CN105696014A - Nitrogen doped graphene N-rGO and nano lamella cluster MoSe2 composite structure and preparation method - Google Patents
Nitrogen doped graphene N-rGO and nano lamella cluster MoSe2 composite structure and preparation method Download PDFInfo
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- CN105696014A CN105696014A CN201610149983.4A CN201610149983A CN105696014A CN 105696014 A CN105696014 A CN 105696014A CN 201610149983 A CN201610149983 A CN 201610149983A CN 105696014 A CN105696014 A CN 105696014A
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Abstract
The invention discloses a preparation method of a nitrogen doped graphene N-rGO and nano lamella cluster MoSe2 composite structure. The preparation method is used for improving the efficiency for generating hydrogen through photoelectric chemical water decomposition. By the adoption of two steps of hydrothermal reaction synthesis, the heterogeneous composite structure with MoSe2 nano lamella clusters and N-rGO lamellas being mutually wound and with the diameter being about 100 nm is formed through annealing treatment, the MoSe2/N-rGO composite structure has the visible light absorption characteristic superior to that of an independent MoSe2 structure, a heterogeneous interface formed by the MoSe2 and N-rGO can effectively restrain compounding of photo-induced electrons and holes and enhance separation of the electrons from the holes, and the photo-induced electrons are rapidly captured by H+ in electrolyte under the effect of an external electric field to generate hydrogen. The technical idea is simple and clear, and the composite structure can remarkably enhance the efficiency for generating hydrogen through photoelectric chemical water decomposition. The technical idea for preparing the N-rGO and MoSe2 heterogeneous structure through the two-step hydrothermal method and enhancing the efficiency for generating hydrogen through photoelectric chemical water decomposition is disclosed.
Description
[technical field]
The invention belongs to Photoelectrochemistry of semiconductor hydrogen production by water decomposition field, relate to a kind of nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction and preparation method。
[background technology]
Industrialized quickly propel the demand to the energy and grow with each passing day, using oil, coal Fossil fuel as conventional energy resource, by approach exhaustion, and a large amount of use of Fossil fuel causes that the problem of environmental pollutions such as haze are day by day serious。Therefore, exploitation cleaning green energy resource capable of circulation has very important significance。Hydrogen Energy has cleaning, high-energy-density, can store, the advantage such as be readily transported, utilize inexhaustible solar energy that water resource the abundantest on the earth is resolved into reproducible secondary energy sources-hydrogen, the oxidized afterproduct that releases energy of hydrogen is water, environment is not had any harm by whole process, and capable of circulation, there is huge potential application foreground。
Quasiconductor has the advantages that to absorb photon generation light induced electron and hole, by hydrion, light induced electron active for its conduction band can be captured generation hydrogen by the method for Optical Electro-Chemistry decomposition water, uses as Hydrogen Energy。As the quasiconductor of Optical Electro-Chemistry decomposition water liberation of hydrogen, the productivity of the separation efficiency appreciable impact hydrogen in its optical absorption characteristics and himself internal light induced electron and hole。
Since 2004 find Graphene, start people's research boom to two-dimensional material。Two selenizing molybdenum (MoSe2) as the Typical Representative of magnesium-yttrium-transition metal disulphide, there is the stratiform sandwich structure of uniqueness, interlayer is combined by Van der Waals for, is similar to Graphene, MoSe2Ultra-thin two-dimensional structure can be grown into, band gap with the number of plies between 1.1～1.9eV variable, it may be achieved in absorption to visible ray in a big way, there is good optical absorption characteristics, and two dimension MoSe2There is the features such as specific surface area is big, edge dangling bonds are abundant, provide possibility for realizing efficient photoelectricity treater chemolysis water hydrogen manufacturing。
But single MoSe2The recombination rate in internal light induced electron and hole is very fast, the utilization rate of light induced electron is relatively low, it can be carried out compound with two-dimensional material N-rGO, by strong heterogeneous interface effect, light induced electron and hole are effectively separated, and this special two-dimensional material heterogeneous interface can improve the absorption of visible ray further by coupling, it is possible to promote the performance of Optical Electro-Chemistry hydrogen production by water decomposition further。
[summary of the invention]
