CN103236549A - Catalyst material for ether group lithium air battery and preparation method thereof - Google Patents

Catalyst material for ether group lithium air battery and preparation method thereof Download PDF

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CN103236549A
CN103236549A CN2013101275045A CN201310127504A CN103236549A CN 103236549 A CN103236549 A CN 103236549A CN 2013101275045 A CN2013101275045 A CN 2013101275045A CN 201310127504 A CN201310127504 A CN 201310127504A CN 103236549 A CN103236549 A CN 103236549A
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air battery
catalyst material
preparation
glue
lithium
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张新波
徐吉静
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Changchun Institute of Applied Chemistry of CAS
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Changchun Institute of Applied Chemistry of CAS
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Abstract

The invention relates to a catalyst material for ether group lithium air battery and preparation method thereof. The invention solves technology problem that the catalyst can not satisfy the industrialization requirement of the high performance ether group lithium-air battery. The catalyst material for ether group lithium air battery provided by the invention is a three dimensional ordered macroporous perovskite structure composite oxide, and the chemical formula is LaMO3, and M is a transition metal ion. The preparation method of catalyst material for ether group lithium air battery provided by the invention employs a colloidal crystal template, and the product is obtained by precursor solution immersion and template removal. The catalyst material provided by the invention can effectively charge and discharge utilization efficiency, multiplying power performance and cycle stability of lithium air battery. The invention simultaneously has the advantages of simple preparation technology, convenient operation, low cost and large scale.

