CN110203964A - A kind of preparation of induced with laser metal sulfide/three-dimensional porous graphene complex light electrode - Google Patents
A kind of preparation of induced with laser metal sulfide/three-dimensional porous graphene complex light electrode Download PDFInfo
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- CN110203964A CN110203964A CN201910367631.XA CN201910367631A CN110203964A CN 110203964 A CN110203964 A CN 110203964A CN 201910367631 A CN201910367631 A CN 201910367631A CN 110203964 A CN110203964 A CN 110203964A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
- C01G11/02—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/21—Sulfides
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- G—PHYSICS
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Abstract
A kind of preparation method of induced with laser metal sulfide/three-dimensional porous graphene complex light electrode, it uses induced with laser preparation method.Metal ion match is dissolved in polysulfones-like polymer solution, obtained viscosity solution is spin-coated to indium tin oxide-coated glass surface, it is heated make solvent volatilize after, indium tin oxide-coated glass surface formed metal ion mixing polysulfones-like polymer film, utilize CO2Laser scanning metal ion mixing polysulfones-like polymer film surface prepares to form metal sulfide/three-dimensional porous graphene complex light electrode.
Description
Technical field
It is in situ, synchronous that the present invention relates to a kind of metal sulfide/three-dimensional porous graphene complex light electrode induced with laser
Novel preparation method.
Background technique
Photic electrochemical sensing is a kind of analytical technology of great development prospect, due to its excitaton source (light) and output signal
The form of energy of (electric current) is different, can greatly reduce background signal and it is significant improve sensitivity, led in analytical chemistry
Domain causes extensive concern.In the past ten years, researchers have been devoted to make using various metal sulfides
Photic electrochemical sensing platform is constructed for the light active material of optoelectronic pole, for example, cadmium sulfide, vulcanized lead, bismuth sulfide and silver sulfide
Deng.To further increase photoelectric current transfer efficiency, researcher is by metal sulfide and binary metal oxide semiconductor, ternary
Metal-oxide semiconductor (MOS), carbonitride combine, and are prepared for various metals sulfide composite material, greatly improve based on gold
Belong to the sensitivity of the photic electrochemical sensor of sulfide.Graphene transmits carrier as a kind of excellent carrier, extensive
For constructing the heterojunction composite of metal sulfide, the compound of electron-hole in metal sulfide can be effectively suppressed, thus
Promote its photoelectric current transformation efficiency.However, conventional metals sulfide/graphene complex light electrode preparation method generally comprise it is all
Mostly cumbersome tediously long step, such as: the preparation of graphene, the preparation of metal sulfide, the assembling of graphene and metal sulfide,
Modification and protection etc. of the metal sulfide/graphene composite material in electrode surface.Therefore, this patent is directed to this problem, hair
A kind of novel metal sulfide/three-dimensional porous graphene complex light electrode novel preparation method has been opened up, polysulfones-like polymer is utilized
It is used as carbon source and sulphur source simultaneously, the metal complex doped polysulfones-like polymer film on indium tin oxide-coated glass surface is in situ,
It synchronizes and is converted into metal sulfide/three-dimensional porous graphene composite material, being formed has answering for excellent photic chemical property
Light combination electrode.This method is simple, stable, versatile, and can realize and be prepared on a large scale.
Summary of the invention
The object of the present invention is to provide a kind of induced with laser metal sulfides based on polysulfones-like polymer film/three-dimensional porous
Graphene complex light electrode preparation method.
Technical solution of the present invention is as follows
A kind of preparation method of induced with laser metal sulfide/three-dimensional porous graphene complex light electrode, as shown in Figure 1, it is adopted
With induced with laser preparation method.Metal ion match is dissolved in polysulfones-like polymer solution, the viscosity solution that will be obtained
Be spin-coated to indium tin oxide-coated glass surface, it is heated so that solvent is volatilized after, form metal on indium tin oxide-coated glass surface
The polysulfones-like polymer film of ion doping, utilizes CO2Laser scanning metal ion mixing polysulfones-like polymer film surface, that is, prepare
Form metal sulfide/three-dimensional porous graphene complex light electrode.
Above-mentioned metal ion match is acetylacetone,2,4-pentanedione cadmium, porphyrin cadmium, cadmium acetate, acetylacetone,2,4-pentanedione lead, porphyrin lead, acetic acid
Lead.
Above-mentioned polysulfones-like polymer is polysulfones, polyether sulfone, polyphenylsulfone.
Above-mentioned induced with laser metal sulfide/three-dimensional porous graphene complex light electrode preparation method, it is by following step
Rapid composition:
0.8-1.2 g metal ion match is added in 20-30 mL n,N-Dimethylformamide solution by step 1., magnetic
Power stirring, is allowed to be completely dissolved；
Step 2., which divides 2.0-3.0 g polysulfones-like polymer 3-5 times (time interval is 20-30 minutes), to be added to obtained by step 1
It is lasting to stir in solution, form the metal ion polysulfones-like polymer solution with certain viscosity；
The metal ion polysulfones-like polymer solution that step 2 synthesizes is spin-coated to the clean tin indium oxide of processing and led by step 3.
