CN105679848A - Preparation method of three-dimensional graphene foam composite nano-cadmium sulfide photoelectrochemical electrode - Google Patents
Preparation method of three-dimensional graphene foam composite nano-cadmium sulfide photoelectrochemical electrode Download PDFInfo
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- CN105679848A CN105679848A CN201610034393.7A CN201610034393A CN105679848A CN 105679848 A CN105679848 A CN 105679848A CN 201610034393 A CN201610034393 A CN 201610034393A CN 105679848 A CN105679848 A CN 105679848A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 222
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 222
- 239000006260 foam Substances 0.000 title claims abstract description 210
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 130
- 239000002131 composite material Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 154
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 claims abstract description 115
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 77
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000005530 etching Methods 0.000 claims abstract description 14
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 90
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 72
- 239000001257 hydrogen Substances 0.000 claims description 63
- 229910052739 hydrogen Inorganic materials 0.000 claims description 61
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 54
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 49
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 49
- 229910052786 argon Inorganic materials 0.000 claims description 45
- 239000000126 substance Substances 0.000 claims description 41
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 27
- 238000001291 vacuum drying Methods 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000000758 substrate Substances 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000010792 warming Methods 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 13
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 11
- 239000003292 glue Substances 0.000 claims description 11
- 238000000137 annealing Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 150000002431 hydrogen Chemical class 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 4
- -1 graphite alkene Chemical class 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 239000008246 gaseous mixture Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 2
- 239000012780 transparent material Substances 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 150000001875 compounds Chemical class 0.000 description 9
- 230000005518 electrochemistry Effects 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 7
- 230000006798 recombination Effects 0.000 description 7
- 238000005215 recombination Methods 0.000 description 7
- 238000004506 ultrasonic cleaning Methods 0.000 description 7
- 238000001069 Raman spectroscopy Methods 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002848 electrochemical method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000005476 size effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000012353 t test Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0296—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1828—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIBVI compounds, e.g. CdS, ZnS, CdTe
Abstract
The invention discloses a preparation method of a three-dimensional graphene foam composite nano-cadmium sulfide photoelectrochemical electrode. The method comprises the following steps: growing graphene on nickel foam by a chemical vapor deposition method, removing the nickel foam by an etching process to obtain three-dimensional graphene foam; compounding nano-cadmium sulfide with the three-dimensional graphene foam through the chemical vapor deposition method; and finally preparing the photoelectrochemical electrode from the three-dimensional graphene foam composite nano-cadmium sulfide by a photoelectrochemical electrode process. The three-dimensional graphene has excellent conductive grids and large specific surface area, provides a conductive channel with sufficient cadmium sulfide for electron transportation and reduces the photocurrent loss. The novel preparation method of the three-dimensional graphene foam composite nano-cadmium sulfide photoelectrochemical electrode, which is low in cost and beneficial to mass production has a potential application prospect in the fields of the photoelectrochemical electrode and a sensor.
Description
Technical field
The invention belongs to PhotoelectrochemicalTechnique Technique field, be specifically related to the photoelectric chemical electrode preparation method field of three-dimensional graphene foam composite Nano cadmium sulfide.
Background technology
Optical Electro-Chemistry is one of mode utilizing solar energy, merges photochemistry and electrochemical method, by metal or semi-conducting electrode absorbed light, produces energy accumulation or electrode reaction, completes the conversion of luminous energy and electric energy and chemical energy. Optical Electro-Chemistry is compared to other advantages of methods obtaining solar energys and is in that its low cost, but conversion efficiency is low, electrode easily occurs electron hole in conjunction with phenomenon. Therefore, photoelectric chemical electrode needs possess the ability quickly transmitting electronics.
Cadmium sulfide is intrinsic/n-type quasiconductor, has a wide range of applications in opto-electronic conversion and photocatalysis field. Nano cadmium sulphide has bigger specific surface area, Small-scale fading and quantum size effects. Quantum size effect makes that the energy level of cadmium sulfide changes, energy gap broadens, and Absorption and emission spectra moves to shortwave direction; Skin effect causes the change of CdS nano-particle surface atom transport and configuration, also causes the change of surface electronic spin conformation and electron spectrum simultaneously. The photoelectric chemical electrode of the titanium dioxide composite sulfur cadmium currently mainly adopted, but owing to the electron transport ability of titanium dioxide itself is more weak, its technology enters the bottleneck phase. On this basis, people pass through graphene-supported cadmium sulfide, but traditional two-dimensional graphene is due to its two-dimension plane structure, the cadmium sulfide limited material of institute's load.
Summary of the invention
The purpose of the present invention is contemplated to overcome the deficiency of above-mentioned background technology, it is provided that the preparation method of the photoelectric chemical electrode of a kind of three-dimensional graphene foam composite Nano cadmium sulfide.