It is an object of the invention to the shortcoming overcoming above-mentioned prior art, it is provided that a kind of nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction and preparation method, the method is to prepare nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe by two one-step hydrothermals2Composite construction, defines a kind of nanoscale twins cluster MoSe2With the heterojunction structure of nitrogen-doped graphene N-rGO compact winding, the heterojunction structure of two kinds of two-dimensional material formation can be effectively improved visible light absorption, it is suppressed that the compound in light induced electron and hole, significantly improves the performance of Optical Electro-Chemistry hydrogen production by water decomposition。
In order to achieve the above object, the present invention is achieved by the following technical solutions:
A kind of nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The preparation method of composite construction, comprises the following steps:
1) graphene oxide of 10～30mg, the hydrazine hydrate of 0.5～5mL, concentration are the ammonia of 30% and the deionized water of 30mL is sufficiently mixed, obtain homodisperse mixed solution A；Wherein, ammonia is 1:(5～50 with the volume ratio of hydrazine hydrate)；
2) with autoclave for holding vessel, mixed solution A, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO；
3) selenium powder of 0.1～0.3g is dissolved in the hydrazine hydrate of 1～10mL, stands 20～40h, obtain selenium powder hydrazine hydrate solution；Again nitrogen-doped graphene N-rGO, the selenium powder hydrazine hydrate solution of 1～10mL and the two molybdic acid hydrate sodium of 0.1～0.5g are joined in 30mL deionized water, be sufficiently mixed and obtain homodisperse mixed solution B；Wherein, the addition of nitrogen-doped graphene N-rGO is the 1%～5% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；
5) mixture it is carried out and dries, obtaining MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is annealed processing, and improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state。
The present invention is further improved by:
Described step 1) in, it is sufficiently mixed by stirring and ultrasonic Treatment。
Described step 2) and step 4) in, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL。
Described step 2) in, mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then take out product, dried for standby after furnace cooling or water-cooled。
Described step 3) in, mixed solution B obtains homodisperse suspension by stirring and ultrasonic Treatment。
Described step 4) in, the reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 10～20h, furnace cooling or after water-cooled take out product。
Described step 5) in, cleaning treatment is for be first carried out mixture with acetone, then 10min is processed with the centrifugation of 8000r/min, it is carried out followed by dehydrated alcohol, centrifugal treating 10min under the speed of 8000r/min again, finally it is carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
Described step 5) in, cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, stand-by。
Described step 6) in, at H2+N2Being annealed under atmosphere processing, annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
A kind of nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction, the MoSe of preparation2In/N-rGO composite construction, MoSe2In nanoscale twins cluster, cluster diameter is about 100～170nm, MoSe2Cluster and N-rGO lamella are wound heterojunction structure mutually。
Compared with prior art, the method have the advantages that
N-rGO/MoSe prepared by the present invention2MoSe in composite2Nanoscale twins cluster is dispersed on N-rGO lamella, and interface cohesion is good。When illumination, MoSe2Producing light induced electron and hole owing to absorbing photon, light induced electron and hole can be effectively separated by its heterogeneous interface with N-rGO, and under the effect of extra electric field, light induced electron can quickly by the H in electrolyte+Capture generation hydrogen, improve the efficiency of Optical Electro-Chemistry decomposition water liberation of hydrogen。The present invention is with two molybdic acid hydrate sodium for molybdenum source, with selenium powder for selenium source, additionally adds N-rGO, forms MoSe by hydro-thermal2The heterojunction structure that nanoscale twins cluster and N-rGO lamella are combined closely, improves the crystallization degree of composite construction by follow-up annealing。
[accompanying drawing explanation]
Fig. 1 is MoSe2The SEM photograph of/N-rGO-2 composite construction；
Fig. 2 is MoSe2The TEM photo of/N-rGO-2 composite construction；
Fig. 3 is MoSe2/ N-rGO-2 composite construction and MoSe2Absorbing properties；
Fig. 4 is MoSe2/ N-rGO-2 composite construction and MoSe2PL spectrogram；
Fig. 5 is MoSe2/ N-rGO-2 composite construction and MoSe2Respectively at dark and under illumination condition LSV curve。
[detailed description of the invention]
