CN113322487A - MoS based on supported electrocatalysis nitrogen reduction catalyst2-Fe3O4Preparation method of (1) - Google Patents
MoS based on supported electrocatalysis nitrogen reduction catalyst2-Fe3O4Preparation method of (1) Download PDFInfo
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Abstract
Ammonia, one of the most important modern industrial chemicals, plays an irreplaceable role in the fields of pesticides, fertilizers, textiles and the like. However, the production of ammonia is a difficult problem which is puzzling the world, and the traditional Habobosch method is still adopted in the industry at present, so that the reaction can be carried out under the condition of high temperature and high pressure, and a large amount of fossil raw materials are wasted and the environment is seriously polluted. Researchers are looking for a way to reduce nitrogen to ammonia under ambient conditions. The electrochemical catalysis nitrogen reduction reaction can convert N under the condition of environment under the condition of applied voltage2Reduction to NH3Mild reaction condition, less carbon discharge and raw materialAre readily available and have therefore gained increased attention in recent years. The strong dipole moment of N.ident.N, adsorption of nitrogen and severe hydrogen evolution reactions lead to electrochemical catalytic nitrogen reduction still facing difficulties. The development of high activity and high selectivity electrochemical catalysts is therefore key to the electrochemical catalysis of nitrogen reduction. The invention provides a method for preparing MoS by a hydrothermal method2Fe loaded on nanoflower3O4And its electrocatalytic nitrogen reduction application.
Description
Technical Field
The invention relates to the field of preparation and application of inorganic nano powder, in particular to a hydrothermal method based on MoS2Fe loaded on nanoflower3O4Catalyst on MoS2-Fe3O4A method and its application in the field of electrocatalytic nitrogen reduction.
Background
Ammonia as an efficient energy carrier (17.8% hydrogen density by weight) and is CO-free2The emission becomes energy convenient for transportation. With the increasing population, the world's demand for fertilizers and energy is increasing day by day, and the haber-bosch process, as the current industrial ammonia production primary means, produces over 500 tons of ammonia each year. However, the ammonia preparation process by the Haber-Bosch process has the disadvantages of high energy consumption, large scale and severe reaction conditions (200 atmospheric pressure and 400 atmospheric pressure)oC. Iron based catalyst) and 3 hundred million tons per year of CO2The problems of greenhouse effect and the like caused by the emission of the noble metal into the atmosphere are caused, and the noble metal resources are scarce and the price is high. Therefore, the production of non-noble metal catalysts that can fix the reduction of nitrogen to ammonia under mild conditions is the focus of research today.
Noble metals have excellent catalytic properties, but their expensive price and resource scarcity make them impossible to use in industrial production. The unique d-orbitals and rich electron density of transition metals compared to noble metals are beneficial for the weakening of N ≡ N. It is also advantageous for the formation of metallic H bonds, and therefore there is a need to improve the selectivity of the catalyst by means of interfacial engineering, doping and structural defects. A plurality of articles report that molybdenum disulfide has excellent electrochemical catalytic nitrogen reduction performance, and ferroferric oxide nanospheres are loadedLoaded to MoS2Nano flower of Feeder3O4Can provide H+A channel and can be connected with MoS2Collectively facilitating the running of eNRRs. Fe3O4Are nanospheres with a porous structure that allows the interior of the sphere to also provide active sites. MoS2The nanoflower is composed of nanosheets, can be fully contacted with an electrolyte, has an excellent specific surface area, and better exposes the edges of the nanosheets with higher catalytic activity. The combination of the two can better inhibit hydrogen evolution. In this, we invented Fe based on interface engineering3O4Nanosphere loading to MoS2The nanoflower is used as a catalyst for electrochemically catalyzing nitrogen reduction. Both can adsorb N together2The occurrence of electrochemically catalyzed nitrogen reduction is promoted by a synergistic effect. While Fe3O4Has hydrophobic property, and can well inhibit the generation of hydrogen evolution reaction.
Disclosure of Invention
One of the objects of the present invention is a MoS2-Fe3O4A novel method for preparing nano-rods.
The other purpose of the invention is to apply the synthesized nano rod-shaped catalyst to an electro-catalytic nitrogen reduction system.