The preparation method step of the photoelectric chemical electrode of a kind of three-dimensional graphene foam composite Nano cadmium sulfide involved in the present invention is as follows:
Step one: grow Graphene in nickel foam;
By chemical vapour deposition technique, deposited graphite alkene in nickel foam; Graphene growth condition is growth at atmosphere, growth temperature is 700～1100 DEG C, pass into the gaseous mixture of argon, hydrogen and three kinds of gases of methane, the mixed proportion of these three gas is argon: hydrogen: methane=200:80:5, growth time controls, at 10～30min, to finally give the three-dimensional grapheme not etching nickel foam;
Graphene growth specifically includes: heats up, anneal, grow three steps; Temperature-rise period: 60min is warming up to 700～1100 DEG C, argon=200sccm, hydrogen=80sccm; Annealing process: 10～15min, maintains same temperature, argon=200sccm, hydrogen=80sccm; Growth course: 10～30min, maintains same temperature, methane: hydrogen: argon=5:80:200sccm; Growth closes methane after terminating, and opens fan fast cooling, finally gently takes out the nickel foam of the upper Graphene of growth;
Step 2: etched nickel but do not removed the three-dimensional graphene foam of PMMA protecting film;
By being uniformly coated with the PMMA solution of 0.1～1.5% on the graphene film in square nickel foam, in vacuum drying oven, heating 10～60min, heating-up temperature is 80～150 DEG C; Being put into by the sample scribbling PMMA in 1～5MHCl of constant temperature 80 DEG C, etch period is 6～24hour again; After etching, sample is positioned in deionized water and invades bubble 5～10min, repeat 3 times; Again three-dimensional graphene foam is placed in vacuum drying oven, in a low voltage state, is warming up to 60～100 DEG C, keep 40min; In this dry run, every 10min opens vacuum pump, pumps the water vapour in vacuum drying oven; Finally give the three-dimensional graphene foam etching nickel but do not remove PMMA protecting film;
Step 3: obtain removing the dry three-dimensional graphene foam of PMMA protecting film
Will etch nickel but do not remove the three-dimensional graphene foam of PMMA protecting film and put in tube furnace, in low pressure, in 10～40sccm hydrogen, 400～600 DEG C of heating, 30～120min; After having annealed, PMMA protecting film can be removed, obtain the three-dimensional graphene foam dried;
Step 4: obtain three-dimensional graphene foam composite Nano cadmium sulfide;
By chemical vapour deposition technique, three-dimensional graphene foam deposits Nano cadmium sulphide; The condition of deposition Nano cadmium sulphide is low-pressure growth, passes into hydrogen, and cadmium sulfide source is the cadmium sulfide powder of 99.999%, and cadmium sulfide source temperature is 400～800 DEG C; Three-dimensional graphene foam is being placed from 0.1～1dm place, source; Growth time is 1～10mins; Finally give three-dimensional graphene foam composite Nano cadmium sulfide;
Step 5: obtain the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide;
Being fixed in transparent substrates 2 by three-dimensional graphene foam composite Nano cadmium sulfide, transparent substrates is PET, glass or the quartzy transparent material for base material. Connect by conductive silver paste 4 on three-dimensional graphene foam composite Nano cadmium sulfide surface and draw circuit 3, connect and draw circuit 3 for copper cash or silver wire; Use AB glue to be connect on three-dimensional graphene foam composite Nano cadmium sulfide surface to draw the part of circuit 3, conductive silver paste 4 place and connecing and draw circuit 3 and contact the part covering of transparent substrates 2; Finally give the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide.
Three-dimensional graphene foam is the two-dimensional graphene a kind of existing way in the middle of three dimensions, is by one of two-dimensional graphene important way expanding to three dimensional structure. Three-dimensional graphene foam not only remains the original excellent physical chemical property of two-dimensional graphene, simultaneously because the microstructure of its foam-like porous, gives its low-density, bigger serface and high conductivity. Three-dimensional graphene foam composite Nano cadmium sulfide possesses the ability quickly transmitting electronics as the conductive network that Optical Electro-Chemistry anode material provides, reduce electron hole pair to combine, widen the absorbing light spectral region of Nano cadmium sulphide, improve the electrooptical device efficiency of material after compound.Therefore, this novel low-cost, be conducive to the method for the photoelectric chemical electrode of the three-dimensional graphene foam composite Nano cadmium sulfide of large-scale production will to have potential application prospect at photoelectric chemical electrode and sensor field.
Nano cadmium sulphide generally seldom individually application, is because himself having a large amount of efficient photo-generated carrier, but owing to the carrier transport ability of cadmium sulfide is weak, just causes again the substantial amounts of compound again of photo-generated carrier, thus reducing again its photoelectric transformation efficiency. Therefore the application of cadmium sulfide needs effectively assist it quickly to transmit the material of photo-generated carrier. For traditional cadmium sulfide composite material, being generally metal-oxide, metal-oxide is loose structure, has big surface area, it is possible to the more Nano cadmium sulphide of load, but electron transport ability is more weak. Since grapheme material development, by three-dimensional grapheme and cadmium sulfide compound, it is possible to improved the electrology characteristic of entirety by the superpower electron transport ability of Graphene. But existing three-dimensional grapheme is prepared by self assembly, the three-dimensional grapheme prepared by this method being partially bordering on chemical preparation is in electron transport ability and not up to its desirable. Three-dimensional graphene foam be prepared by chemical vapour deposition technique, three-dimensional graphene foam prepared by this method is it is verified that have the electron transport ability close to two-dimensional graphene. Therefore, contrasting existing three-dimensional grapheme composite Nano cadmium sulfide Optical Electro-Chemistry anode, three-dimensional graphene foam composite Nano cadmium sulfide Optical Electro-Chemistry anode has better light transfer characteristic and less impedance.
