04 | 广州大学 | Pt-MnO2Material, preparation method and application thereof |
| CN113249739A (en) * | 2021-06-04 | 2021-08-13 | 中国科学技术大学 | Metal phosphide-loaded monatomic catalyst, preparation method thereof and application of metal phosphide-loaded monatomic catalyst as hydrogen evolution reaction electrocatalyst |
| CN113249739B (en) * | 2021-06-04 | 2022-07-15 | 中国科学技术大学 | Metal phosphide-loaded monatomic catalyst, preparation method thereof and application of metal phosphide-loaded monatomic catalyst as hydrogen evolution reaction electrocatalyst |
| CN114318403A (en) * | 2021-12-31 | 2022-04-12 | 上海大学 | Method for preparing platinum monoatomic material by adopting alkyl imidazole ionic liquid |
| CN114318403B (en) * | 2021-12-31 | 2023-08-25 | 上海大学 | Method for preparing platinum monoatomic material by adopting alkyl imidazole ionic liquid |
| CN114807996A (en) * | 2022-04-13 | 2022-07-29 | 北京工业大学 | Preparation method of monatomic platinum-loaded transition metal phosphide hydrogen evolution catalyst |
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