CN108745373A - A kind of preparation method of precious metal alloys/carbon material supported type catalyst - Google Patents
A kind of preparation method of precious metal alloys/carbon material supported type catalyst Download PDFInfo
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- CN108745373A CN108745373A CN201810620407.2A CN201810620407A CN108745373A CN 108745373 A CN108745373 A CN 108745373A CN 201810620407 A CN201810620407 A CN 201810620407A CN 108745373 A CN108745373 A CN 108745373A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8913—Cobalt and noble metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/892—Nickel and noble metals
Abstract
A kind of preparation method of precious metal alloys/carbon material supported type catalyst, 1) prepare at least one precious metal salt or acid and at least one kind of transition metal salt or the mixed solution of acid and carbon material and dispersant；1) mixed solution obtained is prepared into composite powder by being sprayed to the quick-drying method in high-temp solid surface；3) 2) composite powder obtained is annealed in a reducing atmosphere, makes metallic alloying, obtain precious metal alloys/carbon material supported type catalyst.The precious metal salt or acid, transition metal salt or acid and the mixed solution of carbon material and dispersant include precious metal salt or acid, transition metal salt or acid, carbon material, dispersant and solvent；The present invention utilizes the rapid evaporation of water when being sprayed to the rapid draing of high-temp solid surface, and precious metal alloys particle is separated by carbon material powder, alloying pellet is not grown up in annealing process, and the tiny precious metal alloys nano particle uniform load of size is in carbon material surface.
Description
Technical field
The present invention relates to a kind of preparation methods of precious metal alloys/carbon material supported type catalyst, belong to nano material conjunction
At with electrochemical catalysis field.
Background technology
Precious metal alloys nanocatalyst has suitable suction/desorption ability to reactants and products, in environmental catalysis, combustion
Particularly important role is play in the heterogeneous catalytic reactions such as material battery, fine chemistry industry.For example, 3 effects of purification vehicle exhaust are urged
The active component of agent is exactly platinum family element, and platinum base nano structure electrode shows excellent in fuel cell electrocatalytic reaction
Performance.Since noble metal reserves are rare and expensive, reduce its usage amount but maintain or even increase simultaneously its catalytic performance and
Its cyclic utilization rate becomes the focus of research.Precious metal alloys grain diameter smaller, thinner nanocatalyst are prepared, it can
The mass activity and service efficiency of noble metal are improved to increase its specific surface area.
Currently, the preparation method in relation to precious metal alloys loaded catalyst is a lot of, low temperature organic liquid phase reduction method, micro emulsion
Liquid method, vapour deposition process, electrochemical deposition method andPool-high temperature reduction method.In contrast, related high temperature reduction method is prepared expensive
Metal alloy catalyst has its unique advantage.Since the crystal structure of alloy needed for obtaining can be easy to control in high annealing,
The required equipment of this method and raw material are commonplace, and process is simply easy to control, and are hopeful large-scale production reduction
Production cost.But precious metal alloys catalyst particle size size and consistency, crystal knot prepared by current high temperature reduction method
The problem of controllability of structure etc., still than more prominent, largely affects the catalytic performance of precious metal alloys catalyst.
In addition, common spray drying is by the heating realization drying in the gas of heat after solution atomization, due to dry speed
Spend slow, dried powder particle is bigger.
Invention content
For problem of the prior art, the object of the present invention is to provide a kind of precious metal alloys and carbon material supported type
The preparation method of catalyst.The characteristics of being higher than gas using solid conductive heat speed, by mixed solution by the method for spraying by liquid
Drop is ejected into high-temp solid surface and realizes rapid draing.The fast rapid-curing cutback that the rapid evaporation of water is realized when by being sprayed to the surface of solids
Dry and precious metal alloys particle is separated by carbon material powder, keeps precious metal alloys particle not grow during reduced anneal
Precious metal alloys/carbon materials of the tiny precious metal alloys nano particle uniform load of big feature preparation size in carbon material surface
Expect loaded catalyst.
