CN112250118B - Preparation method of composite material modified graphene, product and application thereof - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000012298 atmosphere Substances 0.000 claims abstract description 10
- 239000011261 inert gas Substances 0.000 claims abstract description 9
- 238000001514 detection method Methods 0.000 claims abstract description 8
- 239000013082 iron-based metal-organic framework Substances 0.000 claims abstract description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 21
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 20
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims description 17
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 9
- 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
- 238000002156 mixing Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 230000005855 radiation Effects 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical group [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims 1
- 239000000446 fuel Substances 0.000 abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010923 batch production Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000010406 cathode material Substances 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 2
- 230000004044 response Effects 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
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Abstract
The invention discloses a preparation method of composite material modified graphene, and a product and application thereof2O3/g‑C3N4And a layer of Fe-MOF structure is grown on the surface of the composite material, and then the composite material is roasted in an inert gas atmosphere to obtain alpha-Fe2O3/g‑C3N4Modified graphene composite structures. The preparation process is relatively simple, easy to operate and capable of realizing batch production. The material prepared by the method can be used in the fields of gas detection sensitive materials, lithium ion battery cathode materials, gas catalytic materials, photocatalytic materials, fuel cell catalysts and the like.
Description
Technical Field
The invention relates to a method for modifying graphene by using a composite material, in particular to alpha-Fe2O3/g-C3N4A preparation method of modified graphene, and a product and application thereof.
Background
Due to the unique structure, the graphene has very wide application value in various fields, such as fuel cells, gas detection, wearable equipment and the like. However, the simple graphene material used for gas detection has few active sites, so that the catalytic reaction with gas is difficult to perform, and the application of the graphene material in the field of gas detection is limited.
In the field of gas detection and gas remediation, alpha-Fe2O3Has better performance as a valence-variable metal oxide, but the poor conductivity of the metal oxide causes the performance to be difficult to fully exert, and the valence-variable metal oxide is mixed with g-C3N4And the graphene is compounded, so that the gas sensitive material for room temperature is expected to be developed.
The invention provides a simple method for realizing alpha-Fe2O3/g-C3N4The method for modifying the graphene has the advantages of simple preparation process and low preparation cost, and has great value for further promoting the practical application of the graphene.
Disclosure of Invention
The invention aims to provide a preparation method of composite material modified graphene.
Yet another object of the present invention is to: the composite material modified graphene product prepared by the method is provided.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: preparation method of composite material modified graphene, wherein the composite material is alpha-Fe2O3/g-C3N4Uniformly mixing urea, ferric salt and graphene, and roasting to obtain alpha-Fe2O3/g-C3N4And graphite, then growing a layer of Fe-MOF structure on the surface of the material, and finally roasting in an inert gas atmosphere to obtain alpha-Fe2O3/g-C3N4A modified graphene composite structure comprising the steps of:
the method comprises the following steps: grinding and mixing 20g of urea and 2 to 5mmol of ferric salt, adding into 20g of deionized water, and grinding for 20 to 30min; placing 5-10g of graphene in a mortar, continuously grinding for 20-30min, and freeze-drying the obtained slurry at-65 ℃ to obtain powder A;
step two: placing the powder A in a crucible with a cover, and roasting in a muffle furnace to obtain a sample B;
step three: taking 0.2 to 0.3mmol of Fe (NO)3)3•9H2Placing O, 0.1-0.15mmol of 2, 5-dihydroxy-1, 4-phthalic acid, 3-5mL of dimethylformamide, 0.1g of isopropanol and 0.1g of deionized water in a beaker, stirring for 2-3h, then adding the sample B obtained in the second step, stirring for 1-2h, reacting for 3-5h by adopting a microwave radiation heating method, after the reaction is finished, centrifuging and precipitating, and freeze-drying the obtained precipitate at-65 ℃ to obtain a sample C;
step four: roasting the sample C obtained in the third step in an inert gas atmosphere to obtain alpha-Fe2O3/g-C3N4Modifying graphene.
Wherein in the step one, the ferric salt is FeSO4•9H2O and FeCl2·4H2At least one of O.
And secondly, keeping the temperature of the baking atmosphere in air at 250-300 ℃ for 2-3 h, 350-400 ℃ for 1-2h and 500-600 ℃ for 2h, wherein the temperature rise speed is 1-5 ℃/min.
In the third step, the roasting gas atmosphere is argon or nitrogen, the roasting temperature is 550 to 650 ℃, the time is 2 to 3h, and the heating speed is 1 to 5 ℃/min. High purity argon or high purity nitrogen is preferred.
