CN114082425A - Bi2S3/AgBiS2Method for preparing nanoclusters - Google Patents
Bi2S3/AgBiS2Method for preparing nanoclusters Download PDFInfo
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 29
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 28
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 24
- 239000011593 sulfur Substances 0.000 claims abstract description 24
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 22
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 22
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 22
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052709 silver Inorganic materials 0.000 claims abstract description 13
- 239000004332 silver Substances 0.000 claims abstract description 13
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000002114 nanocomposite Substances 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 238000004729 solvothermal method Methods 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 65
- 238000006243 chemical reaction Methods 0.000 claims description 19
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 10
- KKMOSYLWYLMHAL-UHFFFAOYSA-N 2-bromo-6-nitroaniline Chemical compound NC1=C(Br)C=CC=C1[N+]([O-])=O KKMOSYLWYLMHAL-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- BRWIZMBXBAOCCF-UHFFFAOYSA-N hydrazinecarbothioamide Chemical compound NNC(N)=S BRWIZMBXBAOCCF-UHFFFAOYSA-N 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- QYIGOGBGVKONDY-UHFFFAOYSA-N 1-(2-bromo-5-chlorophenyl)-3-methylpyrazole Chemical compound N1=C(C)C=CN1C1=CC(Cl)=CC=C1Br QYIGOGBGVKONDY-UHFFFAOYSA-N 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- RBWNDBNSJFCLBZ-UHFFFAOYSA-N 7-methyl-5,6,7,8-tetrahydro-3h-[1]benzothiolo[2,3-d]pyrimidine-4-thione Chemical compound N1=CNC(=S)C2=C1SC1=C2CCC(C)C1 RBWNDBNSJFCLBZ-UHFFFAOYSA-N 0.000 claims description 2
- KQJQICVXLJTWQD-UHFFFAOYSA-N N-Methylthiourea Chemical compound CNC(N)=S KQJQICVXLJTWQD-UHFFFAOYSA-N 0.000 claims description 2
- XGEGHDBEHXKFPX-UHFFFAOYSA-N N-methylthiourea Natural products CNC(N)=O XGEGHDBEHXKFPX-UHFFFAOYSA-N 0.000 claims description 2
- MNOILHPDHOHILI-UHFFFAOYSA-N Tetramethylthiourea Chemical compound CN(C)C(=S)N(C)C MNOILHPDHOHILI-UHFFFAOYSA-N 0.000 claims description 2
- QSBNOZODKXUXSP-UHFFFAOYSA-K bismuth;azane;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound N.[Bi+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QSBNOZODKXUXSP-UHFFFAOYSA-K 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 2
- 229940071536 silver acetate Drugs 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 239000002086 nanomaterial Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000013077 target material Substances 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000002524 electron diffraction data Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052678 stilbite Inorganic materials 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The invention discloses a Bi2S3/AgBiS2The preparation method of the nanocluster is characterized by comprising the following steps: bi is prepared by adopting a bismuth source, a sulfur source and a silver source, adopting ethylene glycol as a solvent, adopting polyethylene glycol as a stable template and adopting a one-step solvothermal method under the action of polyvinylpyrrolidone as a surfactant2S3/AgBiS2Nanocomposite material of Bi2S3/AgBiS2The nano composite material is a cluster formed by dendritic short rods, has uniform size and good dispersity, and is an excellent photocatalytic material.
Description
Technical Field
The invention belongs to the field of nano material preparation, and particularly relates to Bi2S3/AgBiS2A method for preparing nanoclusters.
Background
Bi2S3Is the main component of bismuth stilbite, belongs to an orthorhombic system, has a band gap of 1.3-1.7eV, and has an absorption coefficient of 104To 105cm-1The photoelectric conversion efficiency can reach 5%, the electron mobility (28cm2 & V-1 & s-1) is high, and the photoelectric conversion material is insoluble in water and soluble in acid. Clustered Bi2S3The nano material has larger specific surface area and excellent optical property and photoelectric property.
AgBiS2Is I-V-VI belonging to the marmatite mineral group2The compound is an N-type direct band gap semiconductor material, Eg is approximately equal to 1.2ev, and the absorption coefficient can reach 105cm-1It can be used in the fields of optics, thermoelectrics and photocatalysis by controlling the size and form of the material.