Description

Lithium-air battery catalyst material and preparation method thereof
Technical field
The invention belongs to electrochemical energy material technology field, be specifically related to lithium-air battery catalyst material and preparation method thereof.
Background technology
Lithium-air battery is subjected to extensive concern owing to having the high theoretical energy density.Another advantage of lithium-air battery is that anodal active material oxygen is to be directed to surrounding air, thereby is inexhaustible, and does not need to be stored in inside battery, has so not only reduced cost but also has alleviated the weight of battery.But want it realize is used, also need to solve a series of problems, low such as electrolyte stability, high rate performance is poor, cyclical stability difference etc.The catalyst of lithium-air battery use at present is mainly metal oxide, metal nitride, metal nanoparticle, and the corresponding electrolyte that uses is carbonates with it.These catalyst can be accelerated hydrogen reduction and oxygen evolution reaction to a certain extent, can bring side reaction again in the catalysis electrode reaction, as the decomposition of catalytic electrolysis liquid.Therefore, can there be above-mentioned shortcoming in existing lithium-air battery.
For addressing the above problem, people adopt ethers as the electrolyte of lithium-air battery, and ethers electrolyte can not decomposed by employed catalyst, cause the decomposing phenomenon of electrolyte to take place.The catalyst that has catalytic activity in ethers electrolyte of report mainly contains noble metal, pyrochlore oxide and Co at present 3O 4Deng, still, these catalyst all are to be deposited in the air electrode with granular form, are unfavorable for the mass transfer of air electrode in the performance of its catalytic activity and the cell reaction, cause ethers lithium-air battery performance to reduce.Wherein, also there is the high deficiency of cost in noble metal catalyst.Therefore, above-mentioned existing several catalyst all can not satisfy the requirement of the industrialization of high-performance ether lithium-air battery.
Summary of the invention
The present invention is for solving the technical problem that existing catalyst can not satisfy the requirement of high-performance ether lithium-air battery industrialization, and provide a kind of low cost, high-performance ether lithium-air battery is used, lithium-air battery catalyst material and preparation method thereof.
In order to solve the problems of the technologies described above, technical scheme of the present invention is specific as follows:
Lithium-air battery catalyst material, this catalyst material are three-dimensional ordered macroporous perovskite structure composite oxide, and its chemical expression is: LaMO 3, M is transition metal ions.
In technique scheme, described M is Fe 3+, Ni 2+, Co 2+Or Mn 2+
In technique scheme, the aperture of described catalyst material is 20～30nm.
In technique scheme, the specific area of described catalyst material is 20～80m 2g -1
The lithium-air battery preparation method of catalyst material, this preparation method mainly may further comprise the steps:
(1) be 0.5～2molL with total concentration -1Metal nitrate or acetate be dissolved in the mixed solution of ethylene glycol and methyl alcohol;
(2) the glue crystal template is immersed in the above-mentioned salting liquid;
(3) with the above-mentioned oven dry of the glue crystal template after the immersion in salting liquid, again in 500～700 ℃ of calcinings, be incubated and remove the glue crystal template after 3～5 hours, obtain perovskite structure composite oxide LaMO 3
Described metal nitrate or acetate comprise: the nitrate of lanthanum or acetate, and a kind of transition metal nitrate or acetate.
In technique scheme, described transition metal nitrate or acetate are a kind of in iron, cobalt, nickel, manganese nitrate or the acetate.
In technique scheme, the volume ratio of the ethylene glycol described in the step (1) and methyl alcohol is 1:1.
In technique scheme, the glue crystal template described in the step (2) is polystyrene (PS) glue crystalline substance, silicon dioxide (SiO 2) a kind of in brilliant and polymethyl methacrylate (PMMA) the glue crystalline substance of glue.
In technique scheme, the glue crystal template is dried described in the step (3), bake out temperature is 50～80 ℃, drying time is 2～5 hours.
In technique scheme, the glue crystal template calcining heat described in the step (3) is to rise to temperature required by the speed that normal temperature begins with 1 ℃/minute.
In technique scheme, the glue crystal template described in the step (3) can also be 7～10molL with concentration -1The sodium hydroxide solution dissolution method remove.
Lithium-air battery provided by the invention with the beneficial effect of catalyst material and preparation method thereof is:
