CN109395736A - A kind of preparation method of the selenodont pucherite composite material of interleaved with each other - Google Patents
A kind of preparation method of the selenodont pucherite composite material of interleaved with each other Download PDFInfo
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- CN109395736A CN109395736A CN201811481631.4A CN201811481631A CN109395736A CN 109395736 A CN109395736 A CN 109395736A CN 201811481631 A CN201811481631 A CN 201811481631A CN 109395736 A CN109395736 A CN 109395736A
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- composite material
- pucherite
- tin oxide
- indium tin
- coated glass
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- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000011521 glass Substances 0.000 claims abstract description 26
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims abstract description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 13
- 229910002588 FeOOH Inorganic materials 0.000 claims abstract description 10
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 10
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 6
- 239000002243 precursor Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 12
- 238000004070 electrodeposition Methods 0.000 claims description 9
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- FSJSYDFBTIVUFD-SUKNRPLKSA-N (z)-4-hydroxypent-3-en-2-one;oxovanadium Chemical compound [V]=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FSJSYDFBTIVUFD-SUKNRPLKSA-N 0.000 claims description 4
- 229940005561 1,4-benzoquinone Drugs 0.000 claims description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 229960001760 dimethyl sulfoxide Drugs 0.000 claims description 4
- 229960004756 ethanol Drugs 0.000 claims description 4
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000006193 liquid solution Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical group Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims 2
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 229910052742 iron Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract 2
- 238000002834 transmittance Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 229940024464 emollients and protectives zinc product Drugs 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/847—Vanadium, niobium or tantalum or polonium
- B01J23/8472—Vanadium
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
- Chemically Coating (AREA)
Abstract
The selenodont nickel of interleaved with each other is deposited on a kind of tin indium oxide (ITO) electro-conductive glass: FeOOH/pucherite composite material preparation method belongs to field of material preparation.This method includes the following steps substrate cleaning-precursor solution preparation-bismuth oxyiodide electro-deposition-pucherite generation-nickel: FeOOH/pucherite composite material synthesis.It is an advantage of the invention that forming large area crescent composite structure, process flow is simple, selects light transmittance high, the indium tin oxide-coated glass of good conductivity is as substrate, and no pollution to the environment, operating process is simple, and at low cost, reaction condition is easily realized.The present invention only need to can form nickel by two-step method: FeOOH/pucherite composite material, can enhance the absorption to visible light improves photoelectric conversion efficiency, is with a wide range of applications in the fields such as photocatalysis and solar battery.
Description
Technical field
The present invention relates to nano material synthesis technical fields, more specifically the selenodont about a kind of interleaved with each other
The preparation method of pucherite composite material.
Background technique
Pucherite has suitable band gap (2.4-2.6 eV), with band gap width is moderate, is readily synthesized, is at low cost, ring
The advantages that border compatibility and resistance to photoetch, however there is also some defects, such as light induced electron-sky for the photocatalytic applications of pucherite
Cave is compound to being easy, and photo-generated carrier migration rate is slow etc., these defects reduce the photoelectricity transfer efficiency of pucherite, to limit
Its extensive use is made.For these defects, make pucherite and nickel: FeOOH is compounded to form heterojunction structure, can not only
Promote the separation of charge and can improve to visible absorption efficiency, is widely used in water decomposition and optical electro-chemistry detection etc.
Field.
Currently, nickel in practical applications: FeOOH/pucherite composite material mostly uses electrochemical deposition method and rotation
Coating preparation, for pattern often based on nanoporous, situation is more single.In order to make it have better pattern and performance, I
Use the two-step method on indium tin oxide-coated glass and prepare a kind of selenodont nickel of interleaved with each other: FeOOH/vanadium
Sour bismuth composite material, advantage include that surface area is big, are distributed relatively uniform, function admirable, at low cost, can shorten electronics and sky
The transmission path in cave is conducive to the increase of photoelectric current.
Summary of the invention
Presently, there are aiming at the problem that, the present invention provides a kind of simple and effective on indium tin oxide-coated glass, operation letter
The synthetic method of the selenodont pucherite composite material of single, large specific surface area interleaved with each other.
