CN109360986A - Application of the zinc selenide as aluminium ion cell positive material - Google Patents
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- CN109360986A CN109360986A CN201811139119.1A CN201811139119A CN109360986A CN 109360986 A CN109360986 A CN 109360986A CN 201811139119 A CN201811139119 A CN 201811139119A CN 109360986 A CN109360986 A CN 109360986A
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
Application the present invention relates to zinc selenide as aluminium ion cell positive material belongs to aluminium ion battery technology field.Zinc selenide is used as aluminium ion cell positive material, not only there is high discharge platform, also there is big specific capacity, wherein, discharge voltage plateau is about 1.8V, first circle specific capacity is 164mAh/g or so under 200mA/g current density, so that aluminium ion battery can preferably be applied to various fields, such as electronics industry, communication industry, electric car.Meanwhile the preparation process of zinc selenide is simple, raw material sources are extensive, and at low cost, are suitble to large-scale industrial production.
Description
Technical field
The invention belongs to aluminium ion battery technology fields, and in particular to zinc selenide is answered as aluminium ion cell positive material
With.
Background technique
Compared with present widely used lithium ion battery, aluminium ion battery has many advantages and is widely closed
Note, if aluminium ion battery can shift three electronics in once oxidation reduction, therefore it is close to can provide very high volume energy
Degree and mass energy density.Further, since aluminium is the most abundant metallic element in the earth's crust, can be substantially reduced using it as raw material
The cost of aluminium ion battery, the in addition nonflammable property of aluminium ion electrode material and electrolyte used, therefore aluminium ion battery tool
There is good safety.
Currently, a series of materials such as carbon-based material, transition metal oxide/transient metal sulfide/transition metal selenides
Material is used as the positive electrode of aluminium ion battery.But as aluminium ion cell positive material, there is also not by these materials
Foot.Such as graphite material, although there is the up to discharge voltage plateau of 2.0V, its specific capacity is relatively low, and Dai et al. is by foam stone
Positive electrode of the ink as aluminium ion battery, shows high cyclical stability and high discharge voltage plateau, but this
The capacity of the battery of positive electrode assembling is lower, only 60mAh g-1(see Meng-Chang Lin, Ming Gong, Bingan
Lu,Yingpeng Wu,Diyan Wang,Mingyun Guan,Michael Angell,Changxin Chen,Jiang
Yang,Bing-Joe Hwang,Hongjie Dai.An ultrafast rechargeable aluminium-ion
battery[J].Nature,2015,520:324-328).Although and their ratio such as metal sulfide/oxide/selenides
Capacity is higher, but their discharge voltage plateau is very low, usually in 1.0V or less (see Xuefeng Zhang, Guohua
Zhang,Shuai Wang,Shijie Li and Shuqiang Jiao.Porous CuO microsphere
architectures as high performance cathode materials for aluminum-ion
batteries[J].Journal of Materials Chemistry A,2018,6,3084–3090).And some metal sulphur
Although compound/oxide/selenides has a higher discharge voltage plateau, but positive electrode used contains that price is very high and reserves
Cobalt element less and less is (see Tonghui Cai, Lianming Zhao, Haoyu Hu, Yanpeng Li, Qingzhong
Xue,Wei Xing,Zifeng Yan,Lianzhou Wang.Stable CoSe2/Carbon Nanodice@Reduced
Graphene Oxide Composites for High-performance Rechargeable Aluminum-ion
Batteries[J].Energy&Environmental Science,doi:10.1039/C8EE00822A)。
Zinc selenide can be used as the electrode material of battery, but be mainly used for the cathode material of lithium ion battery or sodium-ion battery
Material, wherein when negative electrode material of the zinc selenide as lithium ion battery, the mechanism of action (Hyuk-Tae Kwon, Cheol- as follows
Min Park.Electrochemical characteristics of ZnSe and its nanostructured
composite for rechargeable Li-ion batteries[J].Journal of Power Sources,2014,
251:319-324.): during discharge: ZnSe → LiSe+Zn → Li2Se+LixZn→Li2Se+LiZn；In charging process
In: Li2Se+LiZn→Li2Se+LixZn→LiSe+Zn→ZnSe；And does not have at present and zinc selenide is used in aluminium ion battery
Relevant report as electrode material.
Summary of the invention
In view of this, the present invention provides zinc selenide conducts in order to reach the insufficient purpose for overcoming existing material technology
The application of aluminium ion cell positive material.
In order to achieve the above objectives, the invention provides the following technical scheme:
1, application of the zinc selenide as aluminium ion cell positive material.
Preferably, the partial size of the zinc selenide be 400-1000nm, it is evenly dispersed and have regular morphology.