Albeit single Bi2S3And AgBiS2The nano material has certain photocatalytic performance, but the effect is not good, the band gaps of the nano material and the nano material are narrow, sunlight can be effectively utilized, and due to the narrow band gaps, photo-generated electrons and holes are easy to combine, so that the photocatalytic effect is weakened.
Disclosure of Invention
In order to solve the technical effects, the invention uses Bi2S3And AgBiS2The two photocatalytic materials are compounded to prepare Bi2S3/AgBiS2The nanoclusters have large specific surface area and wide band gaps, and the overall photocatalytic effect can be improved.
In order to achieve the technical purpose, the invention adopts the technical scheme that:
bi2S3/AgBiS2The preparation method of the nanocluster comprises the following steps:
(1) dissolving a bismuth source, a sulfur source and a surfactant polyvinylpyrrolidone (PVP) K30 in an ethylene glycol solvent in an ultrasonic state to prepare a uniformly dispersed solution A; dissolving a bismuth source, a sulfur source, a silver source and a surfactant polyvinylpyrrolidone (PVP) K30 into an ethylene glycol solution in an ultrasonic state to prepare a uniformly dispersed solution B; dissolving stable template polyethylene glycol (PEG) in glycol in an ultrasonic state to prepare a solution C;
(2) one-step solvothermal method for preparing Bi2S3/AgBiS2Nanoclusters: transferring the solution A into a glass container, slowly dripping the solution B into the glass container under magnetic stirring, uniformly mixing the solution A and the solution B, then adding the solution C into the mixed solution, and continuously stirring for a certain time;
(3) transferring the mixed solution in the step (2) into a polytetrafluoroethylene reaction kettle, putting the polytetrafluoroethylene reaction kettle into a drying oven, obtaining black turbid matters after the reaction is finished at a set temperature and time, performing suction filtration and separation by using a vacuum pump, and washing the turbid matters for multiple times by using deionized water and absolute ethyl alcohol in the suction filtration process;
(4) putting the solid obtained in the step (3) into an oven, and drying for a certain time at a set drying temperature to obtain Bi2S3/AgBiS2Nanocomposite, Bi obtained2S3/AgBiS2The nano composite material is a cluster consisting of dendritic short rods, and has high purity, uniform size and good dispersibility.
Preferably, the bismuth source is one or more of bismuth citrate, ammonium bismuth citrate and bismuth acetate.
Preferably, the sulfur source is one or more of 1.3-dimethylthiourea, N-methylthiourea, thiosemicarbazide, tetramethylthiourea, 1.3-diethylthiourea and thiourea.
Preferably, the silver source is one or more of silver nitrate, silver perchlorate and silver acetate.
Preferably, the ratio of bismuth to sulfur in the bismuth source and the sulfur source in the solution a: the molar ratio of sulfur is 2:3, and the molar ratio of bismuth in the bismuth source, the sulfur source and the silver source in the solution B is as follows: sulfur: the molar ratio of silver is 1: 2:1, and the molar concentration ratio of the bismuth source in the solution A to the bismuth source in the solution B is 2: 1.
Preferably, the concentration of PVP in the solution A and the solution B is kept consistent, and the molar concentration of PVP is 0.1mmol-0.5 mmol.
Preferably, the molar concentration of PEG in the solution C is 0.1-0.5 mmol/L.
Preferably, the total molar concentration of bismuth and sulfur in the bismuth source and the sulfur source in the solution A is 0.05-1.5mol/L, and the total molar concentration of bismuth, sulfur and silver in the bismuth source, the sulfur source and the silver source in the solution B is 0.06-1.8 mol/L.
Preferably, the stirring in the step (2) is continued for 2 to 4 hours.
Preferably, the reaction in the oven in the step (3) is set at the temperature of 140 ℃ and 180 ℃ for 2-6 h.
Preferably, the drying temperature in the vacuum drying oven in the step (4) is controlled at 60 ℃.
Compared with the prior art, the invention has the advantages that:
1. the invention uses PEG as a stable template and PVP as a dispersing agent, and can obtain Bi with uniform size, large specific surface area and good dispersibility by regulating and controlling experimental parameters2S3/AgBiS2Nanoclusters.