The present invention is achieved by the following technical solutions：A kind of system of precious metal alloys and carbon material supported type catalyst
Preparation Method, which is characterized in that include the following steps：
Step 1 prepares at least one precious metal salt or acid and at least one kind of transition metal salt or acid and carbon material and dispersion
The mixed solution of agent；
Step 2 prepares the mixed solution that step 1 is obtained by being sprayed to the quick-drying method in high-temp solid surface
Composite powder；
Step 3 anneals the composite powder that step 2 obtains in a reducing atmosphere, make it is metallic alloying, obtain noble metal conjunction
Gold/carbon material supported type catalyst；
The mixed solution packet of precious metal salt described in step 1 or acid, transition metal salt or acid and carbon material and dispersant
Include precious metal salt or acid, transition metal salt or acid, carbon material, dispersant and solvent；
The precious metal salt or acid include：Platinum, gold, silver, rhodium, palladium, iridium, the nitrate of ruthenium, chlorate, acetate, oxalic acid
Salt and chloroplatinic acid, gold chloride；
The transition metal salt or acid include：The nitre of iron, cobalt, nickel, copper, molybdenum, tungsten, tantalum, tungsten, zinc, manganese, titanium, chromium, manganese, gallium
Hydrochlorate, chlorate, acetate, oxalates and molybdic acid, wolframic acid；
The carbon material includes：Conductive black, graphite, graphene and graphene oxide；
The dispersant includes：Can dispersed electro-conductive carbon black, graphite and graphene in water high molecular material, such as it is water-soluble
Property high-molecular compound polyvinylpyrrolidone (PVP), polyacrylamide (PAM) etc.；
The solvent for constituting solution is water.
The molar ratio of precious metal ion and transition metal ions is 1 in solution described in step 1：(0.1~20)；Noble metal
Ion adds the molar ratio of the sum of transition metal ions and carbon material to be 1:(0.5~10)；The weight ratio of carbon material and dispersant is
1:(0.01~10)；The molar ratio of solute (precious metal salt or acid, transition metal salt or acid, carbon material and dispersant) and water is 1:
(2~500)；
Dry method described in step 2 is by the way that mixed solution is sprayed to high-temp solid surface, solid conductive heat is utilized
Speed is faster than the characteristics of gas, realizes that the rapid draing of mixing liquid prepares composite powder；
Alloying annealing temperature described in step 3 is less than 1000 DEG C, and best temperature is 400 DEG C~700 DEG C；
Reducing atmosphere described in step 3 is H2、H2/N2Mixed gas, H2/ Ar mixed gas.
Advantageous effect：The present invention is using the rapid evaporation and precious metal alloys powder of water when spraying rapid draing by carbon
Material powder separates, and while required crystal structure precious metal alloys are obtained during reduced anneal, keeps precious metal alloys
The characteristics of particle is not grown up is prepared for the tiny precious metal alloys nano particle of size and is evenly distributed on carbon material.Use the party
Method prepare precious metal alloys Nanoparticulate composition is uniform, size is tiny.This method is simple for process, and production efficiency is high, can scale
Metaplasia produces precious metal alloys/carbon material supported type catalyst.
Description of the drawings
Pt prepared by Fig. 1 different conditions3The transmission electron microscope photo of Co/ conductive blacks；Wherein (a), (b) respectively refer to Pt3Co/C
It is height in the upper right corner of 500 DEG C (a), the transmission electron microscope photo of 700 DEG C of (b) hydrogen annealing samples, (a), (b) transmission electron microscope photo
Differentiate photo.
Pt prepared by Fig. 2 different conditions3The XRD results of Co/ conductive blacks；Wherein (a), (b) respectively refer to Pt3Co/C is 500
DEG C and 700 DEG C of hydrogen annealing samples X-ray diffraction spectrum.
