CN112030176B - Silicon photoelectric cathode modified by tungsten sulfide nano particles and preparation method thereof - Google Patents
Silicon photoelectric cathode modified by tungsten sulfide nano particles and preparation method thereof Download PDFInfo
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- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 41
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 36
- 239000010703 silicon Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 46
- 150000003376 silicon Chemical class 0.000 claims abstract description 8
- 238000005530 etching Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 30
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 2
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 239000002957 persistent organic pollutant Substances 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 abstract description 8
- 238000011065 in-situ storage Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000000151 deposition Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract 1
- 230000033116 oxidation-reduction process Effects 0.000 abstract 1
- 239000012429 reaction media Substances 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- -1 Transition metal sulfides Chemical class 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000000089 atomic force micrograph Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- YMZATHYBBBKECM-UHFFFAOYSA-N tris(sulfanylidene)tungsten Chemical compound S=[W](=S)=S YMZATHYBBBKECM-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses a tungsten sulfide nanoparticle modified silicon photocathode and a preparation method thereof, belonging to the field of photoelectrocatalysis semiconductor materials. The invention specifically comprises the following steps: taking a solution of soluble thiotungstate as a reaction raw material, taking a hydrofluoric acid solution as a reaction medium, and depositing tungsten sulfide nano-particles to the surface of a silicon wafer in situ under the oxidation-reduction action of the surface of the silicon wafer which is subjected to fluorinated etching treatment and thiotungstate ions in the hydrofluoric acid medium under the normal temperature condition to prepare the silicon photocathode with the uniformly deposited ultrathin tungsten sulfide nano-particle film.
Description
Technical Field
The invention belongs to the field of photoelectrocatalysis semiconductor materials, and particularly relates to a silicon photocathode modified by tungsten sulfide nanoparticles and a preparation method thereof.
Background
Photoelectrocatalytic pure water decomposition and carbon dioxide reduction is a very effective way to develop and convert solar energy, where the key and most fundamental factor in determining photoelectrocatalytic performance is the need to use a suitable and efficient semiconductor photocathode. Among many semiconductors, silicon, which is abundant and inexpensive, is the most promising small bandgap semiconductor (1.12 eV), and its bandgap absorption almost perfectly matches the near infrared and visible light portions in the solar spectrum, and at the same time it has nearly ideal band structure, and can fully meet the requirements of photoelectrocatalysis pure water decomposition and carbon dioxide reduction on the semiconductor conduction band position. However, the photoelectrocatalysis performance of pure silicon is very poor, mainly due to the retarded hydrogen evolution and carbon dioxide reduction catalytic capability of the surface of the pure silicon, so that a modification promoter needs to be deposited on the surface of the pure silicon to meet the performance requirement of photoelectrocatalysis.
Transition metal sulfides such as tungsten sulfide have shown great potential as novel inexpensive promoters on silicon-based photocathodes. It has been reported that by synthesizing amorphous tungsten disulfide and tungsten trisulfide under high temperature condition and modifying silicon photocathode, initial photogeneration voltage close to 0.4V for standard hydrogen electrode is obtained, and 20mA ∙ cm is reached under 0V condition-2The photo-generated current (appl. mater. inter. 2014, 6, 10408). In general, the co-catalytic properties of tungsten sulfide, and its interaction with the silicon semiconductor, determine the photo-catalytic properties of the silicon photocathode. How to improve the promoting properties of tungsten sulfide and its interaction with the silicon semiconductor depends on what technical means are used to achieve the preparation. Chemical vapor deposition (MRS commu. 2017, 7, 272), thermal synthesis (appl. cat. B: environ. 2018, 237, 158) or pulsed laser deposition (adv. sci. 2019, 6, 1900301) and the like are the most commonly used technical means. Although silicon photocathodes satisfying the photocatalytic performance can occasionally be obtained, these technical means have disadvantages of very low deposition rate, non-uniform deposition thickness, high preparation cost, and the like.
Disclosure of Invention
The invention provides a silicon photoelectric cathode modified by tungsten sulfide nano particles and a preparation method thereof, wherein the preparation method is simple and easy to operate, the reaction condition is mild and controllable, the thickness of the obtained tungsten sulfide nano particles is 1-15nm, the tungsten sulfide nano particles can be simply controlled by changing the concentration of thiotungstate and the reaction time, and the raw material cost and the preparation efficiency are superior to those of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a silicon photoelectric cathode modified by tungsten sulfide nano-particles is characterized in that tungsten sulfide nano-particles are deposited on the surface of p-type monocrystalline silicon in the photoelectric cathode, the tungsten sulfide nano-particles are uniformly distributed on the surface of the p-type monocrystalline silicon, and the thickness of the tungsten sulfide nano-particle layer is 1-15 nm.