The invention also provides the composite material modified graphene prepared by any one of the methods.
The invention also provides application of the composite material modified graphene in a chlorobenzene gas detection sensitive material.
The preparation process is relatively simple, easy to operate and capable of realizing batch production. The material prepared by the method can be used in the fields of gas detection sensitive materials, lithium ion battery cathode materials, gas catalytic materials, photocatalytic materials, fuel cell catalysts and the like.
Drawings
FIG. 1 shows α -Fe according to the present invention2O3/g-C3N4The data graph of the modified graphene for detecting chlorobenzene gases with different concentrations shows that the material has excellent response characteristics to chlorobenzene with different concentrations.
Detailed Description
Example 1:
composite material modified graphene, wherein the composite material is alpha-Fe2O3/g-C3N4The method is characterized in that urea, ferric salt and graphene are uniformly mixed and roasted to obtain alpha-Fe2O3/g-C3N4And a layer of Fe-MOF structure is grown on the surface of the composite material, and finally, the composite material is roasted in an inert gas atmosphere to obtain alpha-Fe2O3/g-C3N4The modified graphene composite structure is prepared by the following steps:
the method comprises the following steps: 20g of urea and 2mmol of ferric salt FeSO are taken4•9H2Grinding and mixing O, adding into 20g of deionized water, and grinding for 20min; placing 5g of graphene in a mortar, continuously grinding for 30min, and freeze-drying the obtained slurry at-65 ℃ to obtain powder A;
step two: placing the powder A in a crucible with a cover, and roasting in a muffle furnace at the roasting temperature of 250 ℃ for 2h, 350 ℃ for 1h and 550 ℃ for 2h at the heating speed of 2 ℃/min to obtain a sample B;
step three: 0.2mmol of Fe (NO) was taken3)3•9H2Placing O, 0.1mmol of 2, 5-dihydroxy-1, 4-phthalic acid, 3mL of dimethylformamide, 0.1g of isopropanol and 0.1g of deionized water in a beaker, stirring for 3 hours, then adding the sample B obtained in the second step, stirring for 2 hours, reacting for 5 hours by adopting a microwave radiation heating method, after the reaction is finished, carrying out centrifugal precipitation, and freeze-drying the obtained precipitate at-65 ℃ to obtain a sample C;
step four: roasting the sample C in an inert gas high-purity argon atmosphere at the roasting temperature of 550 ℃, the roasting time of 3h and the heating speed of 1 ℃/min to obtain alpha-Fe2O3/g-C3N4Modifying graphene.
The powder prepared by the embodiment is dispersedly coated on a six-pin ceramic tube gas-sensitive test element, the test material has the response to chlorobenzene gas, the optimal response temperature to chlorobenzene is 180 ℃, the lowest response limit is 10ppb, and the sensitivity is 5.2. See figure 1 for details.
Example 2:
the composite material modified graphene is prepared by the following steps in the same way as the steps in the embodiment:
the method comprises the following steps: 20g of urea and 5mmol of ferric salt FeSO are taken4•9H2Grinding and mixing, adding into 20g of deionized water, and grinding for 30min; placing 5g of graphene in a mortar, continuously grinding for 30min, and freeze-drying the obtained slurry at-65 ℃ to obtain powder A;
step two: placing the powder A in a crucible with a cover, and roasting in a muffle furnace at the roasting temperature of 300 ℃ for 2h, 350 ℃ for 1h and 550 ℃ for 2h at the heating speed of 2 ℃/min to obtain a sample B;
step three: 0.3mmol of Fe (NO) was taken3)3•9H2Placing O, 0.15mmol of 2, 5-dihydroxy-1, 4-phthalic acid, 3mL of dimethylformamide, 0.1g of isopropanol and 0.1g of deionized water in a beaker, stirring for 3 hours, then adding the sample B, stirring for 2 hours, reacting for 5 hours by adopting a microwave radiation heating method, after the reaction is finished, carrying out centrifugal precipitation, and carrying out freeze drying on the obtained precipitate at-65 ℃ to obtain a sample C;
step four: roasting the sample C in an inert gas high-purity argon atmosphere at the roasting temperature of 550 ℃, the roasting time of 3h and the heating speed of 1 ℃/min to obtain alpha-Fe2O3/g-C3N4And modifying graphene.
The powder prepared by the embodiment is dispersedly coated on a six-pin ceramic tube gas-sensitive test element, the test material has the response to chlorobenzene gas, the optimal response temperature to chlorobenzene is 180 ℃, the lowest response limit is 10ppb, and the sensitivity is 8.4. See figure 1 for details.
