CN113582165A - Preparation method of phosphorus atom doped graphene nanocomposite - Google Patents
Preparation method of phosphorus atom doped graphene nanocomposite Download PDFInfo
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- CN113582165A CN113582165A CN202110824518.7A CN202110824518A CN113582165A CN 113582165 A CN113582165 A CN 113582165A CN 202110824518 A CN202110824518 A CN 202110824518A CN 113582165 A CN113582165 A CN 113582165A
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- C01B32/15—Nano-sized carbon materials
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Abstract
The invention discloses a preparation method of a phosphorus atom doped graphene nanocomposite, which is characterized by utilizing diammonium hydrogen phosphate as a phosphorus precursor, taking graphene oxide and diammonium hydrogen phosphate as reactants, reducing the graphene oxide at a lower temperature and introducing phosphorus atoms, and preparing the phosphorus atom doped graphene nanocomposite by regulating and controlling the proportion of the diammonium hydrogen phosphate and the graphene, the reaction temperature and other conditions. The method has the characteristics of simple preparation method and low reaction temperature, and the phosphorus-doped graphene nanocomposite prepared by the method enhances the electrical conductivity and improves the catalytic performance, can be used as a novel carrier of a fuel cell catalyst, and is used for proton exchange membrane fuel cells, methanol fuel cells and the like.
Description
Technical Field
The invention relates to a preparation technology of a nano material, in particular to a preparation method of a phosphorus atom doped graphene nano composite material.
Background
A fuel cell is a power generation device that directly and continuously converts chemical energy present in a chemical fuel and an oxidant into electrical energy. The fuel cell has great application prospect in the industries of automobiles and the like in the future because of energy conservation and environmental protection. Electrode catalysts are of critical importance for fuel cells, and the catalytic efficiency of the catalyst determines the reaction rate of the electrode and hence the efficiency of the fuel cell. However, catalysts often affect the life of fuel cells due to reduced stability.
The presence of Pt in the catalyst accelerates the corrosion of the carbon support in the fuel cell catalyst. Among carbon supports, graphene is a very popular material. Graphene, however, has a higher tendency to pack, resulting in lower porosity and lower reactivity, which hinders the attachment of nanoparticles. One solution to this problem is to dope atoms such as nitrogen and sulfur on graphene and introduce a heteroatom defect to improve the graphene structure, increase the interlayer distance, and improve the electrical conductivity.
The nitrogen-doped carbon material has already been researched and applied a lot, and the phosphorus element of the same main group has good application prospect. Compared with N atoms, P atoms have larger atomic radius, the formed C-P bond length is also obviously longer than that of C-N bonds, and the doping of the P atoms can bring larger structural deformation to the carbon material structure. And because N has a greater electronegativity than C, P has a lesser electronegativity than C, and therefore the polarity of the C-P bond is opposite to that of the C-N bond, which means that phosphorus-doped graphene can generate more defect sites and active sites.
Disclosure of Invention
The invention aims to provide a preparation method of a phosphorus atom doped graphene nanocomposite.
The invention aims to provide the following scheme for realization: a preparation method of a phosphorus atom doped graphene nanocomposite uses diammonium hydrogen phosphate as a phosphorus source precursor to reduce graphene oxide at a lower temperature and introduce phosphorus atoms, and comprises the following steps:
(1) the phosphorus source is diammonium hydrogen phosphate, 150mg of graphene oxide and 450-600 mg of diammonium hydrogen phosphate are weighed and placed in a beaker;
(2) adding 40ml of deionized water into a beaker, stirring for 0.5 hour, and freeze-drying at-80 ℃;
(3) putting the mixture obtained after freeze-drying into a quartz boat, heating to 450-700 ℃ at a heating rate of 5 ℃/min in a tube furnace under the protection of hydrogen-argon mixed gas, and then preserving heat for 3 hours;
(4) cooling the quartz boat to room temperature in the furnace, taking out the mixture in the quartz boat, and washing the black solid after reaction by using excessive ethanol and deionized water;
(5) and drying the washed sample in a vacuum drying oven for 24 hours to obtain the required phosphorus atom doped graphene nanocomposite.