Indium tin oxide-coated glass is In2O3The semiconductor material of Sn is mixed, film is due to excellent electric conductivity and light
Learn performance, tin indium oxide be in visible light (400~800 nm) range it is transparent, transmissivity can in 90 % or more, and its
The reflectivity of infrared light district is also in 85 % or more.So high visible region transmissivity and the same low-resistivity of infrared light district reflectivity
It combines, indium tin oxide films is made to become typical transparent conductive film material.Simultaneous oxidation indium tin thin film film layer very securely,
Hard, alkaline-resisting, heat-resisting, humidity and performance stabilization, can be used as a kind of base load oxidized zinc products.
In order to solve the above technical problems, the present invention is realized by following measures: a kind of moon of interleaved with each other
Tooth form pucherite composite material, feature the following steps are included:
(1) indium tin oxide-coated glass the cleaning of tin indium oxide (ITO) electro-conductive glass: is sequentially placed into acetone, dehydrated alcohol, two
Secondary water is ultrasonically treated 10 ~ 20 min, and it is dry to be then placed in 40 ~ 60 DEG C of 30 min of baking oven；
(2) preparation of precursor solution: weighing 0.3638 ~ 0.5257 g bismuth nitrate and 6.6404 ~ 6.9352 g potassium iodide are dissolved in
In the nitric acid solution of 100 PH=1.2 mL, 5 ~ 10 min of stirring make it sufficiently dissolve mixing, and 45 ~ 55 mL are added and contain 0.3 M
The ethanol solution of 1,4-benzoquinone stirs 30 ~ 40 min；
(3) indium tin oxide-coated glass handled well in (1) electro-deposition of bismuth oxyiodide: is placed in configured forerunner in (2)
In liquid solution, using the point Stripping Analysis Method For Simultaneous of electrochemical workstation, adjustment parameter first is -0.3 V, and 5 ~ 10s is located in advance
Reason, then adjustment parameter are -0.1 V, and 15 ~ 20 min carry out electrochemical deposition, and taking-up is cleaned three times with secondary water, are put into 25 DEG C
Drying；
(4) generation of pucherite: the indium tin oxide-coated glass prepared in (3) is immersed and contains 0.4 M vanadyl acetylacetonate
Dimethyl sulphoxide solution in 20 ~ 30 s, be then placed into preheating in 120 DEG C of Muffle furnace, headed by design parameter setting
120 DEG C are first preheating to, then is heated to 280 DEG C with the speed of 1 DEG C/min, is heated to 450 DEG C with the speed of 2 DEG C/min, most
Afterwards in 450 DEG C of 1 h of constant temperature, it is down to room temperature taking-up, is dipped in the sodium hydroxide solution of 0.05 M and is slowly stirred 5 ~ 10
Min, taking-up are rinsed with secondary water；
(5) nickel: the synthesis of FeOOH/pucherite composite material: 0.0243 ~ 0.0521 g ferric trichloride is weighed respectively and is set
The urea for being dissolved in 25 ~ 40 mL, 45 mM with 0.1783 ~ 0.3565 g nickel chloride in the urea liquid of 5 ~ 10 mL, 45 mM is molten
In liquid, then the indium tin oxide-coated glass prepared in (4) is immersed in mixed liquor, the heat collecting type constant temperature of the oil bath at 100 DEG C
It heats and reacts 1 ~ 2 h in magnetic stirring apparatus, taking-up is cleaned three times with secondary water, is put into 25 DEG C of drying.
Beneficial effects of the present invention:
(1) the selenodont pucherite composite material of the interleaved with each other synthesized has bigger table compared to other pucherite materials
Area is conducive to improve light absorption.
(2) this method is using indium tin oxide-coated glass as substrate, is advantageously implemented high temperature resistant, conductive performance, can be with
Material as connection electrode.
(3) preparation method is simple, easy to operate, low in cost.
(4) such pucherite composite material has a wide range of applications valence in fields such as photocatalysis, sensor and electronic devices
Value.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the selenodont pucherite composite material of interleaved with each other.
Specific embodiment
Therefore prepare that a kind of surface area is big, and daylighting ability is strong, the pucherite composite material of function admirable is one important
Project.