2. The reaction adopts a one-step solvothermal method to prepare the Bi2S3/AgBiS2 nanocluster, the operation is simple, the yield is stable, the purity is high, the morphology and the structure of the obtained nano material are controllable, and the large-scale production is facilitated.
3. Bi prepared by the invention2S3/AgBiS2Nanoclusters and single Bi2S3And AgBiS2Compared with the nano material, Bi2S3/AgBiS2The effective composition of the nanoclusters enables the nanoclusters to have a better photocatalytic effect.
Drawings
FIG. 1 shows Bi obtained in example 1 of the present invention2S3/AgBiS2X-ray electron diffraction patterns of nanoclusters.
FIG. 2 shows Bi obtained in example 1 of the present invention2S3/AgBiS2Scanning electron microscope pictures of nanoclusters.
FIG. 3 shows Bi obtained in example 1 of the present invention2S3/AgBiS2Scanning electron microscope magnified pictures of nanoclusters.
FIG. 4 shows Bi of large area obtained in example 1 of the present invention2S3/AgBiS2Scanning electron microscope pictures of nanoclusters.
FIG. 5 shows Bi obtained in example 1 of the present invention2S3/AgBiS2And (5) a nanocluster degradation effect graph.
FIG. 6 shows Bi obtained in example 2 of the present invention2S3/AgBiS2Scanning electron microscope pictures of nanoclusters.
FIG. 7 shows Bi obtained in example 3 of the present invention2S3/AgBiS2Scanning electron microscope magnified pictures of nanoclusters.
Detailed Description
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings so that the advantages and features of the invention may be more readily understood by those skilled in the art.
Example 1
Adding 2mmol of bismuth citrate, 3mmol of thiourea and 0.02mmol of PVP into 20mL of ethylene glycol solution to prepare a solution A, performing ultrasonic treatment at room temperature until the bismuth citrate, the thiourea, the silver nitrate and the PVP are fully dissolved and uniformly dispersed, adding 1mmol of bismuth citrate, 2mmol of thiourea, 1mmol of silver nitrate and 0.02mmol of PVP into 20mL of ethylene glycol solution to prepare a solution B, and preparing 0.3mmol of PEG to be dissolved in 10mL of ethylene glycol solution to prepare a solution C. And pouring the uniformly mixed solution A into the solution B, continuously stirring, adding the solution C, continuously stirring for 2 hours, then transferring the mixed solution into a polytetrafluoroethylene reaction kettle, keeping the temperature for 5 hours, performing suction filtration separation on black turbid matters obtained after the reaction is finished by using a vacuum pump, washing the black turbid matters for multiple times by using deionized water and absolute ethyl alcohol in the suction filtration process, finally drying the black turbid matters in a vacuum drying box at 60 ℃, and then collecting a target material sample. For the prepared Bi2S3/AgBiS2Characterization of nanoclusters by X-ray electron diffraction, as shown in fig. 1, the characteristic peaks marked by X in the spectrum correspond to Bi in the orthorhombic phase2S3(JCPDS No.84-0279)，
Characteristic peaks of the markers correspond to AgBiS of the cubic phase2(JCPDS No. 89-2046). XRD pattern proves that the reaction synthesizes Bi2S3/AgBiS2And (3) nano materials. Scanning electron microscopy of the prepared sampleThe mirror characterization is shown in FIGS. 2, 3 and 4, and the synthesized Bi can be seen2S3/AgBiS2The nanometer material is a nanometer cluster composed of a plurality of rod-shaped objects, and the structure of the nanometer cluster is uniform.
Using rhodamine B as degradation object, and testing Bi2S3/AgBiS2Photocatalytic properties of nanoclusters. The obtained AgBiS is put in a dark state2Adding a nano material into a rhodamine B solution (c is 20mg/L), magnetically stirring for 30min to enable a reaction system to reach adsorption-desorption balance, then catalyzing under the irradiation of a xenon lamp (adding an optical filter with the interval of 420 nm), taking out the solution at certain intervals, centrifuging to take supernatant, measuring the absorbance of the solution by using an ultraviolet-visible-near infrared spectrophotometer, calculating the degradation efficiency of the dye by using the absorbance at the maximum absorption wavelength, and showing an explanation effect graph as shown in figure 5. Can degrade about 70 percent of Bi in 180 minutes and is relatively single2S3And AgBiS2The nano material has better degradation effect and benefits from Bi2S3/AgBiS2The formed nanocluster structure, and the effective recombination of the two materials.