The technical scheme of the invention is as follows:
1. catalyst MoS2-Fe3O4The preparation of (1) is carried out by mixing 0-4.0 g of polyethylene glycol HO (CH)2CH2O)nH and 0-10.0 g of sodium acetate CH3COONa is fully dispersed in 0-100 mL of ethylene glycol (CH)2OH)2In the method, 0 to 4.0 g of ferric chloride FeCl hexahydrate3·6H2Adding O into the mixed solution, uniformly dispersing, fully mixing the solution, transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, reacting for 2-10 h at 180-225 ℃, cooling to room temperature after the reaction is finished, washing the obtained product for 3-5 times to obtain Fe with holes3O4Taking 0.01-0.2 g of the prepared Fe with holes as nano microspheres3O4Dispersing the nano microspheres into 80 mL of deionized water, stirring for 60 minutes, and adding 0-1.0 g of sodium molybdate dihydrate Na2MoO4·2H2O and 0 to 1.0 g of Thiourea CH4N2Adding S into the uniformly dispersed solution, fully mixing, transferring into a reaction kettle with a polytetrafluoroethylene lining, reacting for 18-48 h at 180-225 ℃, cooling to room temperature after the reaction is finished, washing the obtained product for 3-5 times to obtain the product in MoS2Fe loaded on nanoflower3O4Catalyst on MoS2-Fe3O4。
2. The brand new H-shaped electro-catalytic electrolytic cell adopts the separation of two electrolytic chambers by a cation exchange membrane, thereby ensuring that H is continuously contained in the electrolyte+Supplying with Na as electrolyte2SO4The solution can prevent the consumption of the electro-catalytic nitrogen reduction catalyst, and the electrolytic cell can circulate water to regulate and control the electro-catalytic temperature at any time.
3.MoS2-Fe3O4The performance of the nano material and the ammonia yield of the electrocatalytic nitrogen reduction reaction reach 73.24 mu g h–1 mg–1The Faraday efficiency reaches 8.22%, and the ammonia yield and the Faraday efficiency are better.
Detailed description of the preferred embodiments
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and to the accompanying drawings, which are included to further illustrate features and advantages of the invention, and not to limit the scope of the invention as claimed.
Example 1
The first step is as follows: weighing 2.000 g of polyethylene glycol and 7.200 g of sodium acetate, fully dispersing into 80 mL of ethylene glycol, adding 2.700 g of ferric chloride hexahydrate into the mixed solution, uniformly dispersing, fully mixing the solution, transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, reacting for 8 hours at 200 ℃, cooling to room temperature after the reaction is finished, washing the obtained product for 5 times to obtain Fe with holes3O4Nano-microspheres;
the second step is that: taking 0.1 g of the Fe with holes prepared above3O4Dispersing the nano microspheres into 80 mL of deionized water, stirring for 60 minutes, adding 0.760 g of sodium molybdate dihydrate and 0.600 g of thiourea into the uniformly dispersed solution, and fully dispersingMixing, transferring into a reaction kettle with a polytetrafluoroethylene lining, reacting at 200 deg.C for 15 h, cooling to room temperature after reaction, washing the obtained product for 5 times to obtain MoS2Fe loaded on nanoflower3O4Catalyst on MoS2-Fe3O4；
The third step: in MoS2-Fe3O4For the working electrode, cyclic voltammetry was performed in a three-electrode system, activating the sample. The voltage range of the cyclic voltammetry test is-1.2-0V, the highest potential is 0V, the lowest potential is-1.2V, the starting potential is-1.2V, the ending potential is 0V, the scanning rate is 0.05V/s, the sampling interval is 0.001V, the standing time is 2 s, and the number of scanning sections is 500;
the fourth step: after cyclic voltammetry, the measurement is carried out in MoS2-Fe3O4Performing a linear voltage scanning test in a three-electrode system as a working electrode, wherein the voltage interval is-1.2-0V, the initial potential is-1.2V, the final potential is 0V, the scanning rate is 5 mV/s, the sampling interval is 0.001V, the standing time is 2 s, firstly, introducing argon into the electrolyte for 30 min, performing a first linear voltage scanning test after the argon is saturated, then introducing nitrogen into the electrolyte for 30 min, and performing a second linear voltage scanning test after the nitrogen is saturated;