Pt prepared by Fig. 3 different conditions3The hydrogen reduction performance of Co/ conductive blacks and commercialization Pt/ conductive black electrodes；
Pt3500 DEG C, 700 DEG C hydrogen annealings of Co/C and commercialization Pt/ conductive blacks electrode are in saturation oxygen 0.1M HClO4Divide in electrolyte
Polarization curves of oxygen reduction (the rotating speed 1600rpm not measured；Sweep speed is 20mV/s)
Pt prepared by Fig. 4 different conditions3The hydrogen reduction cycle characteristics of Co/ conductor charcoal black electrodes.Wherein (a) Pt3Co/C 500
DEG C and (b) Pt3700 DEG C of annealing specimens of Co/C are being saturated oxygen 0.1M HClO after having carried out 5000 times and 10000 times cycles4Electricity
Solve liquid (rotating speed 1600rpm；Sweep speed is 20mV/s) in the redox polarization curve that measures.
Specific implementation mode
With reference to specific example, the present invention is described in detail.
Embodiment 1
Pt3The preparation of Co/ conductive black loaded catalysts
Step 1,1 gram of six water chloroplatinic acid is taken【H2PtCl6·6H2O】, 0.187 gram of cobalt nitrate hexahydrate【Co(NO3)2·6H2O】
In 150mL deionized waters, after ultrasonic dissolution 10min, adds 1.66 grams of Vulcan XC-72R carbon blacks and 1.66 grams of PVP are (flat
Average molecular weight is 8000) and ultrasound is uniformly mixed for 20 minutes.The molar ratio of platinum and cobalt atom is 3:1, platinum adds the weight of cobalt and leads
The weight ratio of electric carbon black is 1:4.
Step 2, the mixed solution mixed is obtained into dry mixed powder by quick-drying method of spraying：It will be tiny
Droplet to be ejected into temperature be on 270 DEG C of quartz plate, rapid evaporation aqueous solution obtains dry mixed-powder, and spray velocity is
20 milliliters of solution/minutes.
Step 3, the dry mixed powder that step 2 obtains is removed from quartz plate, in hydrogen annealing 60 minutes, annealing
Temperature is 500 DEG C, obtains Pt3Co/ conductive black loaded catalysts.
Effect：Pt prepared by embodiment 13The TEM photos of Co/ conductive blacks are as shown in Figure 1, Pt3Co alloy nanoparticles are flat
Equal size 4.4nm.The results are shown in Figure 2 by XRD after 500 DEG C of temperature hydrogen reducings, Pt3The crystal structure of Co nano particles is
Disordered structure.In order to test Pt3The oxygen reduction catalytic activity of Co/ conductive blacks will prepare Pt3Co/ conductive blacks,
Hydrogen reduction performance is tested in 0.1M perchloric acid, the results are shown in Figure 3, Pt3Co/ conductive blacks oxygen reduction catalytic activity can be higher than
Commercial Pt/ conductive black catalyst.Pt3The oxygen reduction catalytic activity of Co conductive blacks is durable in 0.1M perchloric acid solutions
Property test results are shown in figure 4, at 10,000 times recycle after reduce it is smaller.
Embodiment 2
Pt3The preparation of Co/ conductive black loaded catalysts
This example is the change case of embodiment 1.Other implementation conditions are with embodiment 1, variation place：In step 3
The temperature of hydrogen annealing is 700 DEG C.
Effect：Pt prepared by embodiment 23The TEM photos of Co/ conductor carbon blacks are as shown in Figure 1, Pt3Co alloy nanoparticles are flat
Equal size about 5.1nm.The results are shown in Figure 2 by XRD after 700 DEG C of temperature hydrogen reducings, Pt3The crystal structure of Co nano particles
For L10Cubic ordered structure.In order to test Pt3The oxygen reduction catalytic activity of Co/ conductive blacks will prepare Pt3Co/ is conductive
Carbon black tests hydrogen reduction performance in 0.1M perchloric acid, and the results are shown in Figure 3, Pt3Co/ conductive black hydrogen reduction catalysis is lived
Performance is higher than commercial Pt/ conductive black catalyst, the Pt to anneal also above 500 DEG C3The hydrogen reduction catalytic of Co/ conductive blacks
Energy.Pt3The results are shown in Figure 4 for durability test of the oxygen reduction catalytic activity of Co conductive blacks in 0.1M perchloric acid solutions,
It has almost no change after being recycled at 10,000 times, cyclic durability is better than the Pt of 500 DEG C of annealing3Co/ conductive black catalyst.