Wherein, in the step (1), the phosphorus source can also be at least one of triphenylphosphine or phosphoric acid, and when the phosphorus source is triphenylphosphine, the freeze drying operation in the step (2) is changed to grinding until the mixture is uniform.
In the step (4), the black solid is obtained after washing reaction by using excessive ethanol and deionized water, and the washing process needs centrifugal operation, wherein the centrifugal speed is 10000 r/min, and the duration time is about 3 min.
According to the method, graphene oxide and diammonium hydrogen phosphate are used as reactants, the graphene oxide is reduced at a lower temperature, and phosphorus atoms are introduced. The nano composite material prepared by the method enhances the conductivity and improves the catalytic performance. So that the nano material has wider prospect in the field of practical application. The phosphorus-doped graphene nano material prepared by the invention can be used as a novel carrier of a fuel cell catalyst and is used for proton exchange membrane fuel cells, methanol fuel cells and the like.
Drawings
Fig. 1 is an SEM image of a phosphorus atom doped graphene nanocomposite according to the present invention;
fig. 2 is a raman spectrum of the phosphorus atom-doped graphene nanocomposite material of the present invention.
Detailed Description
Example 1:
a phosphorus atom doped graphene nanocomposite is prepared by using diammonium phosphate as a phosphorus source as a precursor, reducing graphene oxide at a lower temperature and introducing phosphorus atoms, and comprises the following steps:
(1) weighing 150mg of graphene oxide and 450mg of diammonium hydrogen phosphate, and placing the graphene oxide and the diammonium hydrogen phosphate in a beaker;
(2) adding 40ml of deionized water into a beaker, stirring for 0.5 hour, and freeze-drying at-80 ℃;
(3) putting the mixture obtained after freeze-drying into a quartz boat, heating to 450 ℃ at a heating rate of 5 ℃/min in a tube furnace under the protection of hydrogen-argon mixed gas, and then preserving heat for 3 hours;
(4) cooling the quartz boat to room temperature in the furnace, taking out the mixture in the quartz boat, and washing the black solid after reaction by using excessive ethanol and deionized water;
(5) and drying the washed sample in a vacuum drying oven for 24 hours to obtain the required phosphorus atom doped graphene nanocomposite.
Fig. 1 is an SEM image of a phosphorus atom-doped graphene nanocomposite material of the present invention. As can be seen from the figure, the phosphorus-doped graphene nanocomposite consists of nanosheets, the proportion of the precursor is adjusted, and the nanomaterial is slightly different in morphology but still consists of the nanosheets.
Fig. 2 is a raman spectrum of the phosphorus atom-doped graphene nanocomposite material of the present invention. In general, in Raman spectra
The number of structural defects and the degree of disorder of the carbon material can be estimated, and the PG can be seen from the figure
Values higher than GO
The values indicate that there are a large number of structural defects in the phosphorus-doped graphene material, which means that the phosphorus-doped graphene has more active sites for loading Pt atoms.
Example 2:
a phosphorus atom doped graphene nanocomposite material is prepared by the following steps, similar to the steps of example 1:
(1) weighing 150mg of graphene oxide and 450mg of diammonium hydrogen phosphate, and placing the graphene oxide and the diammonium hydrogen phosphate in a beaker;
(2) adding 40ml of deionized water into a beaker, stirring for 0.5 hour, and freeze-drying at-80 ℃;
(3) putting the mixture obtained after freeze-drying into a quartz boat, heating to 700 ℃ at a heating rate of 5 ℃/min in a tube furnace under the protection of hydrogen-argon mixed gas, and then preserving heat for 3 hours;
(4) cooling the quartz boat to room temperature in the furnace, taking out the mixture in the quartz boat, and washing the black solid after reaction by using excessive ethanol and deionized water;
(5) and drying the washed sample in a vacuum drying oven for 24 hours to obtain the required phosphorus atom doped graphene nanocomposite.