the fifth step: in MoS2-Fe3O4For a working electrode, carrying out a long-time nitrogen reduction test on the catalyst, and setting the potential to be-0.91V, -1.01V, -1.11V, -1.21V and-1.31V respectively, wherein the running time is 7200 s;
the fourth step: ammonia production test
1. Drawing a working curve: by NH4Cl is a standard reagent, 0.0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 and 1.0 mu g/mL standard solutions are respectively prepared in 0.1 mol/L sodium sulfate solution, and the absorbance is tested by the chromogenic reaction. Taking 4 mL of standard solution, adding 0.75 mol/L of oxidant solution 50 multiplied by 10-3mL (containing 75 wt% NaOH and 75 wt% NaClO), then 0.05 mol/L colorant solution 0.5 mL (containing 40 wt% sodium salicylate and 32 wt% NaOH), and finally 5 wt% catalyst Na2[Fe(NO)(CN)5] ·2H2O solution 50X 10-3mL, standing at room temperature for developing for 1 h, performing spectral scanning in a wavelength range of 550 nm-800 nm by using an ultraviolet-visible spectrophotometer, and recording an absorbance value at 655 nm and a concentration to obtain a standard curve by drawing;
2. and (3) testing the yield of ammonia: respectively taking 4 mL of electrolyte after running for 2 h at each potential, adding 0.75 mol/L oxidant solution 50 multiplied by 10-3mL (containing 75 wt% NaOH and 75 wt% NaClO), then 0.05 mol/L colorant solution 0.5 mL (containing 40 wt% sodium salicylate and 32 wt% NaOH), and finally 5 wt% catalyst Na2[Fe(NO)(CN)5] ·2H2O solution 50X 10-3And (mL). Standing at room temperature for developing for 1 h, performing spectrum scanning within 550-800 nm by using an ultraviolet spectrum, and recording an absorbance value at 655 nm to finally obtain the concentration of ammonia. After data processing and calculation, MoS2-Mo2The effect of C applied to NRR is excellent, and the ammonia yield reaches 73.24 mu g h under-1.11V (relative to a standard hydrogen electrode)–1 mg–1 cat.The Faraday efficiency is as high as 8.22%.
Example 2
The first step is as follows: weighing 2.050 g of polyethylene glycol and 7.250 g of sodium acetate, fully dispersing into 80 mL of ethylene glycol, adding 2.740 g of ferric chloride hexahydrate into the mixed solution, uniformly dispersing, fully mixing the solution, transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, reacting for 8 hours at 200 ℃, cooling to room temperature after the reaction is finished, washing the obtained product for 5 times to obtain Fe with holes3O4Nano-microspheres;
the second step is that: 0.12 g of the porous Fe prepared above was taken3O4Dispersing the nano microspheres into 80 mL of deionized water, stirring for 60 minutes, adding 0.750 g of sodium molybdate dihydrate and 0.620 g of thiourea into the uniformly dispersed solution, fully mixing, transferring into a reaction kettle with a polytetrafluoroethylene lining, reacting for 15 hours at 200 ℃, cooling to room temperature after the reaction is finished, washing the obtained product for 5 times to obtain the product in MoS2Fe loaded on nanoflower3O4Catalyst on MoS2-Fe3O4；
The third step: in MoS2-Fe3O4For the working electrode, cyclic voltammetry was performed in a three-electrode system, activating the sample. The voltage range of the cyclic voltammetry test is-1.2-0V, the highest potential is 0V, the lowest potential is-1.2V, the starting potential is-1.2V, the ending potential is 0V, the scanning rate is 0.05V/s, the sampling interval is 0.001V, the standing time is 2 s, and the number of scanning sections is 500;
the fourth step: after cyclic voltammetry, the measurement is carried out in MoS2-Fe3O4And performing linear voltage scanning test in a three-electrode system as a working electrode, wherein the voltage interval is-1.2-0V, the initial potential is-1.2V, and the final potential is 0V. The scanning speed is 5 mV/s, the sampling interval is 0.001V, the standing time is 2 s, firstly, argon is introduced into the electrolyte for 30 min, the first linear voltage scanning test is carried out after the argon is saturated, then nitrogen is introduced into the electrolyte for 30 min, and the second linear voltage scanning test is carried out after the nitrogen is saturated;