Preferably, the zinc selenide is prepared by the following method:
(1) soluble zinc salt is dissolved in methanol, obtains solution A；Methylimidazole is dissolved in methanol, solution B is obtained；
The solution A is poured into the solution B, forms reaction solution after stirring evenly, reaction is stood and is precipitated, after precipitating drying
Presoma is made；
(2) it is calcined in the mixed atmosphere of hydrogen and argon gas after mixing the presoma obtained in step (1) with selenium powder, i.e.,
It can.
Preferably, in step (1), the soluble zinc salt is one of zinc nitrate hexahydrate or zinc chloride.
Preferably, in step (1), the mass ratio of zinc nitrate hexahydrate and methylimidazole is 42-64 in the reaction solution:
34-58。
Preferably, in step (1), the time for standing reaction is 10-30h.
Preferably, in step (1), the temperature of the drying is less than 90 DEG C.
Preferably, in step (2), the mass ratio 1:1-4 of the presoma and selenium powder.
Preferably, in step (2), the volume fraction of hydrogen is 3-10% in the mixed atmosphere.
Preferably, in step (2), the calcining is kept the temperature after being specifically warming up to 400-800 DEG C with the rate of 2-10 DEG C/min
1-4h。
Using zinc selenide as aluminium ion cell positive material in the present invention, after being assembled into battery, reaction mechanism may are as follows:
During the charging process:
Cathode:
4Al2Cl7 -+3e-→Al+7AlCl4 -
Anode:
AlZnSe+7AlCl4 --3e-→ZnSe+4Al2Cl7 -
During discharge:
Cathode:
Al+7AlCl4 --3e-→4Al2Cl7 -
Anode:
ZnSe+4Al2Cl7 -+3e-→AlZnSe+7AlCl4 -。
The beneficial effects of the present invention are: the application the present invention provides zinc selenide as aluminium ion cell positive material,
Zinc selenide is used as aluminium ion cell positive material, not only there is high discharge platform, also there is big specific capacity, wherein put
Piezoelectric voltage platform is about 1.8V, and first circle specific capacity is 164mAh/g or so under 200mA/g current density, so that aluminium ion battery
Various fields, such as electronics industry, communication industry, electric car can be preferably applied to.Meanwhile the preparation process of zinc selenide
Simply, raw material sources are extensive, and at low cost, are suitble to large-scale industrial production.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out
Illustrate:
Fig. 1 is the XRD diagram of the zinc selenide prepared in embodiment 1；
Fig. 2 is the SEM figure of the zinc selenide prepared in embodiment 1；
Fig. 3 be the zinc selenide that is prepared using in embodiment 1 as positive electrode aluminium ion battery in 200mA/g current density
Under charging and discharging curve figure；
Fig. 4 be the zinc selenide that is prepared using in embodiment 1 as positive electrode aluminium ion battery in 200mA/g current density
Under loop test curve graph.
Specific embodiment
Below by a preferred embodiment of the present invention will be described in detail.
Embodiment 1
(1) 2g zinc nitrate hexahydrate is dissolved in 20mL methanol, obtains solution A；1.6g methylimidazole is dissolved in 20mL
In methanol, solution B is obtained；Solution A is poured into solution B rapidly, forms reaction solution after stirring evenly, is stood after reacting 10h through being centrifuged
It is precipitated, presoma is made in described be deposited at 60 DEG C after vacuum drying 5h；
(2) presoma and selenium powder 1:1 mixed grinding in mass ratio that obtain in step (1) are placed in tube furnace,
1h is kept the temperature after being warming up to 400 DEG C in the mixed atmosphere of hydrogen and argon gas with the rate of 2 DEG C/min, is cooled to room temperature, selenizing is made
Zinc.Wherein, the volume fraction of hydrogen is 3% in mixed atmosphere.X-ray diffraction analysis is carried out to zinc selenide obtained, is as a result seen
Fig. 1, as shown in Figure 1, product obtained are zinc selenide (JCPDS#37-1463), and using scanning electron microscope to zinc selenide obtained
It is detected, for testing result as shown in Fig. 2, as shown in Figure 2, zinc selenide diameter is distributed within the scope of 400-1000nm, dispersion is equal
It is even, in the polyhedron of morphological rules.
(3) zinc selenide obtained is anode, aluminium foil as cathode, AlCl using in step (2)3/ [EMIm] Cl is electrolyte dress
It is made into battery to be tested for the property, test result is shown in Fig. 3 and Fig. 4, from the figure 3, it may be seen that anode of the zinc selenide as aluminium ion battery
Material, discharge potential platform are 1.8V, and as shown in Figure 4, under the current density of 200mA/g, which discharges specific volume for the first time
Measuring is 164mAh/g, and there are also the specific capacities of 82mAh/g after 60 circulations.
