CN110354904A - A kind of Polyglycolic acid fibre-indium sulfide zinc compound film electrode and preparation method thereof - Google Patents
A kind of Polyglycolic acid fibre-indium sulfide zinc compound film electrode and preparation method thereof Download PDFInfo
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- CN110354904A CN110354904A CN201910672960.5A CN201910672960A CN110354904A CN 110354904 A CN110354904 A CN 110354904A CN 201910672960 A CN201910672960 A CN 201910672960A CN 110354904 A CN110354904 A CN 110354904A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 229920000954 Polyglycolide Polymers 0.000 title claims abstract description 22
- 229910052738 indium Inorganic materials 0.000 title claims abstract description 22
- 239000004633 polyglycolic acid Substances 0.000 title claims abstract description 22
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000010936 titanium Substances 0.000 claims abstract description 68
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 68
- 239000002243 precursor Substances 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000008367 deionised water Substances 0.000 claims abstract description 31
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 30
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000004070 electrodeposition Methods 0.000 claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 239000006193 liquid solution Substances 0.000 claims abstract description 17
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 15
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 15
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 14
- 229910052709 silver Inorganic materials 0.000 claims abstract description 14
- 239000004332 silver Substances 0.000 claims abstract description 14
- 239000003792 electrolyte Substances 0.000 claims abstract description 13
- 239000011261 inert gas Substances 0.000 claims abstract description 13
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 claims abstract description 13
- 239000012528 membrane Substances 0.000 claims abstract description 8
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 8
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 8
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 31
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 18
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 16
- 238000006116 polymerization reaction Methods 0.000 claims description 15
- 238000000137 annealing Methods 0.000 claims description 14
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 239000000835 fiber Substances 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 9
- 235000005074 zinc chloride Nutrition 0.000 claims description 9
- 239000011592 zinc chloride Substances 0.000 claims description 9
- 239000001103 potassium chloride Substances 0.000 claims description 8
- 235000011164 potassium chloride Nutrition 0.000 claims description 8
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 8
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 150000001805 chlorine compounds Chemical class 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 12
- 239000000463 material Substances 0.000 description 19
- 230000006872 improvement Effects 0.000 description 9
- 238000001035 drying Methods 0.000 description 8
- 239000000178 monomer Substances 0.000 description 8
- 238000002604 ultrasonography Methods 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 230000005518 electrochemistry Effects 0.000 description 6
- 238000005498 polishing Methods 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 229920000123 polythiophene Polymers 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- YYKKIWDAYRDHBY-UHFFFAOYSA-N [In]=S.[Zn] Chemical class [In]=S.[Zn] YYKKIWDAYRDHBY-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- YMMGRPLNZPTZBS-UHFFFAOYSA-N 2,3-dihydrothieno[2,3-b][1,4]dioxine Chemical compound O1CCOC2=C1C=CS2 YMMGRPLNZPTZBS-UHFFFAOYSA-N 0.000 description 1
- 235000010894 Artemisia argyi Nutrition 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 244000030166 artemisia Species 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 210000004508 polar body Anatomy 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
-
- B01J35/33—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
Abstract
The invention discloses a kind of Polyglycolic acid fibre-indium sulfide zinc compound film electrodes and preparation method thereof, comprising the following steps: step 1, in three-electrode system, using titanium sheet as working electrode, platinized platinum is to electrode, and silver/silver chlorate is reference electrode；Three-electrode system is placed in synthesis ZnIn2S4Precursor solution in, by electrochemical deposition, synthesize ZnIn in titanium sheet substrate2S4Precursor film；Annealed technique obtains ZnIn under atmosphere of inert gases2S4Membrane electrode；Step 2, ethene dioxythiophene is dissolved in deionized water, sodium sulphate is added as electrolyte, prepares and obtains polybenzazole precursor liquid solution；Step 3, it by step 1 treated three-electrode system, is placed in the polybenzazole precursor liquid solution of step 2 acquisition, is polymerize；Step 4, step 3 treated working electrode is cleaned and dried, and obtains Polyglycolic acid fibre-indium sulfide zinc compound film electrode.This invention removes powdered ZnIn2S4The disadvantages of catalyst is easily assembled, hardly possible recycles.
