CN112371155A - g-C3N4/Zn0.2Cd0.8Preparation method of S composite material - Google Patents
g-C3N4/Zn0.2Cd0.8Preparation method of S composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 69
- 239000000463 material Substances 0.000 claims abstract description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 30
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000227 grinding Methods 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 12
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 14
- -1 polytetrafluoroethylene Polymers 0.000 claims description 14
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 14
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 14
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 7
- 229910052717 sulfur Inorganic materials 0.000 claims description 7
- 239000011593 sulfur Substances 0.000 claims description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract description 3
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- 238000001291 vacuum drying Methods 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 239000006104 solid solution Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013473 artificial intelligence Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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Abstract
g-C3N4/Zn0.2Cd0.8The preparation method of the S composite material comprises the following steps: HF was added with stirring to H2Preparing a mixed solution A in the O; taking Zn (CH)3COO)2·2H2O and Cd (CH)3COO)2·2H2Adding O into the mixed solution A and stirring to prepare a mixed solution B; adding thiourea into the mixed solution B to form a mixed solution C; carrying out hydrothermal reaction on the mixed solution C, washing with deionized water and ethanol, drying in vacuum, and grinding to obtain dendritic Zn0.2Cd0.8And (4) S material. Taking melamine in a magnetic boat, calcining in a muffle furnace, cooling to room temperature, grinding a sample to obtain g-C3N4. Crystalline Zn0.2Cd0.8The S material was added to water and stirred to give solution D. Taking g-C3N4And (4) adding the mixture into the solution D, and performing ultrasonic treatment to obtain a mixed solution E. After the mixed solution E is subjected to hydrothermal reaction, centrifugal washing is respectively carried out on the mixed solution E by deionized water and ethanol, vacuum drying is carried out, and grinding is carried out to obtain g-C3N4/Zn0.2Cd0.8And (4) S material. The preparation method has the advantages of simple preparation process and low cost, and the prepared material has high purity and strong crystallinity.
Description
Technical Field
The invention relates to a preparation method of a composite material, in particular to g-C3N4/Zn0.2Cd0.8A preparation method of the S composite material.
Background
In the modern society, along with the progress and development of the society, the degree of industrialization and artificial intelligence is higher and higher, the requirement on the used materials is higher and higher, and the traditional materials can not meet the use requirement, so that more and more functional materials and composite materials are developed rapidly. The II-VI compounds are the key points and hot spots of the current research, and are always paid much attention because of wide application prospects in the fields of semiconductor lasers, sensors, solid light emitting devices, solar cells and the like. Wherein Zn isxCd1-xAs a novel material with good photocatalytic performance, the S (x is more than or equal to 0 and less than or equal to 1) solid solution material is widely researched due to the adjustable transformation forbidden band width and the unique catalytic activity.
ZnxCd1-xThe S solid solution material is used as a semiconductor photocatalyst with direct wide band gap, the forbidden bandwidth of the S solid solution material is gradually reduced from 3.6eV to 2.3eV along with the increase of the using amount of Cd, and the S solid solution material has more proper forbidden bandwidthThe sunlight absorption device can well utilize and absorb a certain amount of visible light and a part of near ultraviolet light in sunlight. And the material has the advantages of low price, strong chemical stability, light corrosion resistance, easy recovery and the like, and has attracted extensive attention once coming out. ZnxCd1-xS has potential applications in many industrial fields and is often used in photoluminescent and photoconductor devices, photocatalytic degradation, hydrogen generation, phosphors and other optoelectronic fields. g-C3N4The preparation is simple, the cost is low, the stability is good, and the visible light response is realized, so that the preparation method is one of the most promising semiconductor materials. However, g-C3N4The practical application of the photo-induced charge is limited by the defects of easy recombination of the charge and weak hole oxidation capability. In all modification methods, only by constructing a heterostructure from two or more semiconductor materials can the advantages of multiple components be integrated, while the photo-generated charge separation efficiency is improved and the high redox capabilities of electrons and holes are maintained. Thus, different types of g-C were designed to be synthesized3N4Base heterojunction photocatalysts have gained widespread attention in recent years.
