CN107046137A - Porous LaCr oxides-carbon composite and its synthetic method - Google Patents
Porous LaCr oxides-carbon composite and its synthetic method Download PDFInfo
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
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- H01M4/90—Selection of catalytic material
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses porous LaCr oxides-carbon composite and its synthetic method, including：LaxCr2-xO3And carbon, the LaxCr2-xO3Uniformly mixed with carbon and form La Cr oxides-carbon composite layer, the La Cr oxides-carbon composite layer is provided with hole, wherein, in the porous La Cr oxides-carbon composite, carbon is 70-90wt%, 0.5≤x≤2, the hole is 200-400nm, is prepared using template impregnation sintering method.Porous La Cr oxides-carbon composite of the present invention can provide bigger specific surface area, with more avtive spots, so as to obtain higher catalytic performance.
Description
Technical field
The invention belongs to novel nano-material field, a kind of porous La Cr oxides-carbon composite and its synthetic method are related in particular to.
Background technology
Oxidationreduction (ORR) reaction is the deciding factor for determining fuel cell and metal-air battery, slow dynamics and complicated reaction mechanism an urgent demand have the new high performance catalyst of exploitation to accelerate reaction to carry out, and current Pt bases catalyst is still maximally effective ORR catalyst.But, Pt reserves are rare, expensive, and easily occur poisoning, dissolving under the working environment of fuel cell, cause its stability to decline.Based on this reason, a kind of inexpensive, efficient, non-noble metal ORR catalyst of active demand research.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of porous La Cr oxides-carbon composite (LaxCr2-xO3- Carbon) and its synthetic method, the porous La Cr oxides-carbon composite can provide bigger specific surface area and more avtive spots, obtain higher catalytic performance.
The purpose of the present invention is achieved by following technical proposals.
A kind of porous La Cr oxides-carbon composite, including：LaxCr2-xO3And carbon, the LaxCr2-xO3Uniformly mixed with carbon and form La Cr oxides-carbon composite layer, the La Cr oxides-carbon composite layer is provided with hole, wherein, in the porous La Cr oxides-carbon composite, carbon is 70-90wt%, and 0.5≤x≤2, the hole is 200-400nm.
In the above-mentioned technical solutions, the thickness of the La Cr oxides-carbon composite layer is 60-200nm, and thickness is preferably 80-150nm.
In the above-mentioned technical solutions, the hole is preferably 250-310nm.
In the above-mentioned technical solutions, carbon is 80-88wt%.
In above-mentioned technical proposal, the LaxCr2-xO3Particle is made up of two oxides material, and the oxide material is La2O3+La2CrO6、La2CrO6+LaCrO4Or LaCrO4+Cr2O3。
A kind of synthetic method of above-mentioned porous La Cr oxides-carbon composite, is carried out as steps described below：
Step 1, by La (NO3)3With Cr (NO3)3Mixture be added in solvent solution and dispersed, obtain reaction solution, wherein, by mol, La (NO3)3With Cr (NO3)3Ratio be (1-3)：(1-3)；The solvent solution is the homogeneous mixture solotion of ethylene glycol and methanol, and in the solvent solution, the volume ratio of ethylene glycol and methanol is 1：(0.9-1.2)；
In the step 1, in the reaction solution, lanthanum, chromium molar concentration and for 1.8-2.2mol/L, preferably 1.9-2.1mol/L.
In the step 1, the volume ratio of ethylene glycol and methanol is 1：(0.95-1.1).
In the step 1, by mol, La (NO3)3With Cr (NO3)3Ratio be (0.5-1)：(2-3).
In the step 1, dispersed selection stirring or ultrasound.
Step 2, a diameter of 200-320 nanometers PMMA microsphere colloid template is added in the reaction solution obtained by step 1, is soaked 20-30 hours, is filtered by vacuum, obtains being coated with the PMMA microsphere colloid template of reaction solution；
In the step 2, a diameter of 210-280nm of the PMMA microsphere colloid template.
In the step 2, PMMA microsphere colloid template is added in the reaction solution, is soaked 22-26 hours.
Step 3, the PMMA microsphere colloid template for being coated with reaction solution that prepared by step 2 into gained is dry 6-12 hours at 50-80 DEG C, after drying in a nitrogen atmosphere, 550-700 DEG C is risen to from the 20-25 DEG C of programming rate with 5-15 DEG C/min of room temperature, and heated 1-3 hours at 550-700 DEG C, 20-25 DEG C of room temperature is naturally cooled to, porous La Cr oxides-carbon composite is obtained.