Embodiment 3
The preparation of PtFeCoNi/ conductive carbon ink loaded catalysts
Step 1,1 gram of six water chloroplatinic acid is taken【H2PtCl6·6H2O】, 0.780 gram of nine water ferric nitrate【Fe(NO3)3·9H2O】、
0.562 gram of cobalt nitrate hexahydrate【Co(NO3)2·6H2O】, 0.561 gram of six water nickel nitrate【Ni(NO3)2·6H2O】, it is dissolved in 150mL and goes
In ionized water, after ultrasonic wave dissolves 10min, 2.846 grams of Vulcan XC-72R carbon blacks and 2.846 grams of PVP (average marks are added
Son amount is 8000) and ultrasound is uniformly mixed for 20 minutes.The atomic molar ratio of platinum and iron, cobalt and nickel is 1:1:1:1, platinum, iron, cobalt and
The sum of weight of nickel and the weight ratio of conductive black are 1:4.
Step 2, the solution mixed is obtained into dry mixed powder by quick-drying method of spraying：By tiny mist
Drop is ejected on the quartz plate that temperature is 250 DEG C, and rapid evaporation aqueous solution obtains dry mixed-powder, and spray velocity is 10 millis
Liter/min.
Step 3, the dry mixed powder that step 2 obtains is removed from quartz plate, is annealed 60 minutes for 700 DEG C in hydrogen
Afterwards, PtFeCoNi/ conductive black loaded catalysts are obtained.
Effect：In PtFeCoNi/ conductive black catalyst prepared by embodiment 3, PtFeCoNi alloy nanoparticles are average
Size 6.2nm.XRD is the result shows that the crystal structure of PtFeCoNi nano particles is cube ordered structure.In order to test
The oxygen reduction catalytic activity of PtFeCoNi/ conductive blacks, the PtFeCoNi/ conductive blacks that will be prepared, in 0.1M perchloric acid
Middle test hydrogen reduction performance, the results showed that PtFeCoNi/ conductive blacks oxygen reduction catalytic activity can be higher than commercial Pt/ conduction charcoals
Black catalyst.Durability test result of the oxygen reduction catalytic activity of PtFeCoNi/ conductive blacks in 0.1M perchloric acid solutions
Show to vary less after recycling at 10,000 times, cyclic durability is higher than commercialization Pt/ conductive black catalyst.
Embodiment 4
The preparation of the graphene-supported type catalyst of PtFeCoNi/
This example is the change case of embodiment 3.Other implementation conditions are with embodiment 3, variation place：It is taken in step 1
0.5 gram of six water chloroplatinic acid【H2PtCl6·6H2O】, 0.390 gram of nine water ferric nitrate【Fe(NO3)3·9H2O】, 0.281 gram of six water nitre
Sour cobalt【Co(NO3)2·6H2O】, 0.281 gram of six water nickel nitrate【Ni(NO3)2·6H2O】, it is dissolved in 75mL deionized waters, ultrasound
After dissolving 10min, 1.423 grams of graphene oxides (since graphene oxide is dissolved in water, PVP is not added in mixed solution) are added
And ultrasound is uniformly mixed for 10 minutes.The atomic molar ratio of platinum and iron, cobalt, nickel is 1:1:1:1, platinum, iron, cobalt and nickel the sum of weight
Weight ratio with graphene oxide is 1:4.
Effect：In the graphene-supported type catalyst of PtFeCoNi/ prepared by embodiment 4, PtFeCoNi alloy nanoparticles
Average-size 3.6nm.XRD after 700 DEG C of temperature hydrogen reducings is the results show that the crystal structure of PtFeCoNi nano particles is
Cube ordered structure.In order to test the oxygen reduction catalytic activity of PtFeCoNi/ graphenes, the PtFeCoNi/ stones that will prepare
Black alkene tests hydrogen reduction performance, the results showed that PtFeCoNi/ graphenes oxygen reduction catalytic activity can be higher than in 0.1M perchloric acid
Commercial Pt/ conductive black catalyst.The oxygen reduction catalytic activity of PtFeCoNi/ graphenes is resistance in 0.1M perchloric acid solutions
Long property test result shows to vary less after recycling at 10,000 times, and cyclic durability is higher than commercialization Pt/ conductive black catalyst.