Disclosure of Invention
The invention aims to provide the g-C with low preparation cost and simple process3N4/Zn0.2Cd0.8Preparation method of S composite material, g-C prepared thereby3N4/Zn0.2Cd0.8The S material has good crystallinity.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method comprises the following steps: adding 0.2-0.4 mL of HF into 50-60 mL of H under stirring2Preparing a mixed solution A in the O;
step two: 0.75 to 1.5mmol of Zn (CH) is respectively taken3COO)2·2H2O and 3-6 mmol of Cd (CH)3COO)2·2H2O is represented by nZn：nCd1: 4, adding the mixture into the mixed solution A and stirring to prepare a mixed solution B;
step three: taking 6-12 mmol of thiourea as a sulfur source, and adding the thiourea into the mixed solution B under stirring to form a mixed solution C;
step four: adding the mixed solution C into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting at 120-150 ℃, after the reaction is finished, respectively centrifugally washing by deionized water and ethanol, drying in vacuum, and grinding to obtain dendritic Zn0.2Cd0.8S material;
step five: 5-8 g of melamine is put into a magnetic boat, calcined in a muffle furnace at 450-550 ℃, cooled to room temperature, and ground to obtain g-C3N4；
Step six: taking 1-3mol dendritic Zn0.2Cd0.8Adding the S material into 40-60mL of water, and uniformly stirring to obtain a solution D;
step seven: taking 10-20mg of g-C3N4Adding the mixed solution into the solution D, and uniformly dispersing by ultrasonic to obtain a mixed solution E;
step eight: adding the mixed solution E into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting at 100-140 ℃, after the reaction is finished, respectively centrifugally washing by deionized water and ethanol, drying in vacuum, and grinding to obtain g-C3N4/Zn0.2Cd0.8And (4) S material.
The reaction time of the fourth step is 10-18 h.
And the calcination time of the fifth step is 1-3 hours.
The ultrasonic dispersion time of the seventh step is 10-20 min.
And the reaction time of the step eight is 6-10 h.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention has simple preparation process and low cost, and simultaneously leads the g-C to be3N4With dendritic Zn0.2Cd0.8The S material is compounded, the two phases have matched valence conduction band potentials, the separation of electron holes is facilitated, the electrons and the holes are respectively limited in different object phases, the inhibition effect on the recombination of the photo-generated electrons and the holes is achieved, and the photo-catalytic performance is better. The prepared material has high purity and strong crystallinity, and can be applied to photocatalytic degradation of organic matters, photolysis of water to produce hydrogen or electronThe luminescent device and other fields can obtain good economic benefit and social benefit, and the application of the material can be well developed due to the excellent performance of the material.
Drawings
FIG. 1 is g-C prepared in example 33N4/Zn0.2Cd0.8XRD pattern of S material;
FIG. 2 is g-C prepared in example 33N4/Zn0.2Cd0.8SEM image of S material;
FIG. 3 is g-C prepared in example 33N4/Zn0.2Cd0.8The hydrogen production time of the S material is oriented.
Detailed Description
The invention is described in further detail below with reference to the following figures and examples:
example 1:
the method comprises the following steps: 0.2mL of HF was added to 50mL of H with stirring2Preparing a mixed solution A in the O;
step two: respectively taking 1mmol of Zn (CH)3COO)2·2H2O and 4mmol of Cd (CH)3COO)2·2H2Adding O into the mixed solution A and stirring to prepare a mixed solution B;
step three: taking 8mmol of thiourea as a sulfur source, and adding the thiourea into the mixed solution B under stirring to form a mixed solution C;
step four: adding the mixed solution C into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 10h at 120 ℃, after the reaction is finished, respectively centrifugally washing by deionized water and ethanol, drying in vacuum, and grinding to obtain dendritic Zn0.2Cd0.8S material;
step five: 5g of melamine is put into a magnetic boat, calcined for 1 hour at 450 ℃ in a muffle furnace, cooled to room temperature and ground to obtain g-C3N4；
Step six: taking 1mol of dendritic Zn0.2Cd0.8Adding the S material into 40mL of water, and uniformly stirring to obtain a solution D;
step seven: taking 10mg of g-C3N4Adding the mixture into the solution D, and adding the mixture into the solution D,performing ultrasonic dispersion for 20min to obtain a mixed solution E;
step eight: adding the mixed solution E into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 6 hours at 100 ℃, after the reaction is finished, respectively centrifugally washing by deionized water and ethanol, drying in vacuum, and grinding to obtain g-C3N4/Zn0.2Cd0.8And (4) S material.