Accompanying drawing explanation
Fig. 1 is the photoelectric chemical electrode preparation flow figure of three-dimensional graphene foam composite Nano cadmium sulfide;
Fig. 2 is nickel foam and SEM figure thereof;
Fig. 3 is graphene film and the SEM figure thereof of growth on nickel foam;
Fig. 4 is dry three-dimensional graphene foam and SEM figure thereof;
Fig. 5 is three-dimensional graphene foam and the SEM figure thereof of composite Nano cadmium sulfide;
Fig. 6 is the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide; Wherein 1 is Optical Electro-Chemistry anode, and 2 is transparent substrates, and 3 draw circuit for connecing, and 4 is conductive silver paste, and 5 is AB glue encapsulated layer;
Fig. 7 is three-dimensional graphene foam and the Raman collection of illustrative plates of three-dimensional graphene foam composite Nano cadmium sulfide; Wherein a be three-dimensional graphene foam Raman collection of illustrative plates, b is the Raman collection of illustrative plates of three-dimensional graphene foam composite Nano cadmium sulfide;
Fig. 8 is the XRD figure spectrum of three-dimensional graphene foam and three-dimensional graphene foam composite Nano cadmium sulfide;
Fig. 9 is the ON/OFF light I-t test figure of three-dimensional grapheme composite sulfur cadmium nano-particle photoelectric chemical electrode;
Figure 10 is the cyclic voltammetry test figure of three-dimensional grapheme composite sulfur cadmium nano-particle photoelectric chemical electrode.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention will be further described.
Implement row 1
The preparation method of the photoelectric chemical electrode of a kind of three-dimensional graphene foam composite Nano cadmium sulfide is as it is shown in figure 1, specifically comprise the following steps that
1) nickel foam as shown in Figure 2 is tailored into the square of 1cm*1cm.
2) square nickel foam is respectively placed in acetone, ethanol, deionized water for ultrasonic cleaning 10min, dries up with nitrogen standby.
3) dried square nickel foam is positioned in CVD system vacuum cavity and carries out graphene film growth, it is thus achieved that graphene film. The growth conditions of graphene film is growth at atmosphere, growth temperature is 700 DEG C, pass into the mixing gas (specific proportions argon: hydrogen: methane=200:80:5sccm) of argon, hydrogen and methane, growth time is 15min, finally giving the graphene film in square nickel foam, on nickel foam, the graphene film of growth is as shown in Figure 3.
Graphene growth specifically includes: heats up, anneal, grow three steps; Temperature-rise period: 60min is warming up to 700 DEG C, argon=200sccm, hydrogen=80sccm; Annealing process: 10～15min, maintains same temperature 700 DEG C, argon=200sccm, hydrogen=80sccm; Growth course: 10～30min, maintains same temperature 700 DEG C, methane: hydrogen: argon=5:80:200sccm; Growth closes methane after terminating, and opens fan fast cooling, finally gently takes out the nickel foam of the upper Graphene of growth;
4) by being uniformly coated with the PMMA solution of 0.2% on the graphene film in square nickel foam, in vacuum drying oven, heating 30min, heating-up temperature is 80 DEG C. Being put into by the sample scribbling PMMA in the 2MHCl of constant temperature 80 DEG C, etch period is 6hour again. After etching, sample is positioned in deionized water and invades bubble 10min, repeat 3 times. Again three-dimensional graphene foam is placed in vacuum drying oven, in a low voltage state, is warming up to 80 DEG C, keep 40min. In this dry run, every 10min opens vacuum pump, pumps the water vapour in vacuum drying oven. Etched nickel but do not removed the three-dimensional graphene foam of PMMA protecting film.
5) will etch nickel but do not remove the three-dimensional graphene foam of PMMA protecting film and put in tube furnace, in low pressure, 30sccm hydrogen, 450 DEG C of heating, 90min. After having annealed, can removing PMMA protecting film, obtain the three-dimensional graphene foam dried, dry three-dimensional graphene foam is as shown in Figure 4.
6) dry three-dimensional graphene foam is positioned over the compound carrying out cadmium sulfide nanoparticles in CVD system vacuum cavity, it is thus achieved that the three-dimensional graphene foam of composite Nano cadmium sulfide. In recombination process, the growth conditions of cadmium sulfide nanoparticles is low-pressure growth, and source temperature is 500 DEG C, and passing into hydrogen flowing quantity is 30sccm. Cadmium sulfide powder by 99.999% is positioned over source position, then three-dimensional graphene foam is positioned over distance sources 1dm place, and growth time is 3min. The three-dimensional graphene foam of composite Nano cadmium sulfide is as shown in Figure 5.