Below in conjunction with specific embodiment, the present invention is described in further detail:
The present invention utilizes two one-step hydrothermals to prepare N-rGO and MoSe2Nanoscale twins cluster composite construction, at H2+N2To N-rGO/MoSe under atmosphere2Composite construction powder is annealed processing and promotes its degree of crystallinity further；Adjust nitrogen content and the addition of N-rGO in course of reaction, it is possible to achieve the regulation and control to composite construction。
Embodiment 1
1) it is the ammonia of 30% and the deionized water of 30mL by stirring and ultrasonic Treatment is sufficiently mixed by the graphene oxide of 30mg, the hydrazine hydrate of 5mL, concentration, obtains homodisperse mixed solution A；Wherein, ammonia is 1:50 with the volume ratio of hydrazine hydrate；
2) mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then take out product, dried for standby after furnace cooling or water-cooled, prepare nitrogen-doped graphene N-rGO；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；
3) selenium powder of 0.3g is dissolved in the hydrazine hydrate of 10mL, stands 40h, obtain selenium powder hydrazine hydrate solution；Again the two molybdic acid hydrate sodium of the selenium powder hydrazine hydrate solution of nitrogen-doped graphene N-rGO, 10mL and 0.5g are joined in 30mL deionized water, obtain homodisperse mixed solution B by stirring and ultrasonic Treatment；Wherein, the addition of nitrogen-doped graphene N-rGO is the 1% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；The reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 10h, furnace cooling or after water-cooled take out product。
5) first with acetone, mixture is carried out, then 10min is processed with the centrifugation of 8000r/min, it is carried out followed by dehydrated alcohol, centrifugal treating 10min under the speed of 8000r/min again, finally it is carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
Cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, obtains MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is at H2+N2It is annealed under atmosphere processing, improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state；Annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
MoSe prepared by the present embodiment2In/N-rGO composite construction, MoSe2In nanoscale twins cluster, cluster diameter is about 100nm, is mutually wound around with N-rGO lamella。
Embodiment 2
1) it is the ammonia of 30% and the deionized water of 30mL by stirring and ultrasonic Treatment is sufficiently mixed by the graphene oxide of 25mg, the hydrazine hydrate of 4mL, concentration, obtains homodisperse mixed solution A；Wherein, ammonia is 1:50 with the volume ratio of hydrazine hydrate；
2) mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then take out product, dried for standby after furnace cooling or water-cooled, prepare nitrogen-doped graphene N-rGO；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；
3) selenium powder of 0.3g is dissolved in the hydrazine hydrate of 9mL, stands 40h, obtain selenium powder hydrazine hydrate solution；Again the two molybdic acid hydrate sodium of the selenium powder hydrazine hydrate solution of nitrogen-doped graphene N-rGO, 9mL and 0.5g are joined in 30mL deionized water, obtain homodisperse mixed solution B by stirring and ultrasonic Treatment；Wherein, the addition of nitrogen-doped graphene N-rGO is the 2% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；The reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 10h, furnace cooling or after water-cooled take out product。
5) first with acetone, mixture is carried out, then 10min is processed with the centrifugation of 8000r/min, it is carried out followed by dehydrated alcohol, centrifugal treating 10min under the speed of 8000r/min again, finally it is carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
Cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, obtains MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is at H2+N2It is annealed under atmosphere processing, improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state；Annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
Accompanying drawing 1 is the composite construction SEM photograph under this preparation condition, it can be seen that MoSe2Nanoscale twins cluster and the close contact of N-rGO lamella, N-rGO lamella is high-visible；MoSe is can be seen that from the TEM photo of Fig. 22Cluster diameter is about 110nm；Fig. 3 gives MoSe2/ N-rGO-2 composite construction and MoSe2Optical absorption characteristics, it is possible to becoming apparent from the obvious blue shift of absorption peak of composite construction, closer to the radiation spectrum of the sun, therefore this composite construction has very excellent absorbing properties；Fig. 4 is MoSe2/ N-rGO-2 composite construction and MoSe2PL spectrum, it can be seen that the PL peak of composite construction substantially reduces, and illustrates that the heterogeneous interface that composite construction is formed effectively inhibits the compound in light induced electron and hole；Fig. 5 adopts the electrochemical workstation LSV curve of test under dark and illumination condition respectively, it can be seen that under identical bias, MoSe2/ N-rGO-2 composite construction compares MoSe2There is bigger current-responsive, illustrate that this composite has good application prospect in Optical Electro-Chemistry hydrogen production by water decomposition。