Example 2
Adding 2mmol of bismuth acetate, 3mmol of thiosemicarbazide and 0.02mmol of PVP into 20mL of ethylene glycol solution to prepare a solution A, performing ultrasonic treatment at room temperature until the solution A is fully dissolved, adding 1mmol of bismuth acetate, 2mmol of thiosemicarbazide, 1mmol of silver nitrate and 0.02mmol of PVP into 20mL of ethylene glycol solution to prepare a solution B, and preparing 0.1mmol of PEG into 10mL of ethylene glycol solution to prepare a solution C. And pouring the uniformly mixed solution A into the solution B, continuously stirring, adding the solution C, continuously stirring for 2 hours, then transferring the mixed solution into a polytetrafluoroethylene reaction kettle, keeping the temperature for 5 hours, performing suction filtration separation on black turbid matters obtained after the reaction is finished by using a vacuum pump, washing the black turbid matters for multiple times by using deionized water and absolute ethyl alcohol in the suction filtration process, finally drying the black turbid matters in a vacuum drying box at 60 ℃, and then collecting a target material sample. The prepared sample was characterized by scanning electron microscopy as shown in FIG. 6, which shows that synthesized Bi2S3/AgBiS2The nanomaterial is a nanocluster composed of a plurality of rods.
Example 3
Adding 2mmol of bismuth citrate, 3mmol of thiosemicarbazide and 0.03mmol of PVP into 20mL of ethylene glycol solution to prepare a solution A, magnetically stirring at room temperature until the bismuth citrate, the thiosemicarbazide, 1mmol of silver nitrate and 0.03mmol of PVP are fully dissolved to prepare a solution B, adding 1mmol of bismuth citrate, 2mmol of thiosemicarbazide, 1mmol of silver nitrate and 0.03mmol of PVP into 20mL of ethylene glycol solution to prepare a solution C, and dissolving 0.1mmol of PEG into 10mL of ethylene glycol to prepare a solution C. And pouring the uniformly mixed solution A into the solution B, continuously stirring, adding the solution C, continuously stirring for 2 hours, then transferring the mixed solution into a polytetrafluoroethylene reaction kettle for 180 ℃, keeping the temperature for 6 hours, performing suction filtration separation on black turbid matters obtained after the reaction is finished by using a vacuum pump, washing the black turbid matters for multiple times by using deionized water and absolute ethyl alcohol in the suction filtration process, finally drying the black turbid matters in a vacuum drying box at 60 ℃, and then collecting a target material sample. The prepared sample is characterized by a scanning electron microscope as shown in FIG. 7, and it can be seen that Bi is successfully synthesized2S3/AgBiS2The nanomaterial is a nanocluster composed of a plurality of rods.
Claims (10)
1. Bi2S3/AgBiS2The preparation method of the nanoclusters is characterized by comprising the following steps of:
(1) dissolving a bismuth source, a sulfur source and a surfactant polyvinylpyrrolidone (PVP) K30 in an ethylene glycol solvent in an ultrasonic state to prepare a uniformly dispersed solution A; dissolving a bismuth source, a sulfur source, a silver source and a surfactant polyvinylpyrrolidone (PVP) K30 into an ethylene glycol solution in an ultrasonic state to prepare a uniformly dispersed solution B; dissolving stable template polyethylene glycol (PEG) in glycol in an ultrasonic state to prepare a solution C;
(2) one-step solvothermal method for preparing Bi2S3/AgBiS2Nanoclusters: transferring the solution A into a glass container, slowly dripping the solution B into the glass container under magnetic stirring, uniformly mixing the solution A and the solution B, then adding the solution C into the mixed solution, and continuously stirring for a certain time;
(3) transferring the mixed solution in the step (2) into a polytetrafluoroethylene reaction kettle, putting the polytetrafluoroethylene reaction kettle into a drying oven, obtaining black turbid matters after the reaction is finished at a set temperature and time, performing suction filtration and separation by using a vacuum pump, and washing the turbid matters for multiple times by using deionized water and absolute ethyl alcohol in the suction filtration process;
(4) putting the solid obtained in the step (3) into an oven, and drying for a certain time at a set drying temperature to obtain Bi2S3/AgBiS2Nanocomposite, Bi obtained2S3/AgBiS2The nano composite material is a cluster consisting of dendritic short rods, and has high purity, uniform size and good dispersibility.