Example 3:
a phosphorus atom doped graphene nanocomposite material is prepared by the following steps, similar to the steps of example 1:
(1) weighing 150mg of graphene oxide and 600mg of diammonium hydrogen phosphate, and placing the graphene oxide and the diammonium hydrogen phosphate in a beaker;
(2) adding 40ml of deionized water into a beaker, stirring for 0.5 hour, and freeze-drying at-80 ℃;
(3) putting the mixture obtained after freeze-drying into a quartz boat, heating to 450 ℃ at a heating rate of 5 ℃/min in a tube furnace under the protection of hydrogen-argon mixed gas, and then preserving heat for 3 hours;
(4) cooling the quartz boat to room temperature in the furnace, taking out the mixture in the quartz boat, and washing the black solid after reaction by using excessive ethanol and deionized water;
(5) and drying the washed sample in a vacuum drying oven for 24 hours to obtain the required phosphorus atom doped graphene nanocomposite.
Example 4:
a phosphorus atom doped graphene nanocomposite material is prepared by the following steps, similar to the steps of example 1:
(1) weighing 150mg of graphene oxide and 600mg of diammonium hydrogen phosphate, and placing the graphene oxide and the diammonium hydrogen phosphate in a beaker;
(2) adding 40ml of deionized water into a beaker, stirring for 0.5 hour, and freeze-drying at-80 ℃;
(3) putting the mixture obtained after freeze-drying into a quartz boat, heating to 700 ℃ at a heating rate of 5 ℃/min in a tube furnace under the protection of hydrogen-argon mixed gas, and then preserving heat for 3 hours;
(4) cooling the quartz boat to room temperature in the furnace, taking out the mixture in the quartz boat, and washing the black solid after reaction by using excessive ethanol and deionized water;
(5) and drying the washed sample in a vacuum drying oven for 24 hours to obtain the required phosphorus atom doped graphene nanocomposite.
Claims (7)
1. A preparation method of a phosphorus atom doped graphene nanocomposite is characterized in that diammonium hydrogen phosphate is used as a phosphorus source precursor, graphene oxide is reduced at a lower temperature, and phosphorus atoms are introduced, and the preparation method comprises the following steps:
(1) the phosphorus source is diammonium hydrogen phosphate, 150mg of graphene oxide and 450-600 mg of diammonium hydrogen phosphate are weighed and placed in a beaker;
(2) adding 40ml of deionized water into a beaker, stirring for 0.5 hour, and freeze-drying at-80 ℃;
(3) putting the mixture obtained after freeze-drying into a quartz boat, heating to 450-700 ℃ at a heating rate of 5 ℃/min in a tube furnace under the protection of hydrogen-argon mixed gas, and then preserving heat for 3 hours;
(4) cooling the quartz boat to room temperature in the furnace, taking out the mixture in the quartz boat, and washing the black solid after reaction by using excessive ethanol and deionized water;
(5) and drying the washed sample in a vacuum drying oven for 24 hours to obtain the required phosphorus atom doped graphene nanocomposite.
2. The method for preparing the phosphorus atom doped graphene nanocomposite material according to claim 1, wherein the method comprises the following steps: in the step (1), the phosphorus source is at least one of triphenylphosphine and phosphoric acid, and when the phosphorus source is triphenylphosphine, the freeze drying operation in the step (2) is changed to grinding until the mixture is uniformly mixed.
3. The method for preparing the phosphorus atom doped graphene nanocomposite material according to claim 1, wherein the method comprises the following steps: and (4) washing and reacting with excessive ethanol and deionized water to obtain a black solid, wherein the washing process needs centrifugal operation, the centrifugal speed is 10000 r/min, and the duration is about 3 min.