the fifth step: in MoS2-Fe3O4For a working electrode, carrying out a long-time nitrogen reduction test on the catalyst, and setting the potential to be-0.91V, -1.01V, -1.11V, -1.21V and-1.31V respectively, wherein the running time is 7200 s;
the fourth step: ammonia production test
1. Drawing a working curve: by NH4Cl is a standard reagent, 0.0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 and 1.0 mu g/mL standard solutions are respectively prepared in 0.1 mol/L sodium sulfate solution, and the absorbance is tested by the chromogenic reaction. Taking 4 mL of standard solution, adding 0.75 mol/L of oxidant solution 50 multiplied by 10-3mL (containing 75 wt% NaOH and 75 wt% NaClO), then 0.05 mol/L colorant solution 0.5 mL (containing 40 wt% sodium salicylate and 32 wt% NaOH), and finally 5 wt% catalyst Na2[Fe(NO)(CN)5] ·2H2O solution 50X 10-3And (mL). Standing at room temperature for developing for 1 h, performing spectral scanning with an ultraviolet-visible spectrophotometer within the wavelength range of 550 nm-800 nm, and recording the absorbance value at 655 nm and the concentration to obtain a standard curveA wire;
2. and (3) testing the yield of ammonia: respectively taking 4 mL of electrolyte after running for 2 h at each potential, adding 0.75 mol/L oxidant solution 50 multiplied by 10-3mL (containing 75 wt% NaOH and 75 wt% NaClO), then 0.05 mol/L colorant solution 0.5 mL (containing 40 wt% sodium salicylate and 32 wt% NaOH), and finally 5 wt% catalyst Na2[Fe(NO)(CN)5] ·2H2O solution 50X 10-3And (mL). Standing at room temperature for developing for 1 h, performing spectrum scanning within 550-800 nm by using an ultraviolet spectrum, and recording an absorbance value at 655 nm to finally obtain the concentration of ammonia. After data processing and calculation, MoS2-Mo2The effect of C applied to NRR is excellent, and the ammonia yield reaches 73.11 mu g h under-1.11V (relative to a standard hydrogen electrode)–1 mg–1 cat.The Faraday efficiency is as high as 8.20%.
Example 3
The first step is as follows: weighing 2.010 g of polyethylene glycol and 7.200 g of sodium acetate, fully dispersing into 80 mL of ethylene glycol, adding 2.690 g of ferric chloride hexahydrate into the mixed solution, uniformly dispersing, fully mixing the solution, transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, reacting for 8 hours at 200 ℃, cooling to room temperature after the reaction is finished, washing the obtained product for 5 times to obtain Fe with holes3O4Nano-microspheres;
the second step is that: 0.102 g of the Fe with holes prepared above was taken3O4Dispersing the nano microspheres into 80 mL of deionized water, stirring for 60 minutes, adding 0.768 g of sodium molybdate dihydrate and 0.610 g of thiourea into the uniformly dispersed solution, fully mixing, transferring into a reaction kettle with a polytetrafluoroethylene lining, reacting for 15 hours at 200 ℃, cooling to room temperature after the reaction is finished, washing the obtained product for 5 times to obtain the product in MoS2Fe loaded on nanoflower3O4Catalyst on MoS2-Fe3O4；
The third step: in MoS2-Fe3O4For the working electrode, cyclic voltammetry was performed in a three-electrode system, activating the sample. The voltage range of the cyclic voltammetry test is-1.2-0V, and the highest potential0V, the lowest potential is-1.2V, the starting potential is-1.2V, the ending potential is 0V, the scanning rate is 0.05V/s, the sampling interval is 0.001V, the standing time is 2 s, and the number of scanning segments is 500;
the fourth step: after cyclic voltammetry, the measurement is carried out in MoS2-Fe3O4Performing a linear voltage scanning test in a three-electrode system as a working electrode, wherein the voltage interval is-1.2-0V, the initial potential is-1.2V, the final potential is 0V, the scanning rate is 5 mV/s, the sampling interval is 0.001V, the standing time is 2 s, firstly, introducing argon into the electrolyte for 30 min, performing a first linear voltage scanning test after the argon is saturated, then introducing nitrogen into the electrolyte for 30 min, and performing a second linear voltage scanning test after the nitrogen is saturated;