Embodiment 1
(1) indium tin oxide-coated glass the cleaning of tin indium oxide (ITO) electro-conductive glass: is sequentially placed into acetone, dehydrated alcohol, two
Secondary water is ultrasonically treated 10 min, and it is dry to be then placed in 40 DEG C of 30 min of baking oven；
(2) preparation of precursor solution: weighing 0.3638 g bismuth nitrate and 6.6404 g potassium iodide are dissolved in 100 PH=1.2 mL
In nitric acid solution, 5 min of stirring make it sufficiently dissolve mixing, and the ethanol solution that 45 mL contain 0.3 M 1,4-benzoquinone is added, stirring
30 min；
(3) indium tin oxide-coated glass handled well in (1) electro-deposition of bismuth oxyiodide: is placed in configured forerunner in (2)
In liquid solution, using the point Stripping Analysis Method For Simultaneous of electrochemical workstation, adjustment parameter first is -0.3 V, and 5 s are pre-processed,
Adjustment parameter is -0.1 V again, and 15 min carry out electrochemical deposition, and taking-up is cleaned three times with secondary water, is put into 25 DEG C of drying；
(4) generation of pucherite: the indium tin oxide-coated glass prepared in (3) is immersed and contains 0.4 M vanadyl acetylacetonate
Dimethyl sulphoxide solution in 20 s, be then placed into preheating as in 120 DEG C of Muffle furnace, design parameter is set as first
120 DEG C are preheating to, then is heated to 280 DEG C with the speed of 1 DEG C/min, is heated to 450 DEG C with the speed of 2 DEG C/min, finally
In 450 DEG C of 1 h of constant temperature, it is down to room temperature taking-up, is dipped in the sodium hydroxide solution of 0.05 M and is slowly stirred 5 min, is taken out
It is rinsed with secondary water；
(5) nickel: the synthesis of FeOOH/pucherite composite material: 0.0243 g ferric trichloride is weighed respectively and is placed in 5 mL
It is dissolved in the urea liquid of 25 mL, 45 mM in the urea liquid of 45 mM with 0.1783 g nickel chloride, then by preparation in (4)
Good indium tin oxide-coated glass immerses in mixed liquor, reacts in the heat collecting type constant-temperature heating magnetic stirring apparatus of the oil bath at 100 DEG C
1 h, taking-up are cleaned three times with secondary water, are put into 25 DEG C of drying.
Claims (6)
1. a kind of preparation method of the selenodont pucherite composite material of interleaved with each other, it is characterised in that this method includes following
Step
It is rapid:
(1) indium tin oxide-coated glass the cleaning of tin indium oxide (ITO) electro-conductive glass: is sequentially placed into acetone, dehydrated alcohol, two
Secondary water is ultrasonically treated 10 ~ 20 min, and it is dry to be then placed in 40 ~ 60 DEG C of 30 min of baking oven；
(2) preparation of precursor solution: weighing 0.3638 ~ 0.5257 g bismuth nitrate and 6.6404 ~ 6.9352 g potassium iodide are dissolved in
In the nitric acid solution of 100 PH=1.2 mL, 5 ~ 10 min of stirring make it sufficiently dissolve mixing, and 45 ~ 55 mL are added and contain 0.3 M
The ethanol solution of 1,4-benzoquinone stirs 30 ~ 40 min；
(3) indium tin oxide-coated glass handled well in (1) electro-deposition of bismuth oxyiodide: is placed in configured forerunner in (2)
In liquid solution, using the point Stripping Analysis Method For Simultaneous of electrochemical workstation, adjustment parameter first is -0.3 V, and 5 ~ 10s is located in advance
Reason, then adjustment parameter are -0.1 V, and 15 ~ 20 min carry out electrochemical deposition, and taking-up is cleaned three times with secondary water, are put into 25 DEG C
Drying；
(4) generation of pucherite: the indium tin oxide-coated glass prepared in (3) is immersed and contains 0.4 M vanadyl acetylacetonate
Dimethyl sulphoxide solution in 20 ~ 30 s, be then placed into preheating in 120 DEG C of Muffle furnace, headed by design parameter setting
120 DEG C are first preheating to, then is heated to 280 DEG C with the speed of 1 DEG C/min, is heated to 450 DEG C with the speed of 2 DEG C/min, most
Afterwards in 450 DEG C of 1 h of constant temperature, it is down to room temperature taking-up, is dipped in the sodium hydroxide solution of 0.05 M and is slowly stirred 5 ~ 10
Min, taking-up are rinsed with secondary water；
(5) nickel: the synthesis of FeOOH/pucherite composite material: 0.0243 ~ 0.0521 g ferric trichloride is weighed respectively and is placed in
In the urea liquid of 5 ~ 10 mL, 45 mM and 0.1783 ~ 0.3565 g nickel chloride is dissolved in the urea liquid of 25 ~ 40 mL, 45 mM
In, then the indium tin oxide-coated glass prepared in (4) is immersed in mixed liquor, the heat collecting type constant temperature of the oil bath at 100 DEG C adds
1 ~ 2 h is reacted in pyromagnetic force blender, taking-up is cleaned three times with secondary water, is put into 25 DEG C of drying.