1, lithium-air battery catalyst material provided by the invention is the composite oxides of three-dimensional ordered macroporous structure, and the aperture is 20～30nm, and specific area is 20～80m 2g -1When this three-dimensional ordered macroporous structure catalyst is used for the ether lithium-air battery, can provide enough active places for cell reaction, have good ion transfer ability and conductivity concurrently, that can effectively improve lithium-air battery discharges and recharges utilization ratio, high rate performance and cyclical stability.Compare with existing ether lithium-air battery, cost is lower, and the capacity of battery, multiplying power and cyclical stability all are increased dramatically, and enough satisfies the requirement of high-performance ether lithium-air battery industrialization.
Fig. 1 and 2 has proved that catalyst material of the present invention presents the three-dimensional ordered macroporous alveolate texture of long-range order.Fig. 3 illustrates that catalyst material of the present invention has wideer distribution, and wherein the macropore of 40nm is in the majority, and the source in hole may be the intercommunicating pore of three-dimensional ordered macroporous centre.
2, ether lithium-air battery provided by the invention is with the preparation method of catalyst material, and its preparation technology is simple, easy to operate, cost is low, easily accomplish scale production.This preparation method easily realizes the rapid diffusion of electronics, electrolyte and oxygen in the maximum using of catalyst activity point position and the cell reaction.When the catalyst material of this method preparation was used for the ether lithium-air battery, the effectively reaction of catalysis lithium and oxygen can be convenient to the quick transmission of oxygen and electrolyte again; The capacity of battery, multiplying power and cyclical stability all are increased dramatically, and overpotential reduces; Improve 1.2 times with present lithium-air battery phase specific capacity, cycle performance improves 3 times, and cycle life reaches 124 times.
Fig. 4 is the LaFeO of the embodiment of the invention one preparation 3Catalyst material is used for the charging and discharging curve figure of lithium-air battery, and limit capacity is 1000mA h g Carbon -1, current density is 0.15mA cm -2This figure as can be seen, the ether lithium-air battery cycle life that includes above-mentioned catalyst reaches 124 times, has broken through best 100 circulations in the world of present report.
Fig. 5 is the LaFeO of the embodiment of the invention one preparation 3Catalyst material is used for the cycle performance figure of ether lithium-air battery, and limit capacity is 1000mA h g Carbon -1, current density is 0.15mA cm -2This figure includes the discharge voltage of ether lithium-air battery of above-mentioned catalyst as can be seen along with the increase of cycle-index does not significantly reduce.
Description of drawings
Fig. 1 is the three-dimensional ordered macroporous LaFeO of the embodiment of the invention one preparation 3Material SEM figure.
Fig. 2 is the three-dimensional ordered macroporous LaFeO of the embodiment of the invention one preparation 3Material TEM figure.
Fig. 3 is the three-dimensional ordered macroporous LaFeO of the embodiment of the invention one preparation 3The material graph of pore diameter distribution.
Fig. 4 is the three-dimensional ordered macroporous LaFeO of the embodiment of the invention one preparation 3Material is used for the charging and discharging curve figure of ether lithium-air battery, and limit capacity is 1000mA h g Carbon -1, current density is 0.15mA cm -2
Fig. 5 is the three-dimensional ordered macroporous LaFeO of the embodiment of the invention one preparation 3Material is used for the cycle performance figure of ether lithium-air battery, and limit capacity is 1000mA h g Carbon -1, current density is 0.15mA cm -2
Embodiment
Lithium-air battery catalyst material provided by the invention, this catalyst material are three-dimensional ordered macroporous perovskite structure composite oxides, and the aperture is 20～30nm, and specific area is 20～80m 2g -1, its chemical expression is: LaMO 3, M is transition metal ions.Wherein, described M can be Fe 3+, Ni 2+, Co 2+Or Mn 2+The chemical expression of corresponding perovskite structure composite oxide is respectively: LaFeO 3, LaNiO 3, LaCoO 3Or LaMnO 3
Lithium-air battery catalyst material provided by the invention is prepared by following method:
(1) be 0.5～2molL with total concentration -1Metal nitrate or acetate be dissolved in the mixed solution of ethylene glycol and methyl alcohol;
Described metal nitrate or acetate comprise: the nitrate of lanthanum or acetate, and a kind of in iron, cobalt, nickel, manganese nitrate or the acetate; The volume ratio of described ethylene glycol and methyl alcohol is 1:1;
(2) the glue crystal template is immersed in the above-mentioned salting liquid;
Described glue crystal template is polystyrene (PS) glue crystalline substance, silicon dioxide (SiO 2) a kind of in brilliant and polymethyl methacrylate (PMMA) the glue crystalline substance of glue;
(3) above-mentioned glue crystal template after soaking in salting liquid is dried in baking oven, bake out temperature is 50～80 ℃, drying time is 2～5 hours, again in 500～700 ℃ of calcinings, be incubated and remove the glue crystal template after 3～5 hours, heating rate is 1 ℃/minute, obtains perovskite structure composite oxide LaMO 3