Embodiment 3
1) it is the ammonia of 30% and the deionized water of 30mL by stirring and ultrasonic Treatment is sufficiently mixed by the graphene oxide of 25mg, the hydrazine hydrate of 3mL, concentration, obtains homodisperse mixed solution A；Wherein, ammonia is 1:50 with the volume ratio of hydrazine hydrate；
2) mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then take out product, dried for standby after furnace cooling or water-cooled, prepare nitrogen-doped graphene N-rGO；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；
3) selenium powder of 0.24g is dissolved in the hydrazine hydrate of 8mL, stands 35h, obtain selenium powder hydrazine hydrate solution；Again the two molybdic acid hydrate sodium of the selenium powder hydrazine hydrate solution of nitrogen-doped graphene N-rGO, 8mL and 0.4g are joined in 30mL deionized water, obtain homodisperse mixed solution B by stirring and ultrasonic Treatment；Wherein, the addition of nitrogen-doped graphene N-rGO is the 5% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；The reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 10h, furnace cooling or after water-cooled take out product。
5) first with acetone, mixture is carried out, then 10min is processed with the centrifugation of 8000r/min, it is carried out followed by dehydrated alcohol, centrifugal treating 10min under the speed of 8000r/min again, finally it is carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
Cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, obtains MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is at H2+N2It is annealed under atmosphere processing, improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state；Annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
MoSe prepared by the present embodiment2MoSe in/N-rGO composite construction2In nanoscale twins cluster, cluster diameter is 120nm, and is in close contact with N-rGO lamella, and N-rGO lamella has a small amount of reunion。
Embodiment 4
1) it is the ammonia of 30% and the deionized water of 30mL by stirring and ultrasonic Treatment is sufficiently mixed by the graphene oxide of 20mg, the hydrazine hydrate of 2mL, concentration, obtains homodisperse mixed solution A；Wherein, ammonia is 1:10 with the volume ratio of hydrazine hydrate；
2) mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then take out product, dried for standby after furnace cooling or water-cooled, prepare nitrogen-doped graphene N-rGO；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；
3) selenium powder of 0.2g is dissolved in the hydrazine hydrate of 7mL, stands 35h, obtain selenium powder hydrazine hydrate solution；Again the two molybdic acid hydrate sodium of the selenium powder hydrazine hydrate solution of nitrogen-doped graphene N-rGO, 7mL and 0.3g are joined in 30mL deionized water, obtain homodisperse mixed solution B by stirring and ultrasonic Treatment；Wherein, the addition of nitrogen-doped graphene N-rGO is the 1% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；The reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 20h, furnace cooling or after water-cooled take out product。
5) first with acetone, mixture is carried out, then 10min is processed with the centrifugation of 8000r/min, it is carried out followed by dehydrated alcohol, centrifugal treating 10min under the speed of 8000r/min again, finally it is carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
Cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, obtains MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is at H2+N2It is annealed under atmosphere processing, improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state；Annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
MoSe prepared by the present embodiment2MoSe in/N-rGO composite construction2In nanoscale twins cluster, cluster diameter is 150nm, is mutually wound heterojunction structure with N-rGO lamella。
Embodiment 5
1) it is the ammonia of 30% and the deionized water of 30mL by stirring and ultrasonic Treatment is sufficiently mixed by the graphene oxide of 20mg, the hydrazine hydrate of 3mL, concentration, obtains homodisperse mixed solution A；Wherein, ammonia is 1:10 with the volume ratio of hydrazine hydrate；
2) mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then take out product, dried for standby after furnace cooling or water-cooled, prepare nitrogen-doped graphene N-rGO；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；