the fifth step: in MoS2-Fe3O4For a working electrode, carrying out a long-time nitrogen reduction test on the catalyst, and setting the potential to be-0.91V, -1.01V, -1.11V, -1.21V and-1.31V respectively, wherein the running time is 7200 s;
the fourth step: ammonia production test
1. Drawing a working curve: by NH4Cl is a standard reagent, 0.0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 and 1.0 mu g/mL standard solutions are respectively prepared in 0.1 mol/L sodium sulfate solution, and the absorbance is tested by the chromogenic reaction. Taking 4 mL of standard solution, adding 0.75 mol/L of oxidant solution 50 multiplied by 10-3mL (containing 75 wt% NaOH and 75 wt% NaClO), then 0.05 mol/L colorant solution 0.5 mL (containing 40 wt% sodium salicylate and 32 wt% NaOH), and finally 5 wt% catalyst Na2[Fe(NO)(CN)5] ·2H2O solution 50X 10-3And (mL). Standing at room temperature for developing for 1 h, performing spectral scanning in the wavelength range of 550-800 nm by using an ultraviolet-visible spectrophotometer, and recording the absorbance value at 655 nm and plotting the concentration to obtain a standard curve;
2. and (3) testing the yield of ammonia: respectively taking 4 mL of electrolyte after running for 2 h at each potential, adding 0.75 mol/L oxidant solution 50 multiplied by 10-3mL (containing 75 wt% NaOH and 75 wt% NaClO), and then 0.05 mol/L colorant solution was added0.5 mL (containing 40 wt% sodium salicylate and 32 wt% NaOH), and finally 5 wt% of catalyst Na2[Fe(NO)(CN)5] ·2H2O solution 50X 10-3And (mL). Standing at room temperature for developing for 1 h, performing spectrum scanning within 550-800 nm by using an ultraviolet spectrum, and recording an absorbance value at 655 nm to finally obtain the concentration of ammonia. After data processing and calculation, MoS2-Mo2The effect of C applied to NRR is excellent, and the ammonia yield reaches 73.36 mu g h under-1.11V (relative to a standard hydrogen electrode)–1 mg–1 cat.The Faraday efficiency is as high as 8.24%.
Claims (2)
1. Electro-catalytic nitrogen reduction catalyst MoS2-Fe3O4The supported catalyst MoS2-Fe3O4The preparation method is characterized by comprising the following steps:
(1) 0 to 4.0 g of polyethylene glycol HO (CH)2CH2O)nH and 0-10.0 g of sodium acetate CH3COONa is fully dispersed in 0-100 mL of ethylene glycol (CH)2OH)2In the method, 0 to 4.0 g of ferric chloride FeCl hexahydrate3·6H2Adding O into the mixed solution, uniformly dispersing, fully mixing the solution, transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, reacting for 2-10 h at 180-225 ℃, cooling to room temperature after the reaction is finished, washing the obtained product for 3-5 times to obtain Fe with holes3O4Nano-microspheres;
(2) taking 0.01-0.2 g of the Fe with holes3O4Dispersing the nano microspheres into 80 mL of deionized water, stirring for 60 minutes, and adding 0-1.0 g of sodium molybdate dihydrate Na2MoO4·2H2O and 0 to 1.0 g of Thiourea CH4N2Adding S into the uniformly dispersed solution, fully mixing, transferring into a reaction kettle with a polytetrafluoroethylene lining, reacting for 18-48 h at 180-225 ℃, cooling to room temperature after the reaction is finished, washing the obtained product for 3-5 times to obtain the product in MoS2Fe loaded on nanoflower3O4Catalyst on MoS2-Fe3O4；
Electro-catalytic nitrogen reduction catalyst MoS2-Fe3O4The electrocatalytic nitrogen reduction process is characterized by comprising the following steps: the electrocatalytic nitrogen reduction process adopts a three-electrode system, tests are carried out through an electrochemical workstation, and an electrolytic tank used for the tests is an H-shaped electrolytic tank which is self-designed and uses MoS2-Fe3O4A carbon rod is used as a working electrode, an Ag/AgCl electrode is used as a reference electrode, and 0.1-1.5 mol/L of sodium sulfate solution Na is used2SO4Is an electrolyte.