2. The Bi of claim 12S3/AgBiS2The preparation method of the nanoclusters is characterized in that the bismuth source is one or more of bismuth citrate, ammonium bismuth citrate and bismuth acetate.
3. The Bi of claim 1 or 22S3/AgBiS2The preparation method of the nanocluster is characterized in that the sulfur source is one or more of 1.3-dimethylthiourea, N-methylthiourea, thiosemicarbazide, tetramethylthiourea, 1.3-diethylthiourea and thiourea.
4. The Bi of claim 32S3/AgBiS2The preparation method of the nanoclusters is characterized in that the silver source is one or more of silver nitrate, silver perchlorate and silver acetate.
5. The Bi of claim 12S3/AgBiS2The preparation method of the nanoclusters is characterized in that the bismuth source in the solution A and the bismuth in the sulfur source: the molar ratio of sulfur is 2:3, and the molar ratio of bismuth in the bismuth source, the sulfur source and the silver source in the solution B is as follows: sulfur: the molar ratio of silver is 1: 2:1, and the molar concentration ratio of the bismuth source in the solution A to the bismuth source in the solution B is 2: 1.
6. The Bi of claim 52S3/AgBiS2Method for preparing nanoclusters, characterized in that the solution isThe concentration of PVP in the solution A and the solution B is kept consistent, and the molar concentration of the PVP is 0.1mmol-0.5 mmol.
7. The Bi of claim 62S3/AgBiS2The preparation method of the nanoclusters is characterized in that the molar concentration of PEG in the solution C is 0.1-0.5 mmol/L.
8. The Bi of claim 52S3/AgBiS2The preparation method of the nanoclusters is characterized in that the total molar concentration of bismuth and sulfur in the bismuth source and the sulfur source in the solution A is 0.05-1.5mol/L, and the total molar concentration of bismuth, sulfur and silver in the bismuth source, the sulfur source and the silver source in the solution B is 0.06-1.8 mol/L.
9. The Bi of claim 12S3/AgBiS2The method for preparing nanoclusters is characterized in that the stirring in the step (2) is continued for 2 to 4 hours.
10. The Bi of claim 92S3/AgBiS2The preparation method of the nanoclusters is characterized in that the reaction set temperature in the drying oven in the step (3) is 140-180 ℃, the reaction time is 2-6h, and the drying temperature in the vacuum drying oven in the step (4) is controlled at 60 ℃.
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| CN114774114A (en) * | 2022-03-28 | 2022-07-22 | 北京大学 | AgBiS2Preparation method of quantum dot superlattice and photoelectric detector thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102008966A (en) * | 2010-11-08 | 2011-04-13 | 安徽师范大学 | Sulfur group hetero-structure nano material, preparation method and application thereof |
| US10105687B1 (en) * | 2017-08-24 | 2018-10-23 | Imam Abdulrahman Bin Faisal University | Heterostructured Bi2S3—ZnS photocatalysts and methods thereof |
| CN111185196A (en) * | 2020-01-09 | 2020-05-22 | 南京工业大学 | Bamboo-leaf-shaped bismuth sulfide nano-sheet catalytic material and preparation method and application thereof |
-
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- 2021-08-30 CN CN202111006579.9A patent/CN114082425A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102008966A (en) * | 2010-11-08 | 2011-04-13 | 安徽师范大学 | Sulfur group hetero-structure nano material, preparation method and application thereof |
| US10105687B1 (en) * | 2017-08-24 | 2018-10-23 | Imam Abdulrahman Bin Faisal University | Heterostructured Bi2S3—ZnS photocatalysts and methods thereof |
| CN111185196A (en) * | 2020-01-09 | 2020-05-22 | 南京工业大学 | Bamboo-leaf-shaped bismuth sulfide nano-sheet catalytic material and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 田沙沙: "Bi2S3/AgBiS2复合纳米材料的合成及其在有机染料处理领域的应用", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》, no. 03, pages 46 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114774114A (en) * | 2022-03-28 | 2022-07-22 | 北京大学 | AgBiS2Preparation method of quantum dot superlattice and photoelectric detector thereof |
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