Example 2:
the method comprises the following steps: 0.3mL of HF was added to 55mL of H with stirring2Preparing a mixed solution A in the O;
step two: 1.5mmol of Zn (CH) are respectively taken3COO)2·2H2O and 6mmol of Cd (CH)3COO)2·2H2Adding O into the mixed solution A and stirring to prepare a mixed solution B;
step three: taking 12mmol of thiourea as a sulfur source, and adding the thiourea into the mixed solution B under stirring to form a mixed solution C;
step four: adding the mixed solution C into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 16h at 140 ℃, after the reaction is finished, respectively centrifugally washing by deionized water and ethanol, drying in vacuum, and grinding to obtain dendritic Zn0.2Cd0.8S material;
step five: 6g of melamine is put into a magnetic boat, calcined for 3 hours at 500 ℃ in a muffle furnace, cooled to room temperature and ground to obtain g-C3N4；
Step six: taking 3mol dendritic Zn0.2Cd0.8Adding the S material into 50mL of water, and uniformly stirring to obtain a solution D;
step seven: taking 15mg of g-C3N4Adding the mixture into the solution D, and performing ultrasonic dispersion for 10min to obtain a mixed solution E;
step eight: adding the mixed solution E into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 10 hours at 120 ℃, after the reaction is finished, respectively centrifugally washing by deionized water and ethanol, drying in vacuum, and grinding to obtain g-C3N4/Zn0.2Cd0.8And (4) S material.
Example 3:
the method comprises the following steps: take 0.4mL of HFAdded to 60mL of H with stirring2Preparing a mixed solution A in the O;
step two: 0.75mmol of Zn (CH) is respectively taken3COO)2·2H2O and 3mmol of Cd (CH)3COO)2·2H2Adding O into the mixed solution A and stirring to prepare a mixed solution B;
step three: taking 6mmol of thiourea as a sulfur source, and adding the thiourea into the mixed solution B under stirring to form a mixed solution C;
step four: adding the mixed solution C into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 10 hours at 150 ℃, after the reaction is finished, respectively centrifugally washing by deionized water and ethanol, drying in vacuum, and grinding to obtain dendritic Zn0.2Cd0.8S material;
step five: taking 8g of melamine in a magnetic boat, calcining the melamine in a muffle furnace at 550 ℃ for 2 hours, cooling the melamine to room temperature, and grinding the sample to obtain g-C3N4；
Step six: taking 2mol of dendritic Zn0.2Cd0.8Adding the S material into 60mL of water, and uniformly stirring to obtain a solution D;
step seven: taking 20mg of g-C3N4Adding the mixed solution into the solution D, and performing ultrasonic dispersion for 15min to obtain a mixed solution E;
step eight: adding the mixed solution E into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 6 hours at 140 ℃, after the reaction is finished, respectively centrifugally washing by deionized water and ethanol, drying in vacuum, and grinding to obtain g-C3N4/Zn0.2Cd0.8And (4) S material.
It can be seen from FIG. 1 that the sample prepared in example 3 is Zn0.2Cd0.8S (PDF #49-1302) and g-C3N4(PDF # 87-1526).
From FIG. 2, it can be seen that g-C3N4Is uniformly distributed in Zn0.2Cd0.8The surface of the S material.
As can be seen from FIG. 3, the amount of hydrogen produced in one reaction period (3 hours) for the sample prepared in example 3 was 8.2mmol g-1And the performance is excellent.
Example 4:
the method comprises the following steps: 0.25mL of HF was added to 58mL of H with stirring2Preparing a mixed solution A in the O;
step two: 1.2mmol of Zn (CH) were respectively taken3COO)2·2H2O and 4.8mmol of Cd (CH)3COO)2·2H2Adding O into the mixed solution A and stirring to prepare a mixed solution B;
step three: taking 10mmol of thiourea as a sulfur source, and adding the thiourea into the mixed solution B under stirring to form a mixed solution C;
step four: adding the mixed solution C into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 18h at 130 ℃, after the reaction is finished, respectively centrifugally washing by deionized water and ethanol, drying in vacuum, and grinding to obtain dendritic Zn0.2Cd0.8S material;
step five: taking 7g of melamine in a magnetic boat, calcining the melamine in a muffle furnace at 480 ℃ for 3 hours, cooling the melamine to room temperature, and grinding the sample to obtain g-C3N4；
Step six: taking 1.5mol of dendritic Zn0.2Cd0.8Adding the S material into 45mL of water, and uniformly stirring to obtain a solution D;
step seven: taking 13mg of g-C3N4Adding the mixed solution into the solution D, and performing ultrasonic dispersion for 18min to obtain a mixed solution E;
step eight: adding the mixed solution E into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 8 hours at 130 ℃, after the reaction is finished, respectively centrifugally washing by deionized water and ethanol, drying in vacuum, and grinding to obtain g-C3N4/Zn0.2Cd0.8And (4) S material.