7) three-dimensional graphene foam composite Nano cadmium sulfide is fixed in the transparent substrates 2 that PET is base material as Optical Electro-Chemistry anode 1, connect by conductive silver paste 4 on three-dimensional graphene foam composite Nano cadmium sulfide surface and draw circuit 3, connect and draw circuit 3 for silver wire. Use AB glue to be connect on three-dimensional graphene foam composite Nano cadmium sulfide surface as AB glue encapsulated layer 5 draw the part of circuit 3, conductive silver paste 4 place and connect and draw circuit 3 and contact the part covering of transparent substrates 2. Finally giving the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide, the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide is as shown in Figure 6. This electrode has been carried out performance characterization and test, such as Raman spectrum analysis, XRD test and electrochemical Characterization analysis, Raman spectrum analysis result as it is shown in fig. 7, wherein a be three-dimensional graphene foam Raman collection of illustrative plates, b is the Raman collection of illustrative plates of three-dimensional graphene foam composite Nano cadmium sulfide; As shown in Figure 8, electrochemical Characterization analyzes result as shown in Figure 9 and Figure 10 to XRD test result.
Implement row 2
The preparation method of the photoelectric chemical electrode of a kind of three-dimensional graphene foam composite Nano cadmium sulfide, specifically comprises the following steps that
1) nickel foam as shown in Figure 2 is tailored into the square of 1cm*1cm.
2) square nickel foam is respectively placed in acetone, ethanol, deionized water for ultrasonic cleaning 10min, dries up with nitrogen standby.
3) dried square nickel foam is positioned in CVD system vacuum cavity and carries out graphene film growth, it is thus achieved that graphene film. The growth conditions of graphene film is growth at atmosphere, growth temperature is 1000 DEG C, pass into the mixing gas (specific proportions argon: hydrogen: methane=200:80:5sccm) of argon, hydrogen and methane, growth time is 30min, finally gives the graphene film in square nickel foam.
Graphene growth specifically includes: heats up, anneal, grow three steps; Temperature-rise period: 60min is warming up to 1000 DEG C, argon=200sccm, hydrogen=80sccm; Annealing process: 10～15min, maintains same temperature 1000 DEG C, argon=200sccm, hydrogen=80sccm; Growth course: 10～30min, maintains same temperature 1000 DEG C, methane: hydrogen: argon=5:80:200sccm; Growth closes methane after terminating, and opens fan fast cooling, finally gently takes out the nickel foam of the upper Graphene of growth;
4) by being uniformly coated with the PMMA solution of 0.5% on the graphene film in square nickel foam, in vacuum drying oven, heating 30min, heating-up temperature is 120 DEG C. Being put into by the sample scribbling PMMA in the 5MHCl of constant temperature 100 DEG C, etch period is 12hour again. After etching, sample is positioned in deionized water and invades bubble 10min, repeat 3 times. Again three-dimensional graphene foam is placed in vacuum drying oven, in a low voltage state, is warming up to 80 DEG C, keep 40min. In this dry run, every 10min opens vacuum pump, pumps the water vapour in vacuum drying oven. Etched nickel but do not removed the three-dimensional graphene foam of PMMA protecting film.
5) will etch nickel but do not remove the three-dimensional graphene foam of PMMA protecting film and put in tube furnace, in low pressure, 30sccm hydrogen, 500 DEG C of heating, 150min. After having annealed, PMMA protecting film can be removed, obtain the three-dimensional graphene foam dried.
6) dry three-dimensional graphene foam is positioned over the compound carrying out cadmium sulfide nanoparticles in CVD system vacuum cavity, it is thus achieved that the three-dimensional graphene foam of composite Nano cadmium sulfide. In recombination process, the growth conditions of cadmium sulfide nanoparticles is low-pressure growth, and source temperature is 600 DEG C, and passing into hydrogen flowing quantity is 30sccm. Cadmium sulfide powder by 99.999% is positioned over source position, then three-dimensional graphene foam is positioned over distance sources 1dm place, and growth time is 8min.
7) three-dimensional graphene foam composite Nano cadmium sulfide is fixed in the transparent substrates 2 that PET is base material, is connect by conductive silver paste 4 on three-dimensional graphene foam composite Nano cadmium sulfide surface and draw circuit 3, connect and draw circuit 3 for silver wire. Use AB glue to be connect on three-dimensional graphene foam composite Nano cadmium sulfide surface to draw the part of circuit 3, conductive silver paste 4 place and connecing and draw circuit 3 and contact the part covering of transparent substrates 2. Finally giving the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide, the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide is as shown in Figure 6.
Implement row 3
The preparation method of the photoelectric chemical electrode of a kind of three-dimensional graphene foam composite Nano cadmium sulfide is as it is shown in figure 1, specifically comprise the following steps that
1) nickel foam as shown in Figure 2 is tailored into the square of 1cm*1cm.
2) square nickel foam is respectively placed in acetone, ethanol, deionized water for ultrasonic cleaning 10min, dries up with nitrogen standby.