Example 3:
the composite material modified graphene is prepared by the following steps in the same way as the steps in the embodiment:
the method comprises the following steps: 20g of urea and 2mmol of iron salt FeSO are taken4•9H2Grinding and mixing, adding into 20g of deionized water, and grinding for 30min; placing 10g of graphene in a mortar, continuously grinding for 30min, and freeze-drying the obtained slurry at-65 ℃ to obtain powder A;
step two: placing the powder A in a crucible with a cover, roasting in a muffle furnace, and keeping the roasting temperature at 300 ℃ for 2h, 350 ℃ for 1h and 550 ℃ for 2h at the heating speed of 5 ℃/min to obtain a sample B;
step three: 0.2mmol of Fe (NO) was taken3)3•9H2Placing O, 0.15mmol of 2, 5-dihydroxy-1, 4-phthalic acid, 3mL of dimethylformamide, 0.1g of isopropanol and 0.1g of deionized water in a beaker, stirring for 3 hours, then adding the sample B, stirring for 2 hours, reacting for 3 hours by adopting a microwave radiation heating method, after the reaction is finished, carrying out centrifugal precipitation, and carrying out freeze drying on the obtained precipitate at-65 ℃ to obtain a sample C;
step four: roasting the sample C in an inert gas high-purity argon atmosphere at the roasting temperature of 650 ℃ for 2h at the heating speed of 5 ℃/min to obtain alpha-Fe2O3/g-C3N4Modifying graphene.
The powder prepared by the embodiment is dispersedly coated on a six-pin ceramic tube gas-sensitive test element, the test material has the response to chlorobenzene gas, the optimal response temperature to chlorobenzene is 180 ℃, the lowest response limit is 10ppb, and the sensitivity is 3.24. See figure 1 for details.
The embodiments described above are presented to facilitate one of ordinary skill in the art to understand and practice the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications to the present invention based on the disclosure of the present invention within the protection scope of the present invention.
Claims (4)
1. Preparation method of composite material modified graphene, wherein the composite material is alpha-Fe2O3/g-C3N4The method is characterized in that the method comprises the following steps of,
uniformly mixing urea, ferric salt and graphene, and roasting to obtain alpha-Fe2O3/g-C3N4And graphene, and then growing a layer of Fe-MOF junction on the surface of the materialAnd finally, roasting in an inert gas atmosphere to obtain alpha-Fe2O3/g-C3N4A modified graphene composite structure comprising the steps of:
the method comprises the following steps: grinding and mixing 20g of urea and 2-5mmol of ferric salt, adding into 20g of deionized water, and grinding for 20-30min; placing 5-10 g of graphene in a mortar, continuously grinding for 20-30min, and freeze-drying the obtained slurry at-65 ℃ to obtain powder A;
step two: placing the powder A in a crucible with a cover, and roasting in a muffle furnace to obtain a sample B;
step three: taking 0.2 to 0.3mmol of Fe (NO)3)3•9H2Placing O, 0.1 to 0.15mmol of 2, 5-dihydroxy-1, 4-phthalic acid, 3 to 5mL of dimethylformamide, 0.1g of isopropanol and 0.1g of deionized water in a beaker, stirring for 2 to 3 hours, then adding the sample B obtained in the second step, stirring for 1 to 2 hours, reacting for 3 to 5 hours by adopting a microwave radiation heating method, after the reaction is finished, centrifuging and precipitating, and freeze-drying the obtained precipitate at-65 ℃ to obtain a sample C;
step four: roasting the sample C in an inert gas atmosphere to obtain alpha-Fe2O3/g-C3N4Modifying graphene; wherein
Step two, the baking atmosphere is air, the temperature is kept at 250 to 300 ℃ for 2 to 3 hours, at 350 to 400 ℃ for 1 to 2h and at 500 to 600 ℃ for 2 hours, and the temperature rising speed is 1 to 5 ℃/min;
in the fourth step, the atmosphere of the baking gas is argon or nitrogen, the baking temperature is 550 to 650 ℃, the time is 2 to 3h, and the heating speed is 1 to 5 ℃/min.
2. The preparation method of the composite material modified graphene according to claim 1, characterized by comprising the following steps: in the first step, the ferric salt is FeSO4•9H2O and FeCl2·4H2At least one of O.
3. Composite material modified graphene, characterized in that it is prepared according to the method of claim 1 or 2.
4. The application of the composite material modified graphene according to claim 3 in a chlorobenzene gas detection sensitive material.
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