3) selenium powder of 0.2g is dissolved in the hydrazine hydrate of 6mL, stands 30h, obtain selenium powder hydrazine hydrate solution；Again the two molybdic acid hydrate sodium of the selenium powder hydrazine hydrate solution of nitrogen-doped graphene N-rGO, 6mL and 0.3g are joined in 30mL deionized water, obtain homodisperse mixed solution B by stirring and ultrasonic Treatment；Wherein, the addition of nitrogen-doped graphene N-rGO is the 2% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；The reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 20h, furnace cooling or after water-cooled take out product。
5) first with acetone, mixture is carried out, then 10min is processed with the centrifugation of 8000r/min, it is carried out followed by dehydrated alcohol, centrifugal treating 10min under the speed of 8000r/min again, finally it is carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
Cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, obtains MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is at H2+N2It is annealed under atmosphere processing, improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state；Annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
MoSe prepared by the present embodiment2MoSe in/N-rGO composite construction2In nanoscale twins cluster, cluster diameter is that 160nm, N-rGO lamella is high-visible, is mutually wound heterojunction structure with N-rGO。
Embodiment 6
1) it is the ammonia of 30% and the deionized water of 30mL by stirring and ultrasonic Treatment is sufficiently mixed by the graphene oxide of 20mg, the hydrazine hydrate of 2mL, concentration, obtains homodisperse mixed solution A；Wherein, ammonia is 1:10 with the volume ratio of hydrazine hydrate；
2) mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then take out product, dried for standby after furnace cooling or water-cooled, prepare nitrogen-doped graphene N-rGO；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；
3) selenium powder of 0.2g is dissolved in the hydrazine hydrate of 5mL, stands 30h, obtain selenium powder hydrazine hydrate solution；Again the two molybdic acid hydrate sodium of the selenium powder hydrazine hydrate solution of nitrogen-doped graphene N-rGO, 5mL and 0.3g are joined in 30mL deionized water, obtain homodisperse mixed solution B by stirring and ultrasonic Treatment；Wherein, the addition of nitrogen-doped graphene N-rGO is the 5% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；The reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 10h, furnace cooling or after water-cooled take out product。
5) first with acetone, mixture is carried out, then 10min is processed with the centrifugation of 8000r/min, it is carried out followed by dehydrated alcohol, centrifugal treating 10min under the speed of 8000r/min again, finally it is carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
Cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, obtains MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is at H2+N2It is annealed under atmosphere processing, improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state；Annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
MoSe prepared by the present embodiment2MoSe in/N-rGO composite construction2In nanoscale twins cluster, cluster diameter is that 100nm, N-rGO lamella is high-visible, is mutually wound heterojunction structure with N-rGO。
Embodiment 7
1) it is the ammonia of 30% and the deionized water of 30mL by stirring and ultrasonic Treatment is sufficiently mixed by the graphene oxide of 15mg, the hydrazine hydrate of 1mL, concentration, obtains homodisperse mixed solution A；Wherein, ammonia is 1:5 with the volume ratio of hydrazine hydrate；
2) mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then take out product, dried for standby after furnace cooling or water-cooled, prepare nitrogen-doped graphene N-rGO；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；
3) selenium powder of 0.1g is dissolved in the hydrazine hydrate of 4mL, stands 25h, obtain selenium powder hydrazine hydrate solution；Again the two molybdic acid hydrate sodium of the selenium powder hydrazine hydrate solution of nitrogen-doped graphene N-rGO, 4mL and 0.2g are joined in 30mL deionized water, obtain homodisperse mixed solution B by stirring and ultrasonic Treatment；Wherein, the addition of nitrogen-doped graphene N-rGO is the 1% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；The reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 10h, furnace cooling or after water-cooled take out product。
5) first with acetone, mixture is carried out, then 10min is processed with the centrifugation of 8000r/min, it is carried out followed by dehydrated alcohol, centrifugal treating 10min under the speed of 8000r/min again, finally it is carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
Cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, obtains MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is at H2+N2It is annealed under atmosphere processing, improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state；Annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
MoSe prepared by the present embodiment2In/N-rGO composite construction, MoSe2In nanoscale twins cluster, cluster diameter is about 110nm, is mutually wound around with N-rGO lamella。