In the step 3,580-650 DEG C is risen to from the 20-25 DEG C of programming rate with 6-10 DEG C/min of room temperature, and is heated 1.5-2.5 hours at 580-650 DEG C, 20-25 DEG C of room temperature is naturally cooled to, obtains porous La Cr oxides-carbon composite.
Compared to prior art, porous La Cr oxides-carbon composite of the invention can provide bigger specific surface area, with more avtive spots, so as to obtain higher catalytic performance.
Brief description of the drawings
Fig. 1 is porous La Cr oxides-carbon composite La of the invention0.5Cr1.5O3(LaxCr2-xO3, x=0.5) SEM figure；
Fig. 2 is carbon-free LaxCr2-xO3(x=0.5) the SEM figures of sample；
Fig. 3 is porous La Cr oxides-carbon composite La of the invention0.5Cr1.5O3(LaxCr2-xO3, x=0.5) SEM figure；
Fig. 4 is porous La Cr oxides-carbon composite La of the invention0.5Cr1.5O3(LaxCr2-xO3, x=0.5) TEM figure, scale be 0.2 micron；
Fig. 5 is the XRD of sample obtained by embodiment 1-3；
Fig. 6 is La0.5Cr1.5O3With the La of the present invention0.5Cr1.5O3- Carbon is in 1M KOH solution with 10mV s-1Sweep speed carry out dynamic polarization curved scanning.
Embodiment
In an embodiment of the present invention, the preparation process of PMMA microsphere colloid template is：
Go out to prepare PMMA microsphere as Material synthesis using methyl methacrylate and potassium peroxydisulfate, the particle size of monomer microballoon can be controlled by adjusting the addition of methyl methacrylate.Using sheet glass vertical sedimentation evaporation, PMMA microsphere is assembled into the glue crystal template of ordered arrangement.PMMA microsphere (about 220nm) to the glue crystal template for assembling ordered arrangement is with methyl methacrylate (MMA) for monomer, and potassium peroxydisulfate is made for initiator.88mL deionized waters, methyl methacrylate 5mL, are placed on magnetic stirring apparatus under circulation nitrogen protection and are stirred 15 minutes, add 7.5mL potassium persulfate solutions (containing potassium peroxydisulfate 0.059g), are sufficiently stirred for dissolving.Stop after logical nitrogen, heating schedule is set, it is to slowly warm up to 70 DEG C and is incubated 1.5h.It is then extremely cold, centrifuge, be dried to obtain white solid.Extracting waste solid, grinds to form after fine powder, according to mass ratio 1:40 ratio is mixed with water, stirs and ultrasonic disperse makes it become emulsion form again.Beaker is poured into, is placed in drying box at 50 DEG C and dries.Dry the white solid thin slice that strip occurs after finishing on sheet glass and walls of beaker, as PMMA microsphere colloid template.
Following documents are specifically may be referred to be prepared：
1)Sadakane,M.；Takahashi,C.；Kato,N.；Ogihara,H.；Nodasaka,Y.；Doi,Y.；Hinatsu,Y.and Ueda,W.Three-Dimensionally Ordered Macroporous(3DOM)Materials of Spinel-Type Mixed Iron Oxides.Synthesis,Structural Characterization,and Formation Mechanism of Inverse Opals with a Skeleton Structure.Bull.Chem.Soc.Jpn.2007,80(4),677-685.
2)Yuxi Liu,Hongxing Dai,Jiguang Deng,Lei Zhang,Chak Tong Au Three-dimensional ordered macroporous bismuth vanadates:PMMA-templating fabrication and excellent visible light-driven photocatalytic performance for phenol degradation.Nanoscale,2012,4,2317–2325.
In an embodiment of the present invention, the model JSM-7001F for the SEM that SEM photograph is used, manufacturer is Rigaku company；The model Tecinai G2F20 for the transmission electron microscope that TEM photos are used, manufacturer is Dutch Philip；XRD tests the model RJGAKU/DMAX of used X-ray diffractometer, and manufacturer is Rigaku company.
La (NO in following embodiments3)3With Cr (NO3)3Buy from Shanghai Aladdin biochemical technology limited company, wherein, Cr (NO3)3Using Cr (NO3)3 ·9H2O provides Cr, La (NO3)3Using La (NO3)3 ·6H2O provides La.