3) dried square nickel foam is positioned in CVD system vacuum cavity and carries out graphene film growth, it is thus achieved that graphene film.The growth conditions of graphene film is growth at atmosphere, growth temperature is 700 DEG C, pass into the mixing gas (specific proportions argon: hydrogen: methane=200:80:5sccm) of argon, hydrogen and methane, growth time is 10min, finally gives the graphene film in square nickel foam.
Graphene growth specifically includes: heats up, anneal, grow three steps; Temperature-rise period: 60min is warming up to 700 DEG C, argon=200sccm, hydrogen=80sccm; Annealing process: 10min, maintains same temperature 700 DEG C, argon=200sccm, hydrogen=80sccm; Growth course: 10min, maintains same temperature 700 DEG C, methane: hydrogen: argon=5:80:200sccm; Growth closes methane after terminating, and opens fan fast cooling, finally gently takes out the nickel foam of the upper Graphene of growth;
4) by being uniformly coated with the PMMA solution of 0.1% on the graphene film in square nickel foam, in vacuum drying oven, heating 10min, heating-up temperature is 80 DEG C. Being put into by the sample scribbling PMMA in the 1MHCl of constant temperature 80 DEG C, etch period is 6hour again. After etching, sample is positioned in deionized water and invades bubble 5min, repeat 3 times. Again three-dimensional graphene foam is placed in vacuum drying oven, in a low voltage state, is warming up to 60 DEG C, keep 40min. In this dry run, every 10min opens vacuum pump, pumps the water vapour in vacuum drying oven. Etched nickel but do not removed the three-dimensional graphene foam of PMMA protecting film.
5) will etch nickel but do not remove the three-dimensional graphene foam of PMMA protecting film and put in tube furnace, in low pressure, 10sccm hydrogen, 400 DEG C of heating, 30min. After having annealed, PMMA protecting film can be removed, obtain the three-dimensional graphene foam dried.
6) dry three-dimensional graphene foam is positioned over the compound carrying out cadmium sulfide nanoparticles in CVD system vacuum cavity, it is thus achieved that the three-dimensional graphene foam of composite Nano cadmium sulfide. In recombination process, the growth conditions of cadmium sulfide nanoparticles is low-pressure growth, and source temperature is 400 DEG C, and passing into hydrogen flowing quantity is 30sccm. Cadmium sulfide powder by 99.999% is positioned over source position, then three-dimensional graphene foam is positioned over distance sources 1dm place, and growth time is 1min.
7) three-dimensional graphene foam composite Nano cadmium sulfide is fixed in the transparent substrates 2 that PET is base material, connects on three-dimensional graphene foam composite Nano cadmium sulfide surface draw circuit 3 by conductive silver paste 4, connect that to draw circuit 3 be copper cash. Use AB glue to be connect on three-dimensional graphene foam composite Nano cadmium sulfide surface to draw the part of circuit 3, conductive silver paste 4 place and connecing and draw circuit 3 and contact the part covering of transparent substrates 2. Finally giving the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide, the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide is as shown in Figure 6.
Implement row 4
The preparation method of the photoelectric chemical electrode of a kind of three-dimensional graphene foam composite Nano cadmium sulfide is as it is shown in figure 1, specifically comprise the following steps that
1) nickel foam as shown in Figure 2 is tailored into the square of 1cm*1cm.
2) square nickel foam is respectively placed in acetone, ethanol, deionized water for ultrasonic cleaning 10min, dries up with nitrogen standby.
3) dried square nickel foam is positioned in CVD system vacuum cavity and carries out graphene film growth, it is thus achieved that graphene film. The growth conditions of graphene film is growth at atmosphere, growth temperature is 1100 DEG C, pass into the mixing gas (specific proportions argon: hydrogen: methane=200:80:5sccm) of argon, hydrogen and methane, growth time is 30min, finally gives the graphene film in square nickel foam.
Graphene growth specifically includes: heats up, anneal, grow three steps; Temperature-rise period: 60min is warming up to 1100 DEG C, argon=200sccm, hydrogen=80sccm; Annealing process: 15min, maintains same temperature 1100 DEG C, argon=200sccm, hydrogen=80sccm; Growth course: 30min, maintains same temperature 1100 DEG C, methane: hydrogen: argon=5:80:200sccm; Growth closes methane after terminating, and opens fan fast cooling, finally gently takes out the nickel foam of the upper Graphene of growth;
4) by being uniformly coated with the PMMA solution of 1.5% on the graphene film in square nickel foam, in vacuum drying oven, heating 60min, heating-up temperature is 150 DEG C. Being put into by the sample scribbling PMMA in the 5MHCl of constant temperature 80 DEG C, etch period is 24hour again. After etching, sample is positioned in deionized water and invades bubble 10min, repeat 3 times. Again three-dimensional graphene foam is placed in vacuum drying oven, in a low voltage state, is warming up to 100 DEG C, keep 40min. In this dry run, every 10min opens vacuum pump, pumps the water vapour in vacuum drying oven. Etched nickel but do not removed the three-dimensional graphene foam of PMMA protecting film.
5) will etch nickel but do not remove the three-dimensional graphene foam of PMMA protecting film and put in tube furnace, in low pressure, 40sccm hydrogen, 600 DEG C of heating, 120min. After having annealed, PMMA protecting film can be removed, obtain the three-dimensional graphene foam dried.