Embodiment 8
1) it is the ammonia of 30% and the deionized water of 30mL by stirring and ultrasonic Treatment is sufficiently mixed by the graphene oxide of 15mg, the hydrazine hydrate of 1mL, concentration, obtains homodisperse mixed solution A；Wherein, ammonia is 1:5 with the volume ratio of hydrazine hydrate；
2) mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then take out product, dried for standby after furnace cooling or water-cooled, prepare nitrogen-doped graphene N-rGO；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；
3) selenium powder of 0.1g is dissolved in the hydrazine hydrate of 2mL, stands 25h, obtain selenium powder hydrazine hydrate solution；Again the two molybdic acid hydrate sodium of the selenium powder hydrazine hydrate solution of nitrogen-doped graphene N-rGO, 2mL and 0.2g are joined in 30mL deionized water, obtain homodisperse mixed solution B by stirring and ultrasonic Treatment；Wherein, the addition of nitrogen-doped graphene N-rGO is the 2% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；The reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 10h, furnace cooling or after water-cooled take out product。
5) first with acetone, mixture is carried out, then 10min is processed with the centrifugation of 8000r/min, it is carried out followed by dehydrated alcohol, centrifugal treating 10min under the speed of 8000r/min again, finally it is carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
Cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, obtains MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is at H2+N2It is annealed under atmosphere processing, improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state；Annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
MoSe prepared by the present embodiment2In/N-rGO composite construction, MoSe2In nanoscale twins cluster, it is high-visible that cluster diameter is about 120nm, N-rGO, MoSe2Cluster and N-rGO lamella are wound around mutually。
Embodiment 9
1) it is the ammonia of 30% and the deionized water of 30mL by stirring and ultrasonic Treatment is sufficiently mixed by the graphene oxide of 10mg, the hydrazine hydrate of 0.5mL, concentration, obtains homodisperse mixed solution A；Wherein, ammonia is 1:5 with the volume ratio of hydrazine hydrate；
2) mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then take out product, dried for standby after furnace cooling or water-cooled, prepare nitrogen-doped graphene N-rGO；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；
3) selenium powder of 0.1g is dissolved in the hydrazine hydrate of 1mL, stands 20h, obtain selenium powder hydrazine hydrate solution；Again the two molybdic acid hydrate sodium of the selenium powder hydrazine hydrate solution of nitrogen-doped graphene N-rGO, 1mL and 0.1g are joined in 30mL deionized water, obtain homodisperse mixed solution B by stirring and ultrasonic Treatment；Wherein, the addition of nitrogen-doped graphene N-rGO is the 5% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；The reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 20h, furnace cooling or after water-cooled take out product。
5) first with acetone, mixture is carried out, then 10min is processed with the centrifugation of 8000r/min, it is carried out followed by dehydrated alcohol, centrifugal treating 10min under the speed of 8000r/min again, finally it is carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
Cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, obtains MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is at H2+N2It is annealed under atmosphere processing, improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state；Annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
MoSe prepared by the present embodiment2In/N-rGO composite construction, MoSe2In nanoscale twins cluster, cluster diameter is about 170nm, MoSe2Cluster and N-rGO lamella are wound around mutually, and N-rGO lamella has a small amount of reunion。
Embodiment 10
1) it is the ammonia of 30% and the deionized water of 30mL by stirring and ultrasonic Treatment is sufficiently mixed by the graphene oxide of 10mg, the hydrazine hydrate of 0.5mL, concentration, obtains homodisperse mixed solution A；Wherein, ammonia is 1:20 with the volume ratio of hydrazine hydrate；
2) mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then take out product, dried for standby after furnace cooling or water-cooled, prepare nitrogen-doped graphene N-rGO；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；
3) selenium powder of 0.3g is dissolved in the hydrazine hydrate of 6mL, stands 35h, obtain selenium powder hydrazine hydrate solution；Again the two molybdic acid hydrate sodium of the selenium powder hydrazine hydrate solution of nitrogen-doped graphene N-rGO, 6mL and 0.5g are joined in 30mL deionized water, obtain homodisperse mixed solution B by stirring and ultrasonic Treatment；Wherein, the addition of nitrogen-doped graphene N-rGO is the 4% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；The reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 20h, furnace cooling or after water-cooled take out product。