Example 5:
the method comprises the following steps: 0.35mL of HF was added to 53mL of H with stirring2Preparing a mixed solution A in the O;
step two: 0.8mmol of Zn (CH) is respectively taken3COO)2·2H2O and 3.2mmol of Cd (CH)3COO)2·2H2Adding O into the mixed solution A and stirring to prepare a mixed solution B;
step three: taking 9mmol of thiourea as a sulfur source, and adding the thiourea into the mixed solution B under stirring to form a mixed solution C;
step four: adding the mixed solution C into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 13h at 145 ℃, after the reaction is finished, respectively centrifugally washing by deionized water and ethanol, drying in vacuum, and grinding to obtain dendritic Zn0.2Cd0.8S material;
step five: 5g of melamine is put into a magnetic boat, calcined for 1 hour at 530 ℃ in a muffle furnace, cooled to room temperature and ground to obtain g-C3N4；
Step six: taking 2.5mol of dendritic Zn0.2Cd0.8Adding the S material into 55mL of water, and uniformly stirring to obtain a solution D;
step seven: taking 18mg of g-C3N4Adding the mixture into the solution D, and performing ultrasonic dispersion for 13min to obtain a mixed solution E;
step eight: adding the mixed solution E into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 7 hours at 135 ℃, after the reaction is finished, respectively centrifugally washing by deionized water and ethanol, drying in vacuum, and grinding to obtain g-C3N4/Zn0.2Cd0.8And (4) S material.
Claims (5)
1. g-C3N4/Zn0.2Cd0.8The preparation method of the S composite material is characterized by comprising the following steps of:
the method comprises the following steps: adding 0.2-0.4 mL of HF into 50-60 mL of H under stirring2Preparing a mixed solution A in the O;
step two: 0.75 to 1.5mmol of Zn (CH) is respectively taken3COO)2·2H2O and 3-6 mmol of Cd (CH)3COO)2·2H2O is represented by nZn：nCd1: 4, adding the mixture into the mixed solution A and stirring to prepare a mixed solution B;
step three: taking 6-12 mmol of thiourea as a sulfur source, and adding the thiourea into the mixed solution B under stirring to form a mixed solution C;
step four: adding the mixed solution C into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting at 120-150 ℃, and finishing the reactionAfter the formation, the Zn is respectively centrifugally washed by deionized water and ethanol, dried in vacuum and ground to obtain dendritic Zn0.2Cd0.8S material;
step five: 5-8 g of melamine is put into a magnetic boat, calcined in a muffle furnace at 450-550 ℃, cooled to room temperature, and ground to obtain g-C3N4；
Step six: taking 1-3mol dendritic Zn0.2Cd0.8Adding the S material into 40-60mL of water, and uniformly stirring to obtain a solution D;
step seven: taking 10-20mg of g-C3N4Adding the mixed solution into the solution D, and uniformly dispersing by ultrasonic to obtain a mixed solution E;
step eight: adding the mixed solution E into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting at 100-140 ℃, after the reaction is finished, respectively centrifugally washing by deionized water and ethanol, drying in vacuum, and grinding to obtain g-C3N4/Zn0.2Cd0.8And (4) S material.
2. g-C according to claim 13N4/Zn0.2Cd0.8The preparation method of the S composite material is characterized by comprising the following steps: the reaction time of the fourth step is 10-18 h.
3. g-C according to claim 13N4/Zn0.2Cd0.8The preparation method of the S composite material is characterized by comprising the following steps: and the calcination time of the fifth step is 1-3 hours.
4. g-C according to claim 13N4/Zn0.2Cd0.8The preparation method of the S composite material is characterized by comprising the following steps: the ultrasonic dispersion time of the seventh step is 10-20 min.
5. g-C according to claim 13N4/Zn0.2Cd0.8The preparation method of the S composite material is characterized by comprising the following steps: and the reaction time of the step eight is 6-10 h.
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