6) dry three-dimensional graphene foam is positioned over the compound carrying out cadmium sulfide nanoparticles in CVD system vacuum cavity, it is thus achieved that the three-dimensional graphene foam of composite Nano cadmium sulfide. In recombination process, the growth conditions of cadmium sulfide nanoparticles is low-pressure growth, and source temperature is 800 DEG C, and passing into hydrogen flowing quantity is 30sccm. Cadmium sulfide powder by 99.999% is positioned over source position, then three-dimensional graphene foam is positioned over distance sources 0.1dm place, and growth time is 10min.
7) three-dimensional graphene foam composite Nano cadmium sulfide is fixed in the transparent substrates 2 that glass is base material, is connect by conductive silver paste 4 on three-dimensional graphene foam composite Nano cadmium sulfide surface and draw circuit 3, connect and draw circuit 3 for silver wire. Use AB glue to be connect on three-dimensional graphene foam composite Nano cadmium sulfide surface to draw the part of circuit 3, conductive silver paste 4 place and connecing and draw circuit 3 and contact the part covering of transparent substrates 2. Finally giving the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide, the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide is as shown in Figure 6.
Implement row 5
The preparation method of the photoelectric chemical electrode of a kind of three-dimensional graphene foam composite Nano cadmium sulfide is as it is shown in figure 1, specifically comprise the following steps that
1) nickel foam as shown in Figure 2 is tailored into the square of 1cm*1cm.
2) square nickel foam is respectively placed in acetone, ethanol, deionized water for ultrasonic cleaning 10min, dries up with nitrogen standby.
3) dried square nickel foam is positioned in CVD system vacuum cavity and carries out graphene film growth, it is thus achieved that graphene film. The growth conditions of graphene film is growth at atmosphere, growth temperature is 700 DEG C, pass into the mixing gas (specific proportions argon: hydrogen: methane=200:80:5sccm) of argon, hydrogen and methane, growth time is 10min, finally gives the graphene film in square nickel foam.
Graphene growth specifically includes: heats up, anneal, grow three steps;Temperature-rise period: 60min is warming up to 700 DEG C, argon=200sccm, hydrogen=80sccm; Annealing process: 10min, maintains same temperature 700 DEG C, argon=200sccm, hydrogen=80sccm; Growth course: 10min, maintains same temperature 700 DEG C, methane: hydrogen: argon=5:80:200sccm; Growth closes methane after terminating, and opens fan fast cooling, finally gently takes out the nickel foam of the upper Graphene of growth;
4) by being uniformly coated with the PMMA solution of 0.1 on the graphene film in square nickel foam, in vacuum drying oven, heating 60min, heating-up temperature is 80 DEG C. Being put into by the sample scribbling PMMA in the 2MHCl of constant temperature 80 DEG C, etch period is 8hour again. After etching, sample is positioned in deionized water and invades bubble 7min, repeat 3 times. Again three-dimensional graphene foam is placed in vacuum drying oven, in a low voltage state, is warming up to 75 DEG C, keep 40min. In this dry run, every 10min opens vacuum pump, pumps the water vapour in vacuum drying oven. Etched nickel but do not removed the three-dimensional graphene foam of PMMA protecting film.
5) will etch nickel but do not remove the three-dimensional graphene foam of PMMA protecting film and put in tube furnace, in low pressure, 20sccm hydrogen, 550 DEG C of heating, 75min. After having annealed, PMMA protecting film can be removed, obtain the three-dimensional graphene foam dried.
6) dry three-dimensional graphene foam is positioned over the compound carrying out cadmium sulfide nanoparticles in CVD system vacuum cavity, it is thus achieved that the three-dimensional graphene foam of composite Nano cadmium sulfide. In recombination process, the growth conditions of cadmium sulfide nanoparticles is low-pressure growth, and source temperature is 600 DEG C, and passing into hydrogen flowing quantity is 30sccm. Cadmium sulfide powder by 99.999% is positioned over source position, then three-dimensional graphene foam is positioned over distance sources 0.5dm place, and growth time is 7min.
7) three-dimensional graphene foam composite Nano cadmium sulfide is fixed in the transparent substrates 2 that quartz is base material, is connect by conductive silver paste 4 on three-dimensional graphene foam composite Nano cadmium sulfide surface and draw circuit 3, connect and draw circuit 3 for silver wire. Use AB glue to be connect on three-dimensional graphene foam composite Nano cadmium sulfide surface to draw the part of circuit 3, conductive silver paste 4 place and connecing and draw circuit 3 and contact the part covering of transparent substrates 2. Finally giving the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide, the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide is as shown in Figure 6.
Implement row 6
The preparation method of the photoelectric chemical electrode of a kind of three-dimensional graphene foam composite Nano cadmium sulfide is as it is shown in figure 1, specifically comprise the following steps that
1) nickel foam as shown in Figure 2 is tailored into the square of 1cm*1cm.
2) square nickel foam is respectively placed in acetone, ethanol, deionized water for ultrasonic cleaning 10min, dries up with nitrogen standby.