The porous La Cr oxides-carbon composite and its synthetic method of the present invention are described in detail with reference to the accompanying drawings and examples.
Embodiment 1
A kind of synthetic method of porous La Cr oxides-carbon composite, is carried out as steps described below：
Step 1, by La (NO3)3With Cr (NO3)3Mixture be added in solvent solution and be stirred until homogeneous it is scattered, obtain lanthanum, chromium molar concentration and for 2mol/L reaction solution, wherein, by mol, La (NO3)3With Cr (NO3)3Ratio be 3：1；The solvent solution is the homogeneous mixture solotion of ethylene glycol and methanol, and in the solvent solution, the volume ratio of ethylene glycol and methanol is 1：1；
Step 2, a diameter of 210-240 nanometers PMMA microsphere colloid template is added in the reaction solution obtained by step 1, is soaked 24 hours, is filtered by vacuum, obtains being coated with the PMMA microsphere colloid template of reaction solution；
Step 3, the PMMA microsphere colloid template for being coated with reaction solution that prepared by step 2 into gained is dried 10 hours at 60 DEG C, after drying in a nitrogen atmosphere, 600 DEG C are risen to from the 20-25 DEG C of programming rate with 10 DEG C/min of room temperature, and heated 2 hours at 600 DEG C, 20-25 DEG C of room temperature is naturally cooled to, porous La Cr oxides-carbon composite La of the present invention is obtained1.5Cr0.5O3-Carbon(LaxCr2-xO3- Carbon, x=1.5).
Embodiment 2
A kind of synthetic method of porous La Cr oxides-carbon composite, is carried out as steps described below：
Step 1, by La (NO3)3With Cr (NO3)3Mixture be added in solvent solution and be stirred until homogeneous it is scattered, obtain lanthanum, chromium molar concentration and for 2mol/L reaction solution, wherein, by mol, La (NO3)3With Cr (NO3)3Ratio be 1：1；The solvent solution is the homogeneous mixture solotion of ethylene glycol and methanol, and in the solvent solution, the volume ratio of ethylene glycol and methanol is 1：1；
Step 2, a diameter of 210-240 nanometers PMMA microsphere colloid template is added in the reaction solution obtained by step 1, is soaked 24 hours, is filtered by vacuum, obtains being coated with the PMMA microsphere colloid template of reaction solution；
Step 3, the PMMA microsphere colloid template for being coated with reaction solution that prepared by step 2 into gained is dried 10 hours at 60 DEG C, after drying in a nitrogen atmosphere, 600 DEG C are risen to from the 20-25 DEG C of programming rate with 10 DEG C/min of room temperature, and heated 2 hours at 600 DEG C, 20-25 DEG C of room temperature is naturally cooled to, porous La Cr oxides-carbon composite La of the present invention is obtained1Cr1O3-Carbon(LaxCr2-xO3- Carbon, x=1).
Embodiment 3
A kind of synthetic method of porous La Cr oxides-carbon composite, is carried out as steps described below：
Step 1, by La (NO3)3With Cr (NO3)3Mixture be added in solvent solution and be stirred until homogeneous it is scattered, obtain lanthanum, chromium molar concentration and for 2mol/L reaction solution, wherein, by mol, La (NO3)3With Cr (NO3)3Ratio be 1：3；The solvent solution is the homogeneous mixture solotion of ethylene glycol and methanol, and in the solvent solution, the volume ratio of ethylene glycol and methanol is 1：1；
Step 2, a diameter of 210-240 nanometers PMMA microsphere colloid template is added in the reaction solution obtained by step 1, is soaked 24 hours, is filtered by vacuum, obtains being coated with the PMMA microsphere colloid template of reaction solution；
Step 3, the PMMA microsphere colloid template for being coated with reaction solution that prepared by step 2 into gained is dried 10 hours at 60 DEG C, after drying in a nitrogen atmosphere, 600 DEG C are risen to from the 20-25 DEG C of programming rate with 10 DEG C/min of room temperature, and heated 2 hours at 600 DEG C, 20-25 DEG C of room temperature is naturally cooled to, porous La Cr oxides-carbon composite La of the present invention is obtained0.5Cr1.5O3(LaxCr2-x O3- Carbon, x=0.5).