Description
Technical field
The invention belongs to photocatalysis and photo-electrocatalytic technology fields, and in particular to a kind of Polyglycolic acid fibre-indium sulfide
Zinc (PEDOT-ZnIn2S4) compound film electrode and preparation method thereof.
Background technique
Photo-electrocatalytic technology is by catalyst using photon energy, and many chemistry for needing to occur under harsh conditions are anti-
The advanced technology reacted under mild environment should be converted into.The ternary of a variety of effective use visible lights has been developed at present
Metal oxide/sulfide, stability are good, it is seen that higher activity is shown under light.Wherein ZnIn2S4With about 2.2eV's
Band gap, photo-catalysis capability are relatively strong and have good charge storage, pyroelectric effect and electrochemical properties, in the drop of pollutant
Solution aspect has very high application value.But for individual ZnIn2S4Catalyst is primarily present problem in terms of following two: (1)
Powdered ZnIn2S4Catalyst is difficult to separate from reaction system, recycle.(2) individual ZnIn2S4Catalyst is visible
The light induced electron generated under light and hole random motion, it is easily compound, lead to invalid excitation, so that quantum efficiency under visible light
It is low.Therefore, in order to efficiently use ZnIn2S4Catalyst need to be modified it.
Summary of the invention
The purpose of the present invention is to provide a kind of Polyglycolic acid fibre-indium sulfide zinc compound film electrode and its preparation sides
Method, to solve above-mentioned one or more technical problems.
In order to achieve the above objectives, the invention adopts the following technical scheme:
A kind of Polyglycolic acid fibre of the invention-indium sulfide zinc compound film electrode preparation method, comprising the following steps:
Step 1, in three-electrode system, using titanium sheet as working electrode, platinized platinum is to electrode, and silver/silver chlorate is reference
Electrode；Three-electrode system is placed in synthesis ZnIn2S4Precursor solution in, by electrochemical deposition, synthesized in titanium sheet substrate
ZnIn2S4Precursor film；Annealed technique obtains ZnIn under atmosphere of inert gases2S4Membrane electrode；
Step 2, ethene dioxythiophene is dissolved in deionized water, sodium sulphate is added as electrolyte, preparation is gathered
Close object precursor solution；
Step 3, it by step 1 treated three-electrode system, is placed in the polybenzazole precursor liquid solution of step 2 acquisition, into
Row polymerization；Wherein, after polymerizeing preset time, working electrode is overturn, by working electrode another side towards to electrode；
Step 4, treated that working electrode is rinsed with dehydrated alcohol for step 3, then is rinsed well with deionized water, dry,
Obtain Polyglycolic acid fibre-indium sulfide zinc compound film electrode.
A further improvement of the present invention is that further including pre-processing in step 1 to titanium sheet, pretreated step is specific
Include:
(1) titanium sheet is mechanically polished；
(2) step (1) treated titanium sheet is ultrasonically treated with acetone, is rinsed well with deionized water；
(3) step (2) treated titanium sheet is ultrasonically treated with isopropanol, is rinsed well with deionized water；
(4) step (3) treated titanium sheet is dry in nitrogen stream.
A further improvement of the present invention is that in step 1 further include: prepare zinc chloride, four water inidum chlorides and thiosulfuric acid
The aqueous solution of sodium is added potassium chloride as electrolyte, obtains synthesis ZnIn2S4Precursor solution；Wherein, excessive in S content
In the case of, with molar ratio computing, Zn:In=1:1.25.
A further improvement of the present invention is that in step 1, the synthesis ZnIn of acquisition2S4Precursor solution after, by solution
PH is adjusted to 2~2.5.
A further improvement of the present invention is that electrochemical deposition current potential is set as -1.1v~-1.3v, electrochemistry in step 1
Sedimentation time is set as 10min~20min.