2. the preparation method of the selenodont pucherite composite material of a kind of interleaved with each other according to claim 1,
Be characterized in: the cleaning of indium tin oxide-coated glass is that indium tin oxide-coated glass is cut into the cm of 1 cm × 5 in step (1)
Size is sequentially placed into acetone, dehydrated alcohol, secondary water and is ultrasonically treated 10 min, it is dry to be then placed in 40 DEG C of 30 min of baking oven.
3. the preparation method of the selenodont pucherite composite material of a kind of interleaved with each other according to claim 1,
Be characterized in: step (2) configuration process weighs 0.3638 g bismuth nitrate and 6.6404 g potassium iodide are dissolved in 100 PH=1.2 mL
In nitric acid solution, 5 min of stirring make it sufficiently dissolve mixing, and the ethanol solution that 45 mL contain 0.3 M 1,4-benzoquinone is added, stirring
30 min。
4. the preparation method of the selenodont pucherite composite material of a kind of interleaved with each other according to claim 1,
Be characterized in: step (3) electrodeposition process be the indium tin oxide-coated glass handled well in (1) is placed in it is configured in (2) before
It drives in liquid solution, using the point Stripping Analysis Method For Simultaneous of electrochemical workstation, adjustment parameter first is -0.3 V, and 5 s are located in advance
Reason, then adjustment parameter are -0.1 V, and 15 min carry out electrochemical deposition, and taking-up is cleaned three times with secondary water, are put into 25 DEG C of bakings
It is dry.
5. the preparation method of the selenodont pucherite composite material of a kind of interleaved with each other according to claim 1,
Be characterized in: the generating process of step (4) pucherite is to immerse the indium tin oxide-coated glass prepared in (3) to contain 0.4 M
20 s in the dimethyl sulphoxide solution of vanadyl acetylacetonate are then placed into preheating specifically to join in 120 DEG C of Muffle furnace
Number is set as being initially pre-heated to 120 DEG C, then is heated to 280 DEG C with the speed of 1 DEG C/min, is heated with the speed of 2 DEG C/min
To 450 DEG C, finally in 450 DEG C of 1 h of constant temperature, it is down to room temperature taking-up, is dipped in the sodium hydroxide solution of 0.05 M slowly
5 min are stirred, taking-up is rinsed with secondary water.
6. the preparation method of the selenodont pucherite composite material of a kind of interleaved with each other according to claim 1,
Be characterized in: step (5) nickel: FeOOH/pucherite composite material synthesis process is to weigh 0.0243 g tri-chlorination respectively
Iron is placed in the urea liquid of 5 mL, 45 mM and 0.1783 g nickel chloride is dissolved in the urea liquid of 25 mL, 45 mM, then
The indium tin oxide-coated glass prepared in (4) is immersed in mixed liquor, the heat collecting type heated at constant temperature magnetic force of the oil bath at 100 DEG C
1 h is reacted in blender, taking-up is cleaned three times with secondary water, is put into 25 DEG C of drying.
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| CN110042391A (en) * | 2019-05-05 | 2019-07-23 | 上海大学 | The nickel array approach of pucherite nano particle package based on anodic oxidation aluminium formwork |
| CN110068570A (en) * | 2019-04-03 | 2019-07-30 | 济南大学 | A kind of preparation of the electrochemical sensor shown with instant visualization colorimetric |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110068570A (en) * | 2019-04-03 | 2019-07-30 | 济南大学 | A kind of preparation of the electrochemical sensor shown with instant visualization colorimetric |
| CN110068570B (en) * | 2019-04-03 | 2021-05-25 | 济南大学 | Preparation of electrochemical sensor with instant visual colorimetric display |
| CN109821549A (en) * | 2019-04-08 | 2019-05-31 | 陕西科技大学 | A kind of preparation method of vanadium doping FeOOH elctro-catalyst |
| CN110042391A (en) * | 2019-05-05 | 2019-07-23 | 上海大学 | The nickel array approach of pucherite nano particle package based on anodic oxidation aluminium formwork |
| CN110042391B (en) * | 2019-05-05 | 2021-04-09 | 上海大学 | Nickel array method for coating bismuth vanadate nano particles based on anodic aluminum oxide template |
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