5) first with acetone, mixture is carried out, then 10min is processed with the centrifugation of 8000r/min, it is carried out followed by dehydrated alcohol, centrifugal treating 10min under the speed of 8000r/min again, finally it is carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
Cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, obtains MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is at H2+N2It is annealed under atmosphere processing, improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state；Annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
Embodiment 11
1) it is the ammonia of 30% and the deionized water of 30mL by stirring and ultrasonic Treatment is sufficiently mixed by the graphene oxide of 10mg, the hydrazine hydrate of 0.5mL, concentration, obtains homodisperse mixed solution A；Wherein, ammonia is 1:30 with the volume ratio of hydrazine hydrate；
2) mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then take out product, dried for standby after furnace cooling or water-cooled, prepare nitrogen-doped graphene N-rGO；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；
3) selenium powder of 0.1g is dissolved in the hydrazine hydrate of 4mL, stands 20h, obtain selenium powder hydrazine hydrate solution；Again the two molybdic acid hydrate sodium of the selenium powder hydrazine hydrate solution of nitrogen-doped graphene N-rGO, 4mL and 0.1g are joined in 30mL deionized water, obtain homodisperse mixed solution B by stirring and ultrasonic Treatment；Wherein, the addition of nitrogen-doped graphene N-rGO is the 2% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；The reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 15h, furnace cooling or after water-cooled take out product。
5) first with acetone, mixture is carried out, then 10min is processed with the centrifugation of 8000r/min, it is carried out followed by dehydrated alcohol, centrifugal treating 10min under the speed of 8000r/min again, finally it is carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
Cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, obtains MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is at H2+N2It is annealed under atmosphere processing, improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state；Annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
Embodiment 12
1) it is the ammonia of 30% and the deionized water of 30mL by stirring and ultrasonic Treatment is sufficiently mixed by the graphene oxide of 10mg, the hydrazine hydrate of 0.5mL, concentration, obtains homodisperse mixed solution A；Wherein, ammonia is 1:40 with the volume ratio of hydrazine hydrate；
2) mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then take out product, dried for standby after furnace cooling or water-cooled, prepare nitrogen-doped graphene N-rGO；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；
3) selenium powder of 0.3g is dissolved in the hydrazine hydrate of 8mL, stands 25h, obtain selenium powder hydrazine hydrate solution；Again the two molybdic acid hydrate sodium of the selenium powder hydrazine hydrate solution of nitrogen-doped graphene N-rGO, 8mL and 0.5g are joined in 30mL deionized water, obtain homodisperse mixed solution B by stirring and ultrasonic Treatment；Wherein, the addition of nitrogen-doped graphene N-rGO is the 3% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；Wherein, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL；The reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 15h, furnace cooling or after water-cooled take out product。
5) first with acetone, mixture is carried out, then 10min is processed with the centrifugation of 8000r/min, it is carried out followed by dehydrated alcohol, centrifugal treating 10min under the speed of 8000r/min again, finally it is carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
Cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, obtains MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is at H2+N2It is annealed under atmosphere processing, improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state；Annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
It also have the advantage that 1) design of the present invention is clear, and principle is understandable；2) preparation method of the present invention is simple, can prepare N-rGO/MoSe by two step hydro-thermal reactions2Composite construction；3) the composite heterogeneous interface that prepared by the present invention can promote efficiently separating of light induced electron and hole, significantly improves Optical Electro-Chemistry hydrogen production by water decomposition efficiency；4) the invention provides a kind of technical thought utilizing two-dimensional material interlayer coupling to realize light absorption and Optical Electro-Chemistry hydrogen production by water decomposition performance enhancement and method。