In technique scheme, the glue crystal template described in the step (3) can also be 7～10molL with concentration -1The sodium hydroxide solution dissolution method is removed.
Embodiment one
Be the LaNO of 1:1 with mol ratio 36H 2O and Fe (NO 3) 39H 2O is dissolved in the mixed solution of ethylene glycol and methyl alcohol, and the slaine total concentration is 2molL -1The volume ratio of ethylene glycol and methyl alcohol is 1:1, then polystyrene (PS) glue crystal template is immersed in the above-mentioned salting liquid 1 hour, outwell excessive solution, sample was placed in 50 ℃ of baking ovens after 5 hours, 500 ℃ of calcinings in air again, temperature retention time is 5 hours, heating rate is 1 ℃/minute, obtains three-dimensional ordered macroporous LaFeO 3Material.
Fig. 1 is the three-dimensional ordered macroporous LaFeO of present embodiment one preparation 3Material SEM figure.As can be seen, catalyst material presents the three-dimensional ordered macroporous alveolate texture of long-range order.This structure is conducive to the raising with the air electrode mass transfer of increasing in catalyst activity site.
Fig. 2 is the three-dimensional ordered macroporous LaFeO of present embodiment one preparation 3Material TEM figure.This figure has further verified the described structure of Fig. 1.
Fig. 3 is the three-dimensional ordered macroporous LaFeO of the embodiment of the invention one preparation 3The material graph of pore diameter distribution.As can be seen, catalyst material has wideer distribution, and wherein the macropore of 40nm is in the majority, and the source in hole may be the intercommunicating pore of three-dimensional ordered macroporous centre.
Fig. 4 is the three-dimensional ordered macroporous LaFeO of the embodiment of the invention one preparation 3Material is used for the charging and discharging curve figure of lithium-air battery, and limit capacity is 1000mA h g Carbon -1, current density is 0.15mA cm -2As can be seen, the lithium-air battery cycle performance that includes above-mentioned catalyst has been broken through best 100 circulations in the world of present report, and cycle-index has reached 124 times.
Fig. 5 is the cycle performance figure that the 3-D ordered multiporous catalyst material of the embodiment of the invention one preparation is used for the ether lithium-air battery, and limit capacity is 1000mA h g Carbon -1, current density is 0.15mA cm -2As can be seen, include the discharge voltage of lithium-air battery of above-mentioned catalyst along with the increase of cycle-index does not significantly reduce.
Embodiment two
Be the LaNO of 1:1 with mol ratio 36H 2O and Co (NO 3) 26H 2O is dissolved in the mixed solution of ethylene glycol and methyl alcohol, and the slaine total concentration is 1.5molL -1, the volume ratio of ethylene glycol and methyl alcohol is 1:1, then with silicon dioxide (SiO 2) the glue crystal template is immersed in the above-mentioned salting liquid 10 hours, outwells excessive solution, with sample in 80 ℃ of baking ovens after the oven dry in 2 hours, 700 ℃ of calcinings in air again, temperature retention time is 3 hours, heating rate is 1 ℃/minute, is 10molL in concentration at last -1Sodium hydroxide solution in remove template, obtain three-dimensional ordered macroporous LaCoO 3Material.
Embodiment three
Be the LaNO of 1:1 with mol ratio 36H 2O and Ni (NO 3) 26H 2O is dissolved in the mixed solution of ethylene glycol and methyl alcohol, and the slaine total concentration is 0.5molL -1, the volume ratio of ethylene glycol and methyl alcohol is 1:1, then with silicon dioxide (SiO 2) the glue crystal template is immersed in the above-mentioned salting liquid 10 hours, outwells excessive solution, with sample in 80 ℃ of baking ovens after the oven dry in 2 hours, 650 ℃ of calcinings in air again, temperature retention time is 3 hours, heating rate is 1 ℃/minute, is 10molL in concentration at last -1Sodium hydroxide solution in remove template, obtain three-dimensional ordered macroporous LaNiO 3Material.
Embodiment four
Be the LaNO of 1:1 with mol ratio 36H 2O and Mn (NO 3) 24H 2O is dissolved in the mixed solution of ethylene glycol and methyl alcohol, and the slaine total concentration is 1.0molL -1, the volume ratio of ethylene glycol and methyl alcohol is 1:1, then with silicon dioxide (SiO 2) the glue crystal template is immersed in the above-mentioned salting liquid 10 hours, outwells excessive solution, with sample in 80 ℃ of baking ovens after the oven dry in 2 hours, 500 ℃ of calcinings in air again, temperature retention time is 5 hours, heating rate is 1 ℃/minute, is 7.0molL in concentration at last -1Sodium hydroxide solution in remove template, obtain three-dimensional ordered macroporous LaMnO 3Material.
Obviously, above-described embodiment only is for example clearly is described, and is not the restriction to execution mode.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give all execution modes exhaustive.And the apparent variation of being extended out thus or change still are among the protection range of the invention.