3) dried square nickel foam is positioned in CVD system vacuum cavity and carries out graphene film growth, it is thus achieved that graphene film. The growth conditions of graphene film is growth at atmosphere, growth temperature is 900 DEG C, pass into the mixing gas (specific proportions argon: hydrogen: methane=200:80:5sccm) of argon, hydrogen and methane, growth time is 20min, finally gives the graphene film in square nickel foam.
Graphene growth specifically includes: heats up, anneal, grow three steps; Temperature-rise period: 60min is warming up to 900 DEG C, argon=200sccm, hydrogen=80sccm;Annealing process: 13min, maintains same temperature 900 DEG C, argon=200sccm, hydrogen=80sccm; Growth course: 25min, maintains same temperature 900 DEG C, methane: hydrogen: argon=5:80:200sccm; Growth closes methane after terminating, and opens fan fast cooling, finally gently takes out the nickel foam of the upper Graphene of growth;
4) by being uniformly coated with the PMMA solution of 1% on the graphene film in square nickel foam, in vacuum drying oven, heating 35min, heating-up temperature is 125 DEG C. Being put into by the sample scribbling PMMA in the 3MHCl of constant temperature 80 DEG C, etch period is 18hour again. After etching, sample is positioned in deionized water and invades bubble 6min, repeat 3 times. Again three-dimensional graphene foam is placed in vacuum drying oven, in a low voltage state, is warming up to 70 DEG C, keep 40min. In this dry run, every 10min opens vacuum pump, pumps the water vapour in vacuum drying oven. Etched nickel but do not removed the three-dimensional graphene foam of PMMA protecting film.
5) will etch nickel but do not remove the three-dimensional graphene foam of PMMA protecting film and put in tube furnace, in low pressure, 25sccm hydrogen, 450 DEG C of heating, 110min. After having annealed, PMMA protecting film can be removed, obtain the three-dimensional graphene foam dried.
6) dry three-dimensional graphene foam is positioned over the compound carrying out cadmium sulfide nanoparticles in CVD system vacuum cavity, it is thus achieved that the three-dimensional graphene foam of composite Nano cadmium sulfide. In recombination process, the growth conditions of cadmium sulfide nanoparticles is low-pressure growth, and source temperature is 700 DEG C, and passing into hydrogen flowing quantity is 30sccm. Cadmium sulfide powder by 99.999% is positioned over source position, then three-dimensional graphene foam is positioned over distance sources 0.3dm place, and growth time is 3min.
7) three-dimensional graphene foam composite Nano cadmium sulfide is fixed in the transparent substrates 2 that quartz is base material, connects on three-dimensional graphene foam composite Nano cadmium sulfide surface draw circuit 3 by conductive silver paste 4, connect that to draw circuit 3 be copper cash. Use AB glue to be connect on three-dimensional graphene foam composite Nano cadmium sulfide surface to draw the part of circuit 3, conductive silver paste 4 place and connecing and draw circuit 3 and contact the part covering of transparent substrates 2. Finally giving the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide, the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide is as shown in Figure 6.
Implement row 7
The preparation method of the photoelectric chemical electrode of a kind of three-dimensional graphene foam composite Nano cadmium sulfide is as it is shown in figure 1, specifically comprise the following steps that
1) nickel foam as shown in Figure 2 is tailored into the square of 1cm*1cm.
2) square nickel foam is respectively placed in acetone, ethanol, deionized water for ultrasonic cleaning 10min, dries up with nitrogen standby.
3) dried square nickel foam is positioned in CVD system vacuum cavity and carries out graphene film growth, it is thus achieved that graphene film. The growth conditions of graphene film is growth at atmosphere, growth temperature is 1100 DEG C, pass into the mixing gas (specific proportions argon: hydrogen: methane=200:80:5sccm) of argon, hydrogen and methane, growth time is 30min, finally gives the graphene film in square nickel foam.
Graphene growth specifically includes: heats up, anneal, grow three steps; Temperature-rise period: 60min is warming up to 1100 DEG C, argon=200sccm, hydrogen=80sccm; Annealing process: 15min, maintains same temperature 1100 DEG C, argon=200sccm, hydrogen=80sccm;Growth course: 30min, maintains same temperature 1100 DEG C, methane: hydrogen: argon=5:80:200sccm; Growth closes methane after terminating, and opens fan fast cooling, finally gently takes out the nickel foam of the upper Graphene of growth;
4) by being uniformly coated with the PMMA solution of 1.5% on the graphene film in square nickel foam, in vacuum drying oven, heating 60min, heating-up temperature is 150 DEG C. Being put into by the sample scribbling PMMA in the 5MHCl of constant temperature 80 DEG C, etch period is 24hour again. After etching, sample is positioned in deionized water and invades bubble 10min, repeat 3 times. Again three-dimensional graphene foam is placed in vacuum drying oven, in a low voltage state, is warming up to 100 DEG C, keep 40min. In this dry run, every 10min opens vacuum pump, pumps the water vapour in vacuum drying oven. Etched nickel but do not removed the three-dimensional graphene foam of PMMA protecting film.