Embodiment 4
A kind of La0.5Cr1.5O3Synthetic method (be used for contrast), carry out as steps described below：
Step 1, by La (NO3)3With Cr (NO3)3Mixture be added in solvent solution and be stirred until homogeneous it is scattered, obtain lanthanum, chromium molar concentration and for 2mol/L reaction solution, wherein, by mol, La (NO3)3With Cr (NO3)3Ratio be 1：3；The solvent solution is the homogeneous mixture solotion of ethylene glycol and methanol, and in the solvent solution, the volume ratio of ethylene glycol and methanol is 1：1；
Step 2, a diameter of 210-240 nanometers PMMA microsphere colloid template is added in the reaction solution obtained by step 1, is soaked 24 hours, is filtered by vacuum, obtains being coated with the PMMA microsphere colloid template of reaction solution；
Step 3, the PMMA microsphere colloid template for being coated with reaction solution that prepared by step 2 into gained is dried 10 hours at 60 DEG C, after drying in air atmosphere, 600 DEG C are risen to from the 20-25 DEG C of programming rate with 10 DEG C/min of room temperature, and heated 2 hours at 600 DEG C, 20-25 DEG C of room temperature is naturally cooled to, La is obtained0.5Cr1.5O3(LaxCr2-x O3, x=0.5).
Fig. 1,3 are porous La Cr oxides-carbon composite (La of the inventionxCr2-x O3- Carbon, x=0.5) SEM photograph, as seen from the figure, with carbon-free La shown in Fig. 2xCr2-xO3(x=0.5, specific preparation method reference implementation example 4) sample is compared, and due to the support of carbon skeleton, loose structure of the invention is not destroyed, and hole substantially becomes big, and connective and order improves.By test, La of the inventionxCr2-x O3- Carbon (x=0.5) specific surface area is 160m2/ g, the La prepared by embodiment 4xCr2-xO3(x=0.5) specific surface area is 151m2/ g, therefore the La of the present inventionxCr2-x O3- Carbon has bigger specific surface area.
Fig. 4 is porous La Cr oxides-carbon composite La of the invention0.5Cr1.5O3(LaxCr2-xO3, x=0.5) TEM figure, scale be 0.2 micron.
Fig. 5 is the XRD of sample obtained by embodiment 1-3, wherein, curve 1 is La2O3The XRD diffraction maximums of (purchasing from Shanghai Fu Sheng Industrial Co., Ltd.s, for being analyzed as standard spectrum), curve 2 is La obtained by embodiment 11.5Cr0.5O3-Carbon(La3CrO6- Carbon) XRD diffraction maximums, curve 3 be La obtained by embodiment 21Cr1O3-Carbon(LaCrO3- Carbon) XRD diffraction maximums, curve 4 be La obtained by embodiment 30.5Cr1.5O3-Carbon(LaCr3O6- Carbon) XRD diffraction maximums, curve 5 be Cr2O3The XRD diffraction maximums of (purchasing from Shanghai Fu Sheng Industrial Co., Ltd.s, for being analyzed as standard spectrum), in Figure 5, ● represent La2O3Phase, ◆ represent La2CrO6Phase, △ represents LaCrO4Phase, zero represents Cr2O3Phase.As seen from the figure, the thing of curve 2 to curve 4 respectively mutually is：La2O3+La2CrO6(curve 2), La2CrO6+LaCrO4(curve 3), LaCrO4+Cr2O3(curve 4), can be obtained, La of the invention0.5Cr1.5O3-Carbon、La1Cr1O3-Carbon、La1.5Cr0.5O3La in-CarbonxCr2-xO3Thing by two oxides material constitute.
Table 1 is porous La Cr oxides-carbon composite (La of the inventionxCr2-x O3- Carbon, x=0.5) EDS collection of illustrative plates, as seen from table, LaxCr2-x O3Phosphorus content atomic percent (carbon mass percent) in-Carbon (x=0.5) has reached 85%, and La/Cr atomic ratio is also substantially 1:3.
Above-mentioned porous La Cr oxides-carbon composite can be very good application as catalyst in redox reaction, and Fig. 6 compared for La0.5Cr1.5O3- Carbon (curve 2) and La0.5Cr1.5O3The hydrogen reduction performance of (curve 1), finds to introduce after carbon, La0.5Cr1.5O3Hydrogen reduction take-off potential diminishes, and current density expands 1 times or so, therefore, compared to La0.5Cr1.5O3, porous La Cr oxides-carbon composite (La of the invention0.5Cr1.5O3- Carbon) hydrogen reduction take-off potential it is minimum.(in three-electrode system working electrode, La of the inventionxCr2-x O3- Carbon reference electrodes are Ag/AgCl, and auxiliary electrode is platinum electrode)
Exemplary description has been done to the present invention above; it should be noted that; in the case where not departing from the core of the present invention, any simple deformation, modification or other skilled in the art can not spend the equivalent substitution of creative work to each fall within protection scope of the present invention.