A preparation method of a tungsten sulfide nanoparticle modified silicon photocathode comprises the following steps:
(1) putting p-type monocrystalline silicon in a mixed solution of concentrated sulfuric acid and hydrogen peroxide at 40-80%oC, cleaning for 30-60min to remove organic pollutants on the surface, and then etching for 5-30min by using 0.5-10% fluorine-containing solution to remove a surface oxide layer;
(2) dissolving soluble thiotungstate in solvent, preparing 0.05-0.5M thiotungstate solution, standing at 5%oC, standby;
(3) and (3) dropwise adding the thiotungstate solution prepared in the step (2) with a certain volume into a hydrofluoric acid solution to prepare thiotungstate mixed hydrofluoric acid solutions with different concentrations, horizontally placing the p-type monocrystalline silicon cleaned in the step (1) in the thiotungstate mixed hydrofluoric acid solution for 1-60min, cleaning, and drying in an argon atmosphere or vacuum to prepare the tungsten sulfide nanoparticle modified silicon photocathode.
In the above step, the fluorine-containing solution in step (1) is a hydrofluoric acid or ammonium fluoride solution; the soluble thiotungstate in the step (2) is (NH4)2WS4、Na2WS4Or K2WS4The solvent is water or ethanol; in the step (3), the concentration of ammonium thiotungstate in the mixed solution of the thiotungstate and the hydrofluoric acid is 0.1-10mM, and the mass percentage concentration of the hydrofluoric acid is 1-10%; the tungsten sulfide is nanoThe thickness of the particle layer is 1-15nm, and the thickness of the tungsten sulfide nano particle layer can be controlled by changing the concentration of thiotungstate and the reaction time.
Has the advantages that: the invention provides a silicon photocathode modified by tungsten sulfide nano particles and a preparation method thereof, wherein thiotungstate is used as a raw material, amorphous tungsten sulfide nano particles are controllably deposited on the silicon photocathode in situ through simple normal-temperature liquid-phase redox reaction, the thickness of the deposited tungsten sulfide nano particle layer is 1-15nm, the thickness can be controlled simply by changing the concentration and the reaction time of the thiotungstate, and the raw material cost and the preparation efficiency are both superior to those of the prior art; the deposited tungsten sulfide nano particles and the silicon photocathode have a tight interface combination effect, so that efficient photoproduction electron transmission is realized; the method has the advantages of simple and easily-operated process, mild and controllable conditions, low cost of reagents and environmental protection, and the prepared silicon photocathode has great application potential in the fields of photoelectrocatalysis water decomposition, photoelectrocatalysis carbon dioxide reduction and the like.
Drawings
FIG. 1 is a schematic structural diagram of a silicon photocathode modified with tungsten sulfide nanoparticles according to the present invention;
FIG. 2 is an atomic force micrograph of amorphous tungsten sulfide deposited in situ on the surface of a silicon photocathode prepared in example 3 of the present invention;
fig. 3 is a profile view showing the thickness of tungsten sulfide nanoparticles in a silicon photocathode prepared in example 3 of the present invention.
Detailed Description
The invention is described in detail below with reference to specific embodiments and with reference to the following figures:
example 1
A silicon photoelectric cathode modified by tungsten sulfide nano particles and a preparation method thereof comprise the following steps:
cutting p-type monocrystalline silicon into square samples with side length of 1cm by using a glass cutter, placing the square samples in a mixed solution of 10mL of concentrated sulfuric acid and 5mL of hydrogen peroxide, and placing the mixture in a 60-mL mixed solutionoC, cleaning for 40min, and etching for 10min by using 2.0% hydrofluoric acid to obtain bare silicon without an oxide layer; 2.0mmol of ammonium thiotungstate is dissolved in 10mL of water to prepare 0.2M ammonium thiotungstate solutionThen, 0.05mL of this ammonium thiotungstate solution was dropped into 10mL of a 5.0% hydrofluoric acid solution to prepare a 1.0mM ammonium thiotungstate hydrofluoric acid mixed solution, and the above-mentioned p-type single crystal silicon having no oxide layer was placed in this solution for 5 minutes, followed by washing with a large amount of ultrapure water and drying with argon gas to prepare a tungsten sulfide nanoparticle thin film-modified silicon photocathode shown in FIG. 1, wherein the thickness of the obtained tungsten sulfide thin film was about 9.0 nm.