Electric glass surface forms uniform metal ion polysulfones-like polymer solution film on indium tin oxide-coated glass surface, rotation
Painting revolving speed is 2000-3000 r/min, and spin-coating time is 80-100 s；
Step 4. exists the film modified indium tin oxide-coated glass of metal ion polysulfones-like polymer solution that step 3 obtains
So that solvent volatilizees gold is prepared on indium tin oxide-coated glass surface in vacuum heat-preserving 1-3 h at a temperature of 75-100 DEG C
Belong to ion doping polysulfones-like polymer film；
The metal ion mixing polysulfones-like polymer film that step 4 obtains is cooled to room temperature by step 5., is put into CO2Laser cutting
Engraving machine workbench, utilizes CO2Laser scanning metal ion mixing polysulfones-like polymer film surface, by tin indium oxide conduction glass
The metal ion mixing polysulfones-like polymer film on glass surface is direct, converted in-situ is metal sulfide/three-dimensional porous graphene.Swash
It is as follows that light carves parameter: laser power is 4.0-4.8 w, and laser engraving speed is 166-250 mm/s, laser engraving resolution ratio
For 600-1200, laser defocus distance is 0.2-0.4 cm.
The above-mentioned induced with laser metal sulfide based on polysulfones-like polymer film/three-dimensional porous graphene complex light electrode system
Standby principle is as follows:
During laser engraving, due to CO2The photo-thermal effect of laser, can be by metal ion mixing polysulfones-like polymer film
Local Instantaneous temperature is increased to close to 3000 DEG C, by sp in polysulfones-like polymer film3Hydridization carbon is transformed into sp2Hydridization carbon, finally
Keep the polysulfones-like polymer film containing a large amount of benzene ring structures high-graphitized, generates graphene.Violent graphitizing process is adjoint
The release of the gases such as water vapour and nitrogen, formed porous structure.Meanwhile the element sulphur in polysulfones-like polymer is in metal ion
Composite nano metal sulfide particle is formed by carbon thermal reduction under the conditions of existing, is uniformly attached on three-dimensional porous graphene, thus
Preparation forms metal sulfide/three-dimensional porous graphene complex light electrode.
Compared with prior art, the present invention having the following characteristics that
In situ, synchronous system that the present invention provides a kind of metal sulfide/three-dimensional porous graphene complex light electrode induced with laser
Standby new method has a characteristic that compared with traditional metal sulfide/graphene composite material preparation method
(1) induced with laser novel preparation method of the present invention, can be direct, in situ, same on indium tin oxide-coated glass surface
Step generates metal sulfide/three-dimensional porous graphene composite photoelectric material, quick, electrode area simple with operating procedure
Controllable precise, versatile feature, and can realize and be prepared on a large scale；
(2) induced with laser of the present invention prepares metal sulfide/three-dimensional porous graphene complex light electrode stability height,
It is reproducible, reusable 30 times or more, and can at room temperature stable storage 10 months or more.
Detailed description of the invention
Fig. 1 metal sulfide/three-dimensional porous graphene complex light electrode production process schematic diagram.
Specific embodiment
The preparation of 1. cadmium sulfide of embodiment/three-dimensional porous graphene complex light electrode:
The preparation sulfolane solution of polyethers containing cadmium ion: 0.8 g acetylacetone,2,4-pentanedione cadmium is added to 20 mL n,N-Dimethylformamide, magnetic force
Stirring, is allowed to be completely dissolved, and then 2.5 g polyether sulfones point 5 times (time interval is 2 hours) are added, lasting to stir, and forms tool
There is the sulfolane solution of polyethers containing cadmium ion of certain viscosity；
Preparation poly (ether sulfone) film containing cadmium ion modifies indium tin oxide-coated glass: the above-mentioned sulfolane solution of polyethers containing cadmium ion is spin-coated to place
Clean indium tin oxide-coated glass surface is managed, spin coating revolving speed is 1000 r/min, and spin-coating time is 60 s, in indium oxide
Tin conductive glass surface forms the uniform solution film of polyether sulfone containing cadmium ion, and obtained polyether sulfone containing cadmium ion solution film is existed
2 h of vacuum heat-preserving, makes solvent volatilize at a temperature of 100 DEG C, i.e., cadmium ion is made on indium tin oxide-coated glass surface and adulterates polyethers
Sulfone film；
Induced with laser prepares cadmium sulfide/three-dimensional porous graphene complex light electrode: obtained cadmium ion doping poly (ether sulfone) film is repaired
Decorations indium tin oxide-coated glass is cooled to room temperature, and is put into CO2Laser cutting engraving machine workbench, utilizes CO2Laser scanning cadmium from
Son doping poly (ether sulfone) film surface, by the cadmium ion doping poly (ether sulfone) film on indium tin oxide-coated glass surface, direct, converted in-situ is
Cadmium sulfide/three-dimensional porous graphene complex light electrode.Laser engraving parameter is as follows: laser power is 4.0 W, laser engraving speed
For 166 mm/s, laser engraving resolution ratio is 1200, and laser defocus distance is 0.3 cm.