A further improvement of the present invention is that specifically including under atmosphere of inert gases in step 1: inert gas flow is
400mL/min~600mL/min；
Annealing process specifically includes: being heated to the rate of 5 DEG C/min 150 DEG C~500 DEG C of annealing temperature from room temperature, stops
Staying the time is 1h.
A further improvement of the present invention is that every 100mL deionized water corresponds to the 3 of 0.072g~0.284g in step 2,
4- ethene dioxythiophene, the sodium sulphate of corresponding 0.710g.
A further improvement of the present invention is that the polybenzazole precursor liquid solution that step 2 is prepared, is added potassium chloride as electrolysis
Matter is added hydrochloric acid for pH value of solution and is adjusted to 2~2.5.
A further improvement of the present invention is that in polybenzazole precursor liquid solution, EDOT concentration be 0.005M, 0.01M or
0.02M, the polymerization time being corresponding in turn to are 1h, 2h or 3h.
A kind of Polyglycolic acid fibre of the invention-indium sulfide zinc compound film electrode, using the above-mentioned preparation side of the present invention
Method preparation；
ZnIn has been sequentially depositing in titanium substrate2S4Film layer and PEDOT film layer.
Compared with prior art, the invention has the following advantages:
The present invention is prepared by two-step method, comprising: the first step, the electrochemistry formated ZnIn in titanium substrate2S4Membrane electrode.
Second step, the electrode material synthesized using this are loaded one layer of PEDOT film by electro-deposition and obtain PEDOT-ZnIn as substrate2S4It is multiple
Close membrane electrode.Wherein, electrodeposition process is a kind of low temperature, antivacuum coating technique, can be realized low cost, large-area coating film.
The method is simple, and operation is easy, and combination electrode is easy to obtained.
Specifically, selecting titanium sheet as base material, powdered ZnIn is avoided2S4The drawbacks of catalyst difficulty recycles, while titanium
Piece has good conductive property.It selects PEDOT to be modified indium sulfide zinc electrode, because it is with low oxidizing potential, fits
Suitable band gap (Eg~1.6eV), and pi-conjugated poly- thiophene of the PEDOT in luminescent material frequently as hole injection layer, in structure
Pheno backbone provides channel for the transmission in hole, with ZnIn2S4Photohole can effectively be transmitted by combining, inhibit light induced electron and
Hole it is compound the advantages that, improve ZnIn2S4Catalyst is fixed on the problems such as catalytic efficiency is not high on base material.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below to embodiment or existing
Attached drawing needed in technical description does simple introduction；It should be evident that the accompanying drawings in the following description is of the invention
Some embodiments to those skilled in the art without creative efforts, can also be according to this
A little attached drawings obtain other attached drawings.
Fig. 1 is a kind of Polyglycolic acid fibre-indium sulfide zinc compound film electrode structural schematic diagram of the embodiment of the present invention；
In figure, 1, titanium substrate；2,ZnIn2S4Film layer；3, PEDOT film layer.
Specific embodiment
To keep the purpose, technical effect and technical solution of the embodiment of the present invention clearer, implement below with reference to the present invention
Attached drawing in example, technical scheme in the embodiment of the invention is clearly and completely described；Obviously, described embodiment
It is a part of the embodiment of the present invention.Based on embodiment disclosed by the invention, those of ordinary skill in the art are not making creation
Property labour under the premise of other embodiments obtained, all should belong to the scope of protection of the invention.
Referring to Fig. 1, a kind of Polyglycolic acid fibre of the embodiment of the present invention-indium sulfide zinc compound film electrode；It is prepared
Method specifically includes the following steps:
Step 1, use titanium sheet as working electrode in three-electrode system, platinized platinum is to electrode, and silver/silver chlorate is reference
Three-electrode system is placed in synthesis ZnIn by electrode2S4Precursor solution in, by electrochemical deposition, synthesized in titanium substrate
ZnIn2S4Precursor film, and annealed technique obtains ZnIn under atmosphere of inert gases2S4Membrane electrode.