4. The method for preparing the phosphorus atom-doped graphene nanocomposite material according to any one of claims 1 to 3, wherein: the preparation method comprises the following steps:
(1) weighing 150mg of graphene oxide and 450mg of diammonium hydrogen phosphate, and placing the graphene oxide and the diammonium hydrogen phosphate in a beaker;
(2) adding 40ml of deionized water into a beaker, stirring for 0.5 hour, and freeze-drying at-80 ℃;
(3) putting the mixture obtained after freeze-drying into a quartz boat, heating to 450 ℃ at a heating rate of 5 ℃/min in a tube furnace under the protection of hydrogen-argon mixed gas, and then preserving heat for 3 hours;
(4) cooling the quartz boat to room temperature in the furnace, taking out the mixture in the quartz boat, and washing the black solid after reaction by using excessive ethanol and deionized water;
(5) and drying the washed sample in a vacuum drying oven for 24 hours to obtain the required phosphorus atom doped graphene nanocomposite.
5. The method for preparing the phosphorus atom-doped graphene nanocomposite material according to any one of claims 1 to 3, wherein: (1) weighing 150mg of graphene oxide and 450mg of diammonium hydrogen phosphate, and placing the graphene oxide and the diammonium hydrogen phosphate in a beaker;
(2) adding 40ml of deionized water into a beaker, stirring for 0.5 hour, and freeze-drying at-80 ℃;
(3) putting the mixture obtained after freeze-drying into a quartz boat, heating to 700 ℃ at a heating rate of 5 ℃/min in a tube furnace under the protection of hydrogen-argon mixed gas, and then preserving heat for 3 hours;
(4) cooling the quartz boat to room temperature in the furnace, taking out the mixture in the quartz boat, and washing the black solid after reaction by using excessive ethanol and deionized water;
(5) and drying the washed sample in a vacuum drying oven for 24 hours to obtain the required phosphorus atom doped graphene nanocomposite.
6. The method for preparing the phosphorus atom-doped graphene nanocomposite material according to any one of claims 1 to 3, wherein: (1) weighing 150mg of graphene oxide and 600mg of diammonium hydrogen phosphate, and placing the graphene oxide and the diammonium hydrogen phosphate in a beaker;
(2) adding 40ml of deionized water into a beaker, stirring for 0.5 hour, and freeze-drying at-80 ℃;
(3) putting the mixture obtained after freeze-drying into a quartz boat, heating to 450 ℃ at a heating rate of 5 ℃/min in a tube furnace under the protection of hydrogen-argon mixed gas, and then preserving heat for 3 hours;
(4) cooling the quartz boat to room temperature in the furnace, taking out the mixture in the quartz boat, and washing the black solid after reaction by using excessive ethanol and deionized water;
(5) and drying the washed sample in a vacuum drying oven for 24 hours to obtain the required phosphorus atom doped graphene nanocomposite.
7. The method for preparing the phosphorus atom-doped graphene nanocomposite material according to any one of claims 1 to 3, wherein: (1) weighing 150mg of graphene oxide and 600mg of diammonium hydrogen phosphate, and placing the graphene oxide and the diammonium hydrogen phosphate in a beaker;
(2) adding 40ml of deionized water into a beaker, stirring for 0.5 hour, and freeze-drying at-80 ℃;
(3) putting the mixture obtained after freeze-drying into a quartz boat, heating to 700 ℃ at a heating rate of 5 ℃/min in a tube furnace under the protection of hydrogen-argon mixed gas, and then preserving heat for 3 hours;
(4) cooling the quartz boat to room temperature in the furnace, taking out the mixture in the quartz boat, and washing the black solid after reaction by using excessive ethanol and deionized water;
(5) and drying the washed sample in a vacuum drying oven for 24 hours to obtain the required phosphorus atom doped graphene nanocomposite.
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2021
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| CN103495430A (en) * | 2013-10-16 | 2014-01-08 | 西华师范大学 | Phosphorus-doped graphene oxygen reduction electro-catalyst and preparation method and application thereof |
| WO2015194142A1 (en) * | 2014-06-20 | 2015-12-23 | パナソニック株式会社 | Carbon-based material, electrode catalyst, electrode, electrochemical device, fuel cell, and method for manufacturing carbon-based material |
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