The foregoing is merely the preferred embodiment of the present invention, are not intended to restrict the invention, for those skilled in the art
For member, all within the spirits and principles of the present invention, made by any modification, improvements, protection of the invention should all be included in
Within the scope of.
Claims (6)
1. a kind of preparation method of precious metal alloys/carbon material supported type catalyst, which is characterized in that include the following steps：
Step 1 prepares at least one precious metal salt or acid and at least one kind of transition metal salt or acid and carbon material and dispersant
Mixed solution；
Step 2, by mixed solution that step 1 is obtained by be sprayed to the quick-drying method in high-temp solid surface prepare it is compound
Powder；
Step 3 anneals the composite powder that step 2 obtains in a reducing atmosphere, make it is metallic alloying, obtain precious metal alloys/
Carbon material supported type catalyst.
Precious metal salt described in step 1 or acid, transition metal salt or acid and the mixed solution of carbon material and dispersant include expensive
Metal salt or acid, transition metal salt or acid, carbon material, dispersant and solvent；
The precious metal salt or acid include：Platinum, gold, silver, rhodium, palladium, iridium, the nitrate of ruthenium, chlorate, acetate, oxalates and
Chloroplatinic acid, gold chloride；
The transition metal salt or acid include：Iron, cobalt, nickel, copper, molybdenum, tungsten, tantalum, tungsten, zinc, manganese, titanium, chromium, manganese, gallium nitrate,
Chlorate, acetate, oxalates and molybdic acid, wolframic acid；
The carbon material includes：Conductive black, graphite, graphene and graphene oxide.
2. the preparation method of precious metal alloys according to claim 1/carbon material supported type catalyst, which is characterized in that
The dispersant includes：Can dispersed electro-conductive carbon black, graphite and graphene in water high molecular material, such as water soluble polymer
Compound polyvinylpyrrolidone (PVP), polyacrylamide (PAM)；The solvent for constituting solution is water.
3. the preparation method of precious metal alloys according to claim 1 or 2/carbon material supported type catalyst, feature exist
In the molar ratio of precious metal ion and transition metal ions is 1 in solution described in step 1：(0.1~20)；Precious metal ion
It is 1 to add the molar ratio of the sum of transition metal ions and carbon material:(0.5~10)；The weight ratio of carbon material and dispersant is 1:
(0.01~10)；Precious metal salt or acid, transition metal salt or acid, carbon material and the molar ratio of dispersant solute and water are 1:(2~
500)。
4. the preparation method of precious metal alloys according to claim 1 or 2/carbon material supported type catalyst, feature exist
In, dry method described in step 2 be by spraying mixed solution to high-temp solid surface, it is fast using solid conductive heat speed
In the gas the characteristics of, realize that the rapid draing of mixing liquid prepares composite powder.
5. the preparation method of precious metal alloys according to claim 1 or 2/carbon material supported type catalyst, feature exist
In alloying annealing temperature described in step 3 is less than 1000 DEG C, and best temperature is 400 DEG C~700 DEG C.