Step 2, using this electrode as working electrode, platinized platinum, silver/silver chlorate are respectively to constitute three electricity to electrode and reference electrode
Polar body system is placed in EDOT containing a certain concentration (ethylenedioxy thiophene) monomer solution, advanced optimizes under best polymerization time
EDOT precursor concentration is to obtain PEDOT-ZnIn2S4Combination electrode.
Step 1 specifically includes:
Step 1.1, titanium sheet is pre-processed, specific steps include:
(1) titanium sheet is mechanically polished；
(2) it by step (1) treated titanium sheet acetone ultrasound 15min, is rinsed well with deionized water；
(3) it by step (2) treated titanium sheet isopropanol ultrasound 15min, is rinsed well with deionized water；
(4) by step (3) treated titanium sheet drying for standby in nitrogen stream.
Step 1.2, the aqueous solution of zinc chloride, four water inidum chlorides and sodium thiosulfate is prepared, precursor solution is obtained.
Step 1.2 specifically includes: zinc chloride, four water inidum chlorides and sodium thiosulfate is dissolved in deionized water respectively,
In the excessive situation of sulfur content, Zn/In=1:1.25 (molar ratio).Using 0.1M potassium chloride as electrolyte, by the way that 1.0M salt is added
PH value of solution is adjusted to 2~2.5 by acid.
Step 1.3, ZnIn is synthesized in three-electrode system2S4Precursor film, specific steps include: in three-electrode system
Middle to use titanium sheet as working electrode, platinized platinum is to electrode, and silver/silver chlorate is reference electrode, and three-electrode system is placed in forerunner
In liquid solution (Containing Zinc Chloride, four water inidum chlorides and sodium thiosulfate), using potentiostatic method, under certain predetermined sedimentation potential,
ZnIn is prepared2S4Film is rinsed well after each electro-deposition with deionized water.
Step 1.4, precursor film step 1.3 obtained makes annealing treatment, and obtains optimal crystallization.It specifically includes；It moves back
Fire carries out in quartz ampoule, keeps certain inert gas flow, is heated to 150 DEG C~700 from room temperature with the rate of 5 DEG C/min
DEG C, residence time 1h obtains ZnIn described in step 12S4Membrane electrode.
Step 2 specifically includes:
Step 2.1, the EDOT monomer of certain volume the preparation of polybenzazole precursor liquid solution: is dissolved in 0.05MNa2SO4Electricity
It solves in liquid matter solution, forms the polybenzazole precursor liquid solution that EDOT concentration is respectively 0.005M, 0.01M and 0.02M.
Firstly, EDOT concentration in step 2.1 is fixed on 0.01M, optimize polymerization time 1h, 2h and 3h.When polymerization carries out
When half, i.e. polymerase 10 .5h, 1h, 1.5h, working electrode is overturn, another surface is towards to electrode.
Further, optimize EDOT precursor concentration: 0.005M, 0.01M and 0.02M under the best polymerization time of determination.
Step 2.2, after reaction, working electrode is rinsed well with dehydrated alcohol, to remove extra EDOT monomer, then
It is rinsed well with deionized water.
Further, combination electrode step 2.2 obtained drying for standby at 60 DEG C.
In the present invention, electrodeposition process is a kind of low temperature, antivacuum coating technique, can be realized low cost, large area plating
Film.The method is simple, and operation is easy, and combination electrode is easy to obtained.It selects titanium sheet as base material, avoids powdered ZnIn2S4
The drawbacks of catalyst difficulty recycles, while titanium sheet has good conductive property.PEDOT is selected to change indium sulfide zinc electrode
Property, because its with low oxidizing potential, suitable band gap (Eg~1.6eV), and PEDOT in luminescent material frequently as hole
Implanted layer, the pi-conjugated polythiophene backbone in structure provides channel for the transmission in hole, with ZnIn2S4Combining effectively to pass
Defeated photohole, inhibit light induced electron and hole it is compound the advantages that, improve ZnIn2S4Catalyst is fixed on base material
The problems such as catalytic efficiency is not high.
Embodiment one
Electrochemistry formated PEDOT-ZnIn in a kind of titanium substrate of the embodiment of the present invention2S4The preparation of composite photoelectric catalysis material
Specific implementation method include:
(1) base material (titanium sheet) pre-processes.