Above content is only the technological thought that the present invention is described, it is impossible to limits protection scope of the present invention, every technological thought proposed according to the present invention, any change done on technical scheme basis with this, each falls within the protection domain of claims of the present invention。
Claims (10)
1. a nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The preparation method of composite construction, it is characterised in that comprise the following steps:
1) graphene oxide of 10～30mg, the hydrazine hydrate of 0.5～5mL, concentration are the ammonia of 30% and the deionized water of 30mL is sufficiently mixed, obtain homodisperse mixed solution A；Wherein, ammonia is 1:(5～50 with the volume ratio of hydrazine hydrate)；
2) with autoclave for holding vessel, mixed solution A, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO；
3) selenium powder of 0.1～0.3g is dissolved in the hydrazine hydrate of 1～10mL, stands 20～40h, obtain selenium powder hydrazine hydrate solution；Again nitrogen-doped graphene N-rGO, the selenium powder hydrazine hydrate solution of 1～10mL and the two molybdic acid hydrate sodium of 0.1～0.5g are joined in 30mL deionized water, be sufficiently mixed and obtain homodisperse mixed solution B；Wherein, the addition of nitrogen-doped graphene N-rGO is the 1%～5% of two molybdic acid hydrate sodium additions；
4) with autoclave for holding vessel, mixed solution B, as reactant, adopts hydro-thermal method, prepares nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2The mixture of composite construction；
5) mixture it is carried out and dries, obtaining MoSe2/ N-rGO composite construction powder；
6) to MoSe2/ N-rGO composite construction powder is annealed processing, and improves MoSe2The degree of crystallinity of/N-rGO composite construction powder and interface state。
2. nitrogen-doped graphene N-rGO according to claim 1 and nanoscale twins cluster MoSe2The preparation method of composite construction, it is characterised in that described step 1) in, it is sufficiently mixed by stirring and ultrasonic Treatment。
3. nitrogen-doped graphene N-rGO according to claim 1 and nanoscale twins cluster MoSe2The preparation method of composite construction, it is characterised in that described step 2) and step 4) in, autoclave is that Teflon still lining is equipped with rustless steel still set, and volume is 50mL。
4. the nitrogen-doped graphene N-rGO according to claim 1 or 3 and nanoscale twins cluster MoSe2The preparation method of composite construction, it is characterised in that described step 2) in, mixed solution A is positioned in autoclave, then autoclave is positioned in baking oven, at the temperature of 180 DEG C, react 12h, then product, dried for standby are taken out after furnace cooling or water-cooled。
5. nitrogen-doped graphene N-rGO according to claim 1 and nanoscale twins cluster MoSe2The preparation method of composite construction, it is characterised in that described step 3) in, mixed solution B obtains homodisperse suspension by stirring and ultrasonic Treatment。
6. nitrogen-doped graphene N-rGO according to claim 1 and nanoscale twins cluster MoSe2The preparation method of composite construction, it is characterised in that described step 4) in, the reaction temperature of hydro-thermal method is 200 DEG C, and the response time is 10～20h, furnace cooling or after water-cooled take out product。
7. nitrogen-doped graphene N-rGO according to claim 1 and nanoscale twins cluster MoSe2The preparation method of composite construction, described step 5) in, cleaning treatment is for be first carried out mixture with acetone, then 10min is processed with the centrifugation of 8000r/min, be carried out followed by dehydrated alcohol, then under the speed of 8000r/min centrifugal treating 10min, be finally carried out with deionized water, and the product dehydrated alcohol after cleaning is disperseed and air-dry, stand-by。
8. the nitrogen-doped graphene N-rGO according to claim 1 or 7 and nanoscale twins cluster MoSe2The preparation method of composite construction, it is characterised in that described step 5) in, cleaned mixture is placed in vacuum drying oven, at the temperature of 70 DEG C, dries 12h, obtain nitrogen-doped graphene N-rGO and nanoscale twins cluster MoSe2Composite construction powder, stand-by。
9. the nitrogen-doped graphene N-rGO according to claim 1 or 7 and nanoscale twins cluster MoSe2The preparation method of composite construction, it is characterised in that described step 6) in, at H2+N2Being annealed under atmosphere processing, annealing temperature is 450 DEG C, and heating rate is 15 DEG C/min, and temperature retention time is 1h, furnace cooling。
10. the nitrogen-doped graphene N-rGO adopting method described in claim 1 to prepare an and nanoscale twins cluster MoSe2Composite construction, it is characterised in that the MoSe of preparation2In/N-rGO composite construction, MoSe2In nanoscale twins cluster, cluster diameter is about 100～170nm, MoSe2Cluster and N-rGO lamella are wound heterojunction structure mutually。
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