6. the preparation method of precious metal alloys according to claim 1 or 2/carbon material supported type catalyst, feature exist
In reducing atmosphere described in step 3 is H2、H2/N2Mixed gas, H2/ Ar mixed gas.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109706364A (en) * | 2019-02-21 | 2019-05-03 | 中国科学技术大学 | Intermetallic compound composite material, preparation method and its application |
| CN109745969A (en) * | 2018-12-20 | 2019-05-14 | 西安交通大学 | A kind of carbon carries super-small precious metal nano-particle catalyst and preparation method |
| CN109759076A (en) * | 2019-03-25 | 2019-05-17 | 河北地质大学 | A kind of composite catalyst and preparation method thereof |
| CN110064423A (en) * | 2019-02-21 | 2019-07-30 | 中国科学技术大学 | Extra small multicomponent alloy composite material, preparation method and its application |
| CN110112430A (en) * | 2019-04-19 | 2019-08-09 | 贵研铂业股份有限公司 | A kind of platinum alloy carbon-supported powder and preparation method thereof |
| CN111224118A (en) * | 2019-11-15 | 2020-06-02 | 一汽解放汽车有限公司 | Multi-element doped platinum-based catalyst and preparation method and application thereof |
| CN111969218A (en) * | 2020-08-31 | 2020-11-20 | 西北有色金属研究院 | Preparation method of graphene-based iridium copper nanocomposite |
| CN113293406A (en) * | 2021-06-03 | 2021-08-24 | 中国科学技术大学 | Nano electro-catalyst, synthesis method, test electrode and preparation method |
| CN114210343A (en) * | 2022-01-24 | 2022-03-22 | 桂林电子科技大学 | Reduced graphene oxide loaded Ru-Ni bimetallic nanocluster catalytic material |
| CN114464789A (en) * | 2022-01-19 | 2022-05-10 | 华中科技大学 | Energy storage secondary battery layered positive electrode material and preparation method thereof |
| CN114618485A (en) * | 2020-12-11 | 2022-06-14 | 中国科学院理化技术研究所 | Carbon-based hollow supported microsphere catalyst and preparation method and application thereof |
| CN114797996A (en) * | 2021-01-27 | 2022-07-29 | 丰田纺织株式会社 | Catalyst supporting alloy fine particles, fuel cell, methods for producing them, and electrode |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109745969A (en) * | 2018-12-20 | 2019-05-14 | 西安交通大学 | A kind of carbon carries super-small precious metal nano-particle catalyst and preparation method |
| CN109706364A (en) * | 2019-02-21 | 2019-05-03 | 中国科学技术大学 | Intermetallic compound composite material, preparation method and its application |
| CN110064423A (en) * | 2019-02-21 | 2019-07-30 | 中国科学技术大学 | Extra small multicomponent alloy composite material, preparation method and its application |
| CN109759076A (en) * | 2019-03-25 | 2019-05-17 | 河北地质大学 | A kind of composite catalyst and preparation method thereof |
| CN110112430A (en) * | 2019-04-19 | 2019-08-09 | 贵研铂业股份有限公司 | A kind of platinum alloy carbon-supported powder and preparation method thereof |
| CN111224118A (en) * | 2019-11-15 | 2020-06-02 | 一汽解放汽车有限公司 | Multi-element doped platinum-based catalyst and preparation method and application thereof |
| CN111969218A (en) * | 2020-08-31 | 2020-11-20 | 西北有色金属研究院 | Preparation method of graphene-based iridium copper nanocomposite |
| CN114618485A (en) * | 2020-12-11 | 2022-06-14 | 中国科学院理化技术研究所 | Carbon-based hollow supported microsphere catalyst and preparation method and application thereof |
| CN114618485B (en) * | 2020-12-11 | 2024-02-23 | 中国科学院理化技术研究所 | Carbon-based hollow supported microsphere catalyst and preparation method and application thereof |
| CN114797996A (en) * | 2021-01-27 | 2022-07-29 | 丰田纺织株式会社 | Catalyst supporting alloy fine particles, fuel cell, methods for producing them, and electrode |
| CN113293406A (en) * | 2021-06-03 | 2021-08-24 | 中国科学技术大学 | Nano electro-catalyst, synthesis method, test electrode and preparation method |
| CN114464789A (en) * | 2022-01-19 | 2022-05-10 | 华中科技大学 | Energy storage secondary battery layered positive electrode material and preparation method thereof |
| CN114464789B (en) * | 2022-01-19 | 2023-03-10 | 华中科技大学 | Energy storage secondary battery layered positive electrode material and preparation method thereof |
| CN114210343A (en) * | 2022-01-24 | 2022-03-22 | 桂林电子科技大学 | Reduced graphene oxide loaded Ru-Ni bimetallic nanocluster catalytic material |
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