Step 1, preferred dimension be 20 × 30 × 2 (width x length × height) mm titanium sheet as base material, and to titanium sheet into
Row mechanical polishing is until mirror surface occurs；
Step 2, the acetone ultrasound 15min of the titanium sheet after polishing, deionized water are rinsed well；
Step 3, by step 2 treated titanium sheet isopropanol ultrasound 15min, deionized water is rinsed well；
Step 4, by step 3 treated titanium sheet drying for standby in nitrogen stream.
(2) ZnIn is synthesized in titanium substrate2S4Precursor film.
Step 1, at room temperature, 0.0136g zinc chloride, tetra- water inidum chloride of 0.0366g and 0.216g sodium thiosulfate is molten
Solution, using 0.1M potassium chloride as electrolyte, is configured to precursor solution in 100mL deionized water, is 1.0M by the way that concentration is added
PH value of solution is adjusted to 2 by hydrochloric acid drop；
Step 2, in three-electrode system, use titanium sheet for working electrode, platinized platinum is to electrode, and silver/silver chlorate is reference
Three-electrode system is placed in synthesis ZnIn by electrode2S4Precursor solution in, synthesized in titanium substrate by potentiostatic method
ZnIn2S4Film.Electrochemical deposition current potential is set as -1.1v in the process, and the electrochemical deposition time is set as 10min.
Step 3, to the ZnIn obtained after electro-deposition2S4Presoma is made annealing treatment, and optimal crystallization is obtained.Annealing is in stone
Ying Guanzhong is carried out, and precursor film is placed in pipe, is added from room temperature with the rate of 5 DEG C/min by inert gas flow 400mL/min
Heat is to 150 DEG C of annealing temperature, residence time 1h.
(3)PEDOT-ZnIn2S4Combination electrode synthesis
Step 1, by 0.072g3,4- ethene dioxythiophene (EDOT) is dissolved in 100mL deionized water, and 0.710g is added
Sodium sulphate is configured to polybenzazole precursor liquid solution as electrolyte；
Step 2, there is ZnIn with load2S4The titanium sheet of precursor film is working electrode, and silver/silver chlorate and platinized platinum are respectively to join
It is placed in the polybenzazole precursor liquid solution of step 1 preparation than electrode and to electrode composition three-electrode system.Polymerization time is 1h, when
Polymerization carries out half, i.e. when polymerase 10 .5h, working electrode is overturn, by working electrode another side towards to electrode.
Step 3, after reaction, working electrode is rinsed several times with dehydrated alcohol, to remove extra EDOT monomer, then is used
Deionized water is rinsed well.Obtain PEDOT-ZnIn2S4Combination electrode drying for standby at 60 DEG C.
Embodiment two
Electrochemistry formated PEDOT-ZnIn in a kind of titanium substrate of the embodiment of the present invention2S4The preparation of composite photoelectric catalysis material
Specific implementation method include:
(1) base material (titanium sheet) pre-processes.
Step 1, preferred dimension be 20 × 30 × 2 (width x length × height) mm titanium sheet as base material, and to titanium sheet into
Row mechanical polishing is until mirror surface occurs；
Step 2, the acetone ultrasound 15min of the titanium sheet after polishing, deionized water are rinsed well；
Step 3, by step 2 treated titanium sheet isopropanol ultrasound 15min, deionized water is rinsed well；
Step 4, by step 3 treated titanium sheet drying for standby in nitrogen stream.
(2) ZnIn is synthesized in titanium substrate2S4Precursor film.
Step 1, at room temperature, 0.068g zinc chloride, tetra- water inidum chloride of 0.183g and 1.08g sodium thiosulfate are dissolved in
In 100mL deionized water, using 0.1M potassium chloride as electrolyte, it is configured to precursor solution, is 1.0M hydrochloric acid by the way that concentration is added
PH value of solution is adjusted to 2.5 by drop；
Step 2, in three-electrode system, use titanium sheet for working electrode, platinized platinum is to electrode, and silver/silver chlorate is reference
Three-electrode system is placed in synthesis ZnIn by electrode2S4Precursor solution in, synthesized in titanium substrate by potentiostatic method
ZnIn2S4Film.Electrochemical deposition current potential is set as -1.2v in the process, and the electrochemical deposition time is set as 15min.