5) will etch nickel but do not remove the three-dimensional graphene foam of PMMA protecting film and put in tube furnace, in low pressure, 40sccm hydrogen, 600 DEG C of heating, 120min. After having annealed, PMMA protecting film can be removed, obtain the three-dimensional graphene foam dried.
6) dry three-dimensional graphene foam is positioned over the compound carrying out cadmium sulfide nanoparticles in CVD system vacuum cavity, it is thus achieved that the three-dimensional graphene foam of composite Nano cadmium sulfide. In recombination process, the growth conditions of cadmium sulfide nanoparticles is low-pressure growth, and source temperature is 800 DEG C, and passing into hydrogen flowing quantity is 30sccm. Cadmium sulfide powder by 99.999% is positioned over source position, then three-dimensional graphene foam is positioned over distance sources 1dm place, and growth time is 10min.
7) three-dimensional graphene foam composite Nano cadmium sulfide is fixed in the transparent substrates 2 that glass is base material, connects on three-dimensional graphene foam composite Nano cadmium sulfide surface draw circuit 3 by conductive silver paste 4, connect that to draw circuit 3 be copper cash. Use AB glue to be connect on three-dimensional graphene foam composite Nano cadmium sulfide surface to draw the part of circuit 3, conductive silver paste 4 place and connecing and draw circuit 3 and contact the part covering of transparent substrates 2. Finally giving the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide, the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide is as shown in Figure 6.
Claims (1)
1. the preparation method of a three-dimensional graphene foam composite Nano cadmium sulfide photoelectric chemical electrode, it is characterised in that the method step is as follows:
Step one: grow Graphene in nickel foam;
By chemical vapour deposition technique, deposited graphite alkene in nickel foam; Graphene growth condition is growth at atmosphere, growth temperature is 700～1100 DEG C, pass into the gaseous mixture of argon, hydrogen and three kinds of gases of methane, the mixed proportion of these three gas is argon: hydrogen: methane=200:80:5, growth time controls, at 10～30min, to finally give the three-dimensional grapheme not etching nickel foam;
Graphene growth specifically includes: heats up, anneal, grow three steps; Temperature-rise period: 60min is warming up to 700～1100 DEG C, argon=200sccm, hydrogen=80sccm; Annealing process: 10～15min, maintains same temperature, argon=200sccm, hydrogen=80sccm; Growth course: 10～30min, maintains same temperature, methane: hydrogen: argon=5:80:200sccm; Growth closes methane after terminating, and opens fan fast cooling, finally gently takes out the nickel foam of the upper Graphene of growth;
Step 2: etched nickel but do not removed the three-dimensional graphene foam of PMMA protecting film;
By being uniformly coated with the PMMA solution of 0.1～1.5% on the graphene film in square nickel foam, in vacuum drying oven, heating 10～60min, heating-up temperature is 80～150 DEG C; Being put into by the sample scribbling PMMA in 1～5MHCl of constant temperature 80 DEG C, etch period is 6～24hour again; After etching, sample is positioned in deionized water and invades bubble 5～10min, repeat 3 times; Again three-dimensional graphene foam is placed in vacuum drying oven, in a low voltage state, is warming up to 60～100 DEG C, keep 40min; In this dry run, every 10min opens vacuum pump, pumps the water vapour in vacuum drying oven; Finally give the three-dimensional graphene foam etching nickel but do not remove PMMA protecting film;
Step 3: obtain removing the dry three-dimensional graphene foam of PMMA protecting film
Will etch nickel but do not remove the three-dimensional graphene foam of PMMA protecting film and put in tube furnace, in low pressure, in 10～40sccm hydrogen, 400～600 DEG C of heating, 30～120min; After having annealed, PMMA protecting film can be removed, obtain the three-dimensional graphene foam dried;
Step 4: obtain three-dimensional graphene foam composite Nano cadmium sulfide;
By chemical vapour deposition technique, three-dimensional graphene foam deposits Nano cadmium sulphide; The condition of deposition Nano cadmium sulphide is low-pressure growth, passes into hydrogen, and cadmium sulfide source is the cadmium sulfide powder of 99.999%, and cadmium sulfide source temperature is 400～800 DEG C; Three-dimensional graphene foam is being placed from 0.1～1dm place, source; Growth time is 1～10mins; Finally give three-dimensional graphene foam composite Nano cadmium sulfide;
Step 5: obtain the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide;
Being fixed in transparent substrates (2) by three-dimensional graphene foam composite Nano cadmium sulfide, transparent substrates is PET, glass or the quartzy transparent material for base material; Connect by conductive silver paste (4) on three-dimensional graphene foam composite Nano cadmium sulfide surface and draw circuit (3), connect and draw circuit (3) for copper cash or silver wire; Use AB glue to be connect on three-dimensional graphene foam composite Nano cadmium sulfide surface draw the part of circuit (3), conductive silver paste (4) place and connect the part covering drawing circuit (3) contact transparent substrates (2); Finally give the photoelectric chemical electrode of three-dimensional graphene foam composite Nano cadmium sulfide.
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