Example 2
A silicon photoelectric cathode modified by tungsten sulfide nano particles and a preparation method thereof comprise the following steps:
cutting p-type monocrystalline silicon into square samples with side length of 1cm by using a glass cutter, placing the square samples in a mixed solution of 10mL of concentrated sulfuric acid and 5mL of hydrogen peroxide, and placing the mixture in a 60-mL mixed solutionoC, cleaning for 40min, and etching for 5min by using 5.0% hydrofluoric acid to obtain bare silicon without an oxide layer; 1.0mmol of ammonium thiotungstate was dissolved in 10mL of water to prepare a 0.1M ammonium thiotungstate solution, 0.02mL of the ammonium thiotungstate solution was then added dropwise to 10mL of a 6.0% hydrofluoric acid solution to prepare a 0.2mM ammonium thiotungstate mixed hydrofluoric acid solution, the above-mentioned oxide-layer-free p-type single crystal silicon was placed in the solution for 20min, and then washed with a large amount of ultrapure water and dried with argon gas to prepare a tungsten sulfide nanoparticle film-modified silicon photocathode as shown in FIG. 1, wherein the thickness of the obtained tungsten sulfide film was about 6.0 nm.
Example 3
A silicon photoelectric cathode modified by tungsten sulfide nano particles and a preparation method thereof comprise the following steps:
cutting p-type monocrystalline silicon into square samples with side length of 1cm by using a glass cutter, placing the square samples in a mixed solution of 10mL of concentrated sulfuric acid and 5mL of hydrogen peroxide, and placing the mixture in a 60-mL mixed solutionoC, cleaning for 40min, and etching for 5min by using 3.0% hydrofluoric acid to obtain bare silicon without an oxide layer; 1.0mmol of ammonium thiotungstate was dissolved in 10mL of water to prepare a 0.1M ammonium thiotungstate solution, 0.01mL of the ammonium thiotungstate solution was added dropwise to 10mL of an 8.0% hydrofluoric acid solution to prepare a 0.1mM ammonium thiotungstate mixed hydrofluoric acid solution, the above-mentioned oxide layer-free p-type single crystal silicon was placed in the solution for 20min, and then washed with a large amount of ultrapure water and dried with argon gas to prepare a tungsten sulfide nanoparticle thin film as shown in FIG. 1The thickness of the obtained tungsten sulfide thin film is about 4.0 nm. As can be seen from FIG. 2, the amorphous tungsten sulfide nanoparticles prepared by the chemical in-situ self-reduction method have uniform size of about 10nm and good dispersibility, and are uniformly distributed on the surface of a Si wafer, and as can be seen from FIG. 3, the thickness of the amorphous tungsten sulfide nanoparticles modified Si surface film prepared by the chemical in-situ self-reduction method is 4-6 nm.
The foregoing is only a preferred embodiment of this invention and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the invention and these modifications should also be considered as the protection scope of the invention.
Claims (7)
1. A preparation method of a tungsten sulfide nanoparticle modified silicon photocathode is characterized by comprising the following steps:
(1) putting p-type monocrystalline silicon in a mixed solution of concentrated sulfuric acid and hydrogen peroxide at 40-80%oC, cleaning for 30-60min to remove organic pollutants on the surface, and then etching for 5-30min by using 0.5-10% fluorine-containing solution to remove a surface oxide layer;
(2) dissolving soluble thiotungstate in solvent, preparing 0.05-0.5M thiotungstate solution, standing at 5%oC, standby;
(3) and (3) dropwise adding the thiotungstate solution prepared in the step (2) with a certain volume into a hydrofluoric acid solution to prepare thiotungstate mixed hydrofluoric acid solutions with different concentrations, horizontally placing the p-type monocrystalline silicon cleaned in the step (1) in the thiotungstate mixed hydrofluoric acid solution for 1-60min, cleaning, and drying in an argon atmosphere or vacuum to prepare the tungsten sulfide nanoparticle modified silicon photocathode.
2. The method for preparing the photocathode of silicon modified by tungsten sulfide nanoparticles as claimed in claim 1, wherein the fluorine-containing solution in step (1) is hydrofluoric acid or ammonium fluoride solution.
3. The tungsten sulfide nanoparticle modified silicon photocathode of claim 1The preparation method is characterized in that the soluble thiotungstate in the step (2) is (NH)4)2WS4、Na2WS4Or K2WS4The solvent is water or ethanol.
4. The method for preparing the photocathode for silicon modified by tungsten sulfide nanoparticles as claimed in claim 3, wherein the concentration of ammonium thiotungstate in the mixed hydrofluoric acid solution of thiotungstate in step (3) is 0.1-10mM, and the concentration of hydrofluoric acid is 1-10% by mass.
5. The method of claim 1, wherein the thickness of the tungsten sulfide nanoparticle layer can be controlled by changing the concentration of thiotungstate and the reaction time during the preparation process.
6. The method for preparing the photocathode for silicon modified by tungsten sulfide nanoparticles as claimed in claim 1, wherein tungsten sulfide nanoparticles are deposited on the surface of p-type single crystal silicon in the silicon photocathode, and the tungsten sulfide nanoparticles are uniformly distributed on the surface of the p-type single crystal silicon.
7. The method for preparing the silicon photocathode modified by the tungsten sulfide nanoparticles as claimed in claim 5 or 6, wherein the thickness of the tungsten sulfide nanoparticles is 1-15 nm.
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