Step 3, to the ZnIn obtained after electro-deposition2S4Presoma is made annealing treatment, and optimal crystallization is obtained.Annealing is in stone
Ying Guanzhong is carried out, and precursor film is placed in pipe, is added from room temperature with the rate of 5 DEG C/min by inert gas flow 500mL/min
Heat is to 350 DEG C of annealing temperature, residence time 1h.
(3)PEDOT-ZnIn2S4Combination electrode synthesis
Step 1, by 0.142g3,4- ethene dioxythiophene (EDOT) is dissolved in 100mL deionized water, and 0.710g is added
Sodium sulphate is configured to polybenzazole precursor liquid solution as electrolyte；
Step 2, there is ZnIn with load2S4The titanium sheet of precursor film is working electrode, and silver/silver chlorate and platinized platinum are respectively to join
It is placed in the polybenzazole precursor liquid solution of step 1 preparation than electrode and to electrode composition three-electrode system.Polymerization time is 2h, when
Polymerization carries out half, that is, when polymerizeing 1h, working electrode is overturn, by working electrode another side towards to electrode.
Step 3, after reaction, working electrode is rinsed several times with dehydrated alcohol, to remove extra EDOT monomer, then is used
Deionized water is rinsed well.Obtain PEDOT-ZnIn2S4Combination electrode drying for standby at 60 DEG C.
Embodiment three
Electrochemistry formated PEDOT-ZnIn in a kind of titanium substrate of the embodiment of the present invention2S4The preparation of composite photoelectric catalysis material
Specific implementation method include: (1) base material (titanium sheet) pretreatment.
Step 1, preferred dimension be 20 × 30 × 2 (width x length × height) mm titanium sheet as base material, and to titanium sheet into
Row mechanical polishing is until mirror surface occurs；
Step 2, the acetone ultrasound 15min of the titanium sheet after polishing, deionized water are rinsed well；
Step 3, by step 2 treated titanium sheet isopropanol ultrasound 15min, deionized water is rinsed well；
Step 4, by step 3 treated titanium sheet drying for standby in nitrogen stream.
(2) ZnIn is synthesized in titanium substrate2S4Precursor film.
Step 1, at room temperature, 0.136g zinc chloride, tetra- water inidum chloride of 0.366g and 2.16g sodium thiosulfate are dissolved in
In 100mL deionized water, using 0.1M potassium chloride as electrolyte, it is configured to precursor solution, is 1.0M hydrochloric acid by the way that concentration is added
PH value of solution is adjusted to 2.5 by drop；
Step 2, in three-electrode system, use titanium sheet for working electrode, platinized platinum is to electrode, and silver/silver chlorate is reference
Three-electrode system is placed in synthesis ZnIn by electrode2S4Precursor solution in, synthesized in titanium substrate by potentiostatic method
ZnIn2S4Film.Electrochemical deposition current potential is set as -1.3v in the process, and the electrochemical deposition time is set as 20min.
Step 3, to the ZnIn obtained after electro-deposition2S4Presoma is made annealing treatment, and optimal crystallization is obtained.Annealing is in stone
Ying Guanzhong is carried out, and precursor film is placed in pipe, is added from room temperature with the rate of 5 DEG C/min by inert gas flow 600mL/min
Heat is to 500 DEG C of annealing temperature, residence time 1h.
(3)PEDOT-ZnIn2S4Combination electrode synthesis
Step 1, by 0.284g3,4- ethene dioxythiophene (EDOT) is dissolved in 100mL deionized water, and 0.710g is added
Sodium sulphate is configured to polybenzazole precursor liquid solution as electrolyte；
Step 2, there is ZnIn with load2S4The titanium sheet of precursor film is working electrode, and silver/silver chlorate and platinized platinum are respectively to join
It is placed in the polybenzazole precursor liquid solution of step 1 preparation than electrode and to electrode composition three-electrode system.Polymerization time is 3h, when
Polymerization carries out half, that is, when polymerizeing 1.5h, working electrode is overturn, by working electrode another side towards to electrode.