Claims (11)

1. the lithium-air battery catalyst material is characterized in that, this catalyst material is three-dimensional ordered macroporous perovskite structure composite oxide, and its chemical expression is: LaMO 3, M is transition metal ions.
2. ether lithium-air battery catalyst material according to claim 1 is characterized in that, described M is Fe 3+, Ni 2+, Co 2+Or Mn 2+
3. ether lithium-air battery catalyst material according to claim 1 is characterized in that, the aperture of described catalyst material is 20～30nm.
4. ether lithium-air battery catalyst material according to claim 1 is characterized in that, the specific area of described catalyst material is 20～80m 2g -1
5. lithium-air battery according to claim 1 is characterized in that this preparation method mainly may further comprise the steps with the preparation method of catalyst material:
(1) be 0.5～2molL with total concentration -1Metal nitrate or acetate be dissolved in the mixed solution of ethylene glycol and methyl alcohol;
(2) the glue crystal template is immersed in the above-mentioned salting liquid;
(3) with the above-mentioned oven dry of the glue crystal template after the immersion in salting liquid, again in 500～700 ℃ of calcinings, be incubated and remove the glue crystal template after 3～5 hours, obtain perovskite structure composite oxide LaMO 3
Described metal nitrate or acetate comprise: the nitrate of lanthanum or acetate, and a kind of transition metal nitrate or acetate.
6. preparation method according to claim 5 is characterized in that, described transition metal nitrate or acetate are a kind of in iron, cobalt, nickel, manganese nitrate or the acetate.
7. preparation method according to claim 5 is characterized in that, the volume ratio of the ethylene glycol described in the step (1) and methyl alcohol is 1:1.
8. preparation method according to claim 5 is characterized in that, the glue crystal template described in the step (2) is polystyrene (PS) glue crystalline substance, silicon dioxide (SiO 2) a kind of in brilliant and polymethyl methacrylate (PMMA) the glue crystalline substance of glue.
9. preparation method according to claim 5 is characterized in that, the glue crystal template is dried described in the step (3), and bake out temperature is 50～80 ℃, drying time is 2～5 hours.
10. preparation method according to claim 5 is characterized in that, the glue crystal template calcining heat described in the step (3) is to rise to temperature required by the speed that normal temperature begins with 1 ℃/minute.
11. preparation method according to claim 5 is characterized in that, the glue crystal template described in the step (3) can also be 7～10molL with concentration -1The sodium hydroxide solution dissolution method remove.
CN2013101275045A 2013-04-12 2013-04-12 Catalyst material for ether group lithium air battery and preparation method thereof Pending CN103236549A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103545537A (en) * 2013-10-30 2014-01-29 上海交通大学 Double-perovskite structure catalyst material for cathode of lithium air battery and preparation method of catalyst material
CN103706389A (en) * 2013-12-31 2014-04-09 南京工业大学 Preparation method of lithium air battery catalyst with double catalytic activities
EP2945210A1 (en) * 2014-05-16 2015-11-18 Robert Bosch Gmbh Inorganic compounds as a cathode material for lithium/air batteries
CN108295849A (en) * 2018-01-18 2018-07-20 中国科学院宁波材料技术与工程研究所 My/LaxSr1-xTi1-yO3Catalyst, its preparation method and application
CN111916770A (en) * 2020-09-02 2020-11-10 厦门理工学院 High-performance air electrode catalyst and preparation method thereof
CN113871638A (en) * 2021-10-14 2021-12-31 南京航空航天大学 Lanthanum ferrite photoelectrode, preparation method thereof and application thereof in lithium-oxygen battery

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103545537A (en) * 2013-10-30 2014-01-29 上海交通大学 Double-perovskite structure catalyst material for cathode of lithium air battery and preparation method of catalyst material
CN103706389A (en) * 2013-12-31 2014-04-09 南京工业大学 Preparation method of lithium air battery catalyst with double catalytic activities
EP2945210A1 (en) * 2014-05-16 2015-11-18 Robert Bosch Gmbh Inorganic compounds as a cathode material for lithium/air batteries
CN108295849A (en) * 2018-01-18 2018-07-20 中国科学院宁波材料技术与工程研究所 My/LaxSr1-xTi1-yO3Catalyst, its preparation method and application
CN108295849B (en) * 2018-01-18 2021-06-22 中国科学院宁波材料技术与工程研究所 My/LaxSr1-xTi1-yO3Catalyst, its preparation method and application
CN111916770A (en) * 2020-09-02 2020-11-10 厦门理工学院 High-performance air electrode catalyst and preparation method thereof
CN111916770B (en) * 2020-09-02 2021-09-24 厦门理工学院 High-performance air electrode catalyst and preparation method thereof
CN113871638A (en) * 2021-10-14 2021-12-31 南京航空航天大学 Lanthanum ferrite photoelectrode, preparation method thereof and application thereof in lithium-oxygen battery
CN113871638B (en) * 2021-10-14 2024-07-05 南京航空航天大学 Lanthanum ferrite photoelectrode, preparation method thereof and application thereof in lithium-oxygen battery

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Application publication date: 20130807