The preparation of 2. vulcanized lead of embodiment/three-dimensional porous graphene complex light electrode:
The preparation solution of polysulfones containing lead ion: 1.0 g acetylacetone,2,4-pentanedione lead are added to 20 mL n,N-Dimethylformamide, magnetic force stirs
It mixes, is allowed to be completely dissolved, then 2.5 g polysulfones point 5 times (time interval is 2 hours) are added, lasting to stir, being formed has one
Determine the solution of polysulfones containing lead ion of viscosity；
Preparation PS membrane containing lead ion modifies indium tin oxide-coated glass: it is dry that the above-mentioned solution of polysulfones containing lead ion is spin-coated to processing
Net indium tin oxide-coated glass surface, spin coating revolving speed are 800 r/min, and spin-coating time is 80 s, in tin indium oxide conduction
Glass surface forms the uniform solution film of polysulfones containing lead ion, by obtained polysulfones containing lead ion solution film at a temperature of 100 DEG C
2 h of vacuum heat-preserving, makes solvent volatilize, i.e., lead ion is made on indium tin oxide-coated glass surface and adulterates PS membrane；
Induced with laser prepares the three-dimensional porous graphene complex light electrode of leaded sulphur: obtained lead ion doping PS membrane is cooled to
Room temperature is put into CO2Laser cutting engraving machine workbench, utilizes CO2Laser scanning lead ion adulterates polysulfones film surface, will aoxidize
The lead ion doping PS membrane of indium tin conductive glass surface is direct, converted in-situ is vulcanized lead/three-dimensional porous graphene complex light
Electrode.Laser engraving parameter is as follows: laser power is 4.5 W, and laser engraving speed is 196 mm/s, and laser engraving resolution ratio is
1200, laser defocus distance is 0.3 cm.
Claims (6)
1. a kind of induced with laser metal sulfide/three-dimensional porous graphene complex light electrode preparation method, it is lured using laser
Lead preparation method.
2. metal ion match is dissolved in polysulfones-like polymer solution, obtained viscosity solution is spin-coated to tin indium oxide
Conductive glass surface, it is heated make solvent volatilize after, indium tin oxide-coated glass surface formed metal ion mixing polysulfones
Quasi polymer film, utilizes CO2Laser scanning metal ion mixing polysulfones-like polymer film surface prepares to form metal vulcanization
Object/three-dimensional porous graphene complex light electrode.
3. induced with laser metal sulfide according to claim 1/three-dimensional porous graphene complex light electrode preparation side
Method, it is characterized in that: the metal ion match be acetylacetone,2,4-pentanedione cadmium, porphyrin cadmium, cadmium acetate, acetylacetone,2,4-pentanedione lead, porphyrin lead,
Lead acetate.
4. the polysulfones-like polymer is polysulfones, polyether sulfone and polyphenylsulfone.
5. induced with laser metal sulfide according to claim 1/three-dimensional porous graphene complex light electrode preparation side
Method, it is characterized in that it is made of the following steps:
0.8-1.2 g metal ion match is added in 20-30 mL n,N-Dimethylformamide solution by step 1., magnetic
Power stirring, is allowed to be completely dissolved；
Step 2., which divides 2.0-3.0 g polysulfones-like polymer 3-5 times (time interval is 20-30 minutes), to be added to obtained by step 1
It is lasting to stir in solution, form the metal ion polysulfones-like polymer solution with certain viscosity；
The metal ion polysulfones-like polymer solution that step 2 synthesizes is spin-coated to the clean tin indium oxide of processing and led by step 3.
Electric glass surface forms uniform metal ion polysulfones-like polymer solution film on indium tin oxide-coated glass surface, rotation
Painting revolving speed is 2000-3000 r/min, and spin-coating time is 80-100 s；
Step 4. exists the film modified indium tin oxide-coated glass of metal ion polysulfones-like polymer solution that step 3 obtains
So that solvent volatilizees gold is prepared on indium tin oxide-coated glass surface in vacuum heat-preserving 1-3 h at a temperature of 75-100 DEG C
Belong to ion doping polysulfones-like polymer film；
The metal ion mixing polysulfones-like polymer film that step 4 obtains is cooled to room temperature by step 5., is put into CO2Laser cutting carving
Quarter machine workbench, utilize CO2Laser scanning metal ion mixing polysulfones-like polymer film surface, by indium tin oxide-coated glass
The metal ion mixing polysulfones-like polymer film on surface is direct, converted in-situ is metal sulfide/three-dimensional porous graphene.
6. induced with laser metal sulfide according to claim 1/three-dimensional porous graphene complex light electrode preparation side
Method, it is characterized in that: laser power is 4.0-4.8 w, laser engraving speed is 166-250 mm/s, and laser engraving resolution ratio is
600-1200, laser defocus distance are 0.2-0.4 cm.
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| CN115420393A (en) * | 2022-09-06 | 2022-12-02 | 河北工业大学 | Preparation method of gas-temperature sensor |
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