Step 3, after reaction, working electrode is rinsed several times with dehydrated alcohol, to remove extra EDOT monomer, then is had
Deionized water is rinsed well.Obtain PEDOT-ZnIn2S4Combination electrode drying for standby at 60 DEG C.
In conclusion from 1977, Japanese Scientists Hideki Shirakawa (Shirakawa Hideki) and American scientist Chinese mugwort
Bertil Ronnmark Diarmid (Alan G M acdiarmid), Alan's black square (Alan J Heeger) have overthrown " polymer for the first time
It is non-conductive " this concept.Conducting polymer penetrates into rapidly multiple fields.Because its electric conductivity between conductor and insulator it
Between, there is biggish pi-electron conjugated structure, there is metallic character, possess excellent physical and chemical performance such as: high conductivity,
Reversible redox active etc., therefore huge application prospect is shown in electrochemical catalysis field.PEDOT be EDOT (3,
4- ethene dioxythiophene monomer) polymer.With low oxidizing potential, suitable band gap (Eg~1.6eV), doped lower height
Conductivity (> 550S/cm) and light transmission rate (> 80%), good redox active and cycle life, excellent light, heat
And environmental stability.For PEDOT frequently as hole injection layer in luminescent material, the pi-conjugated polythiophene backbone in structure is sky
The transmission in cave provides channel, with ZnIn2S4Photohole can effectively be transmitted by combining, and inhibit the compound of light induced electron and hole.
The invention discloses electrochemistry formated PEDOT-ZnIn in a kind of titanium substrate2S4Composite photoelectric catalysis material and its system
Preparation Method.Preparation process is in two steps: the first step, is used as working electrode using titanium sheet in three-electrode system, platinized platinum for electrode,
Silver/silver chlorate is reference electrode, and three-electrode system is placed in synthesis ZnIn2S4Precursor solution in (include zinc chloride, four water
Inidum chloride and sodium thiosulfate), ZnIn is synthesized by being electrochemically-deposited on titanium-base2S4Precursor film, in atmosphere of inert gases
Under annealed technique obtain ZnIn2S4Membrane electrode.Second step, the electrode synthesized using this as working electrode, silver/silver chloride electrode and
Platinized platinum is respectively reference electrode and is placed in the three-electrode system of electrode containing a certain concentration EDOT (3,4-rthylene dioxythiophene)
In monomer solution, EDOT precursor concentration is advanced optimized under best polymerization time to obtain PEDOT-ZnIn2S4Compound electric
Pole.
The present invention by using PEDOT to the ZnIn being supported in titanium substrate2S4It is modified, eliminates powdered
ZnIn2S4The disadvantages of catalyst is easily assembled, hardly possible recycles.And PEDOT has good electron conduction, has with base electrode
Good adhesive force can be used as electron acceptor, electron donor and photosensitizer.Simultaneously PEDOT in luminescent material also frequently as
Hole injection layer, the pi-conjugated polythiophene backbone in structure provides channel for the transmission in hole, with ZnIn2S4Combining can have
Effect transmission photohole inhibits compound, the improvement ZnIn in light induced electron and hole2S4Catalyst is fixed on base material and is catalyzed
The problems such as inefficient
The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof, although referring to above-described embodiment pair
The present invention is described in detail, those of ordinary skill in the art still can to a specific embodiment of the invention into
Row modification perhaps equivalent replacement these without departing from any modification of spirit and scope of the invention or equivalent replacement, applying
Within pending claims of the invention.