Claims (10)
1. a kind of porous La Cr oxides-carbon composite, it is characterised in that including：LaxCr2-xO3And carbon, institute
State LaxCr2-xO3Uniformly mixed with carbon and form La Cr oxides-carbon composite layer, the La Cr oxides-carbon is combined
Layer is provided with hole, wherein, in the porous La Cr oxides-carbon composite, carbon is 70-90wt%, 0.5≤x
≤ 2, the hole is 200-400nm.
2. porous La Cr oxides-carbon composite according to claim 1, it is characterised in that the La Cr
The thickness of oxide-carbon composite layer is 60-200nm, and thickness is preferably 80-150nm, and the hole is preferably 250-310nm,
Carbon is preferably 80-88wt%.
3. porous La Cr oxides-carbon composite according to claim 1, it is characterised in that described
LaxCr2-xO3Particle is made up of two oxides material, and the oxide material is La2O3+La2CrO6、
La2CrO6+LaCrO4Or LaCrO4+Cr2O3。
4. a kind of synthesis side of porous La Cr oxides-carbon composite in 1-3 such as claim as described in any one
Method, it is characterised in that carry out as steps described below：
Step 1, by La (NO3)3With Cr (NO3)3Mixture be added in solvent solution and dispersed, reacted
Solution, wherein, by mol, La (NO3)3With Cr (NO3)3Ratio be (1-3)：(1-3)；The solvent solution
For ethylene glycol and the homogeneous mixture solotion of methanol, and in the solvent solution, the volume ratio of ethylene glycol and methanol is 1：
(0.9-1.2)；
Step 2, a diameter of 200-320 nanometers PMMA microsphere colloid mould is added in the reaction solution obtained by step 1
Plate, soaks 20-30 hours, is filtered by vacuum, obtains being coated with the PMMA microsphere colloid template of reaction solution；
Step 3, the PMMA microsphere colloid template for being coated with reaction solution for being prepared by step 2 into gained is dry at 50-80 DEG C
It is dry 6-12 hours, after drying in a nitrogen atmosphere, risen to from the 20-25 DEG C of programming rate with 5-15 DEG C/min of room temperature
550-700 DEG C, and heated 1-3 hours at 550-700 DEG C, 20-25 DEG C of room temperature is naturally cooled to, porous La Cr oxygen is obtained
Compound-carbon composite.
5. the synthetic method of porous La Cr oxides-carbon composite according to claim 4, it is characterised in that
In the step 1, in the reaction solution, lanthanum, chromium molar concentration and for 1.8-2.2mol/L.
6. the synthetic method of porous La Cr oxides-carbon composite according to claim 5, it is characterised in that
In the step 1, in the reaction solution, lanthanum, chromium molar concentration and for 1.9-2.1mol/L.
7. the synthetic method of porous La Cr oxides-carbon composite according to claim 4, it is characterised in that
The volume ratio of ethylene glycol and methanol is 1：(0.95-1.1)；By mol, La (NO3)3With Cr (NO3)3Ratio be (0.5-1)：
(2-3)。
8. the synthetic method of porous La Cr oxides-carbon composite according to claim 4, it is characterised in that
Dispersed selection stirring or ultrasound.
9. the synthetic method of porous La Cr oxides-carbon composite according to claim 4, it is characterised in that
In the step 2, a diameter of 210-280nm of the PMMA microsphere colloid template；Add in the reaction solution
Enter PMMA microsphere colloid template, soak 22-26 hours.
10. the synthetic method of porous La Cr oxides-carbon composite according to claim 4, its feature exists
In, in the step 3,580-650 DEG C is risen to from the 20-25 DEG C of programming rate with 6-10 DEG C/min of room temperature, and
580-650 DEG C is heated 1.5-2.5 hours, naturally cools to 20-25 DEG C of room temperature, is obtained porous La Cr oxides-carbon and is combined
Material.
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Application publication date: 20170815 |