2. The rod-shaped catalyst MoS according to claim 12-Fe3O4The molybdenum source reagent is ammonium molybdate tetrahydrate H8MoN2O4·4H2O, Anhydrous ammonium molybdate H8MoN2O4Sodium molybdate dihydrate Na2MoO4·4H2One or more of O, the concentration of the molybdenum source solution is 0.01-1.0 mol/L, the iron source reagent is one or more of ferric nitrate nonahydrate, ferric trichloride hexahydrate and ferric sulfate, and the concentration of the iron source solution is 0.1-0.2 mol/L.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113862717A (en) * | 2021-10-12 | 2021-12-31 | 济南大学 | Rose type catalyst VS2@Bi2O3Preparation method of/CC and application thereof in nitrogen reduction |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107999114A (en) * | 2017-12-19 | 2018-05-08 | 成都玖奇新材料科技有限公司 | Electrochemical reduction nitrogen ammonia non-precious metal catalyst |
| CN109806889A (en) * | 2019-02-25 | 2019-05-28 | 宁夏大学 | A kind of molybdenum disulfide/ferroferric oxide magnetic nano composite material and preparation method and application |
| CN111001420A (en) * | 2019-12-13 | 2020-04-14 | 济南大学 | Electro-catalytic nitrogen reduction catalyst MoS2-Fe(OH)3Preparation method of/CC |
| CN111068718A (en) * | 2020-01-08 | 2020-04-28 | 济南大学 | Preparation of nano spherical sulfur-doped iron oxide and application of nano spherical sulfur-doped iron oxide in electrocatalytic nitrogen reduction |
| CN111304689A (en) * | 2018-12-11 | 2020-06-19 | 深圳先进技术研究院 | Titanium diboride/boron carbide composite electrode and preparation method and application thereof |
| CN112226781A (en) * | 2020-09-30 | 2021-01-15 | 湖南大学 | Device and method for generating ammonia gas from nitrogen |
-
2021
- 2021-06-09 CN CN202110641475.9A patent/CN113322487B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107999114A (en) * | 2017-12-19 | 2018-05-08 | 成都玖奇新材料科技有限公司 | Electrochemical reduction nitrogen ammonia non-precious metal catalyst |
| CN111304689A (en) * | 2018-12-11 | 2020-06-19 | 深圳先进技术研究院 | Titanium diboride/boron carbide composite electrode and preparation method and application thereof |
| CN109806889A (en) * | 2019-02-25 | 2019-05-28 | 宁夏大学 | A kind of molybdenum disulfide/ferroferric oxide magnetic nano composite material and preparation method and application |
| CN111001420A (en) * | 2019-12-13 | 2020-04-14 | 济南大学 | Electro-catalytic nitrogen reduction catalyst MoS2-Fe(OH)3Preparation method of/CC |
| CN111068718A (en) * | 2020-01-08 | 2020-04-28 | 济南大学 | Preparation of nano spherical sulfur-doped iron oxide and application of nano spherical sulfur-doped iron oxide in electrocatalytic nitrogen reduction |
| CN112226781A (en) * | 2020-09-30 | 2021-01-15 | 湖南大学 | Device and method for generating ammonia gas from nitrogen |
Non-Patent Citations (2)
| Title |
|---|
| JIAOLONG LIU ET AL.: "Hierarchical flower-like Fe3O4/MoS2 composites for selective broadband electromagnetic wave absorption performance", COMPOSITES: PART A * |
| LEI LIU ET AL.: "A green design for lubrication: multi-functional system containing Fe3O4@MoS2 nanohybrid", ACS SUSTAINABLE CHEMISTRY & ENGINEERING * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113862717A (en) * | 2021-10-12 | 2021-12-31 | 济南大学 | Rose type catalyst VS2@Bi2O3Preparation method of/CC and application thereof in nitrogen reduction |
| CN113862717B (en) * | 2021-10-12 | 2023-06-09 | 济南大学 | Rose-type catalyst VS 2 @Bi 2 O 3 Preparation method of/CC and application thereof in nitrogen reduction |
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