Claims (10)
1. a kind of Polyglycolic acid fibre-indium sulfide zinc compound film electrode preparation method, which is characterized in that including following step
It is rapid:
Step 1, in three-electrode system, using titanium sheet as working electrode, platinized platinum is to electrode, and silver/silver chlorate is reference electrode；
Three-electrode system is placed in synthesis ZnIn2S4Precursor solution in, by electrochemical deposition, synthesized in titanium sheet substrate
ZnIn2S4Precursor film；Annealed technique obtains ZnIn under atmosphere of inert gases2S4Membrane electrode；
Step 2, ethene dioxythiophene is dissolved in deionized water, sodium sulphate is added as electrolyte, prepares and obtains polymer
Precursor solution；
Step 3, it by step 1 treated three-electrode system, is placed in the polybenzazole precursor liquid solution of step 2 acquisition, is gathered
It closes；Wherein, after polymerizeing preset time, working electrode is overturn, by working electrode another side towards to electrode；
Step 4, treated that working electrode is rinsed with dehydrated alcohol for step 3, then is rinsed well with deionized water, dry, obtains
Polyglycolic acid fibre-indium sulfide zinc compound film electrode.
2. a kind of Polyglycolic acid fibre according to claim 1-indium sulfide zinc compound film electrode preparation method, special
Sign is, further includes pre-processing in step 1 to titanium sheet, and pretreated step specifically includes:
(1) titanium sheet is mechanically polished；
(2) step (1) treated titanium sheet is ultrasonically treated with acetone, is rinsed well with deionized water；
(3) step (2) treated titanium sheet is ultrasonically treated with isopropanol, is rinsed well with deionized water；
(4) step (3) treated titanium sheet is dry in nitrogen stream.
3. a kind of Polyglycolic acid fibre according to claim 1-indium sulfide zinc compound film electrode preparation method, special
Sign is, in step 1 further include: prepares the aqueous solution of zinc chloride, four water inidum chlorides and sodium thiosulfate, potassium chloride conduct is added
Electrolyte obtains synthesis ZnIn2S4Precursor solution；Wherein, in the excessive situation of sulfur content, with molar ratio computing, Zn:In
=1:1.25.
4. a kind of Polyglycolic acid fibre according to claim 3-indium sulfide zinc compound film electrode preparation method, special
Sign is, in step 1, the synthesis ZnIn of acquisition2S4Precursor solution after, pH value of solution is adjusted to 2~2.5.
5. a kind of Polyglycolic acid fibre according to claim 1-indium sulfide zinc compound film electrode preparation method, special
Sign is, in step 1, electrochemical deposition current potential is set as -1.1v~-1.3v, the electrochemical deposition time be set as 10min~
20min。
6. a kind of Polyglycolic acid fibre according to claim 1-indium sulfide zinc compound film electrode preparation method, special
Sign is, in step 1, specifically includes under atmosphere of inert gases: inert gas flow is 400mL/min~600mL/min；
Annealing process specifically includes: 150 DEG C~500 DEG C of annealing temperature is heated to the rate of 5 DEG C/min from room temperature, when stop
Between be 1h.
7. a kind of Polyglycolic acid fibre according to claim 1-indium sulfide zinc compound film electrode preparation method, special
Sign is, in step 2, every 100mL deionized water corresponds to the 3,4-rthylene dioxythiophene of 0.072g~0.284g, corresponding 0.710g
Sodium sulphate.
8. a kind of Polyglycolic acid fibre according to claim 7-indium sulfide zinc compound film electrode preparation method, special
Sign is that the polybenzazole precursor liquid solution that step 2 is prepared is added potassium chloride as electrolyte, hydrochloric acid is added and adjusts pH value of solution
It is 2~2.5.
9. a kind of Polyglycolic acid fibre according to claim 1-indium sulfide zinc compound film electrode preparation method, special
Sign is, in polybenzazole precursor liquid solution, EDOT concentration is 0.005M, 0.01M or 0.02M, and the polymerization time being corresponding in turn to is
1h, 2h or 3h；Wherein, when polymerization time carries out half, working electrode is overturn, by working electrode another side towards to electrode.
10. a kind of Polyglycolic acid fibre-indium sulfide zinc compound film electrode, which is characterized in that appoint using in claim 1 to 9
A kind of preparation method preparation；
ZnIn has been sequentially depositing on titanium substrate (1)2S4Film layer (2) and PEDOT film layer (3).
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