Embodiment 2
(1) 2g zinc nitrate hexahydrate is dissolved in 30mL methanol, obtains solution A；2g methylimidazole is dissolved in 30mL first
In alcohol, solution B is obtained；Solution A is poured into solution B rapidly, forms reaction solution after stirring evenly, is obtained after standing reaction 15h through centrifugation
It must precipitate, presoma is made in described be deposited at 60 DEG C after vacuum drying 5h；
(2) presoma and selenium powder 1:2 mixed grinding in mass ratio that obtain in step (1) are placed in tube furnace,
1h is kept the temperature after being warming up to 600 DEG C in the mixed atmosphere of hydrogen and argon gas with the rate of 4 DEG C/min, is cooled to room temperature, selenizing is made
Zinc.Wherein, the volume fraction of hydrogen is 3% in mixed atmosphere.
(3) zinc selenide obtained is anode, aluminium foil as cathode, AlCl using in step (2)3/ [EMIm] Cl is electrolyte dress
Battery is made into be tested for the property, when positive electrode of the zinc selenide as aluminium ion battery, discharge potential platform is 1.8V,
Under the current density of 200mA/g, the material first discharge specific capacity be 168mAh/g, 60 times circulation after there are also 81mAh/g ratio
Capacity.
Embodiment 3
(1) 2g zinc nitrate hexahydrate is dissolved in 40mL methanol, obtains solution A；2.2g methylimidazole is dissolved in 40mL
In methanol, solution B is obtained；Solution A is poured into solution B rapidly, forms reaction solution after stirring evenly, is stood after reacting 18h through being centrifuged
It is precipitated, presoma is made in described be deposited at 60 DEG C after vacuum drying 5h；
(2) presoma and selenium powder 1:2 mixed grinding in mass ratio that obtain in step (1) are placed in tube furnace,
3h is kept the temperature after being warming up to 700 DEG C in the mixed atmosphere of hydrogen and argon gas with the rate of 5 DEG C/min, is cooled to room temperature, selenizing is made
Zinc.Wherein, the volume fraction of hydrogen is 4% in mixed atmosphere.
(3) zinc selenide obtained is anode, aluminium foil as cathode, AlCl using in step (2)3/ [EMIm] Cl is electrolyte dress
It being made into battery to be tested for the property, positive electrode of the zinc selenide as aluminium ion battery, discharge potential platform is 1.8V,
Under the current density of 200mA/g, the material first discharge specific capacity be 172mAh/g, 60 times circulation after there are also 83mAh/g ratio
Capacity.
Embodiment 4
(1) 2g zinc nitrate hexahydrate is dissolved in 60mL methanol, obtains solution A；2.3g methylimidazole is dissolved in 60mL
In methanol, solution B is obtained；Solution A is poured into solution B rapidly, forms reaction solution after stirring evenly, stands reaction for 24 hours afterwards through being centrifuged
It is precipitated, presoma is made in described be deposited at 60 DEG C after vacuum drying 5h；
(2) presoma and selenium powder 1:3 mixed grinding in mass ratio that obtain in step (1) are placed in tube furnace,
2h is kept the temperature after being warming up to 600 DEG C in the mixed atmosphere of hydrogen and argon gas with the rate of 6 DEG C/min, is cooled to room temperature, selenizing is made
Zinc.Wherein, the volume fraction of hydrogen is 4% in mixed atmosphere.
(3) zinc selenide obtained is anode, aluminium foil as cathode, AlCl using in step (2)3/ [EMIm] Cl is electrolyte dress
It being made into battery to be tested for the property, positive electrode of the zinc selenide as aluminium ion battery, discharge potential platform is 1.8V,
Under the current density of 200mA/g, the material first discharge specific capacity be 162mAh/g, 60 times circulation after there are also 79mAh/g ratio
Capacity.
Embodiment 5
(1) 2g zinc nitrate hexahydrate is dissolved in 60mL methanol, obtains solution A；2.5g methylimidazole is dissolved in 60mL
In methanol, solution B is obtained；Solution A is poured into solution B rapidly, forms reaction solution after stirring evenly, is stood after reacting 28h through being centrifuged
It is precipitated, presoma is made in described be deposited at 60 DEG C after vacuum drying 5h；
(2) presoma and selenium powder 1:3 mixed grinding in mass ratio that obtain in step (1) are placed in tube furnace,
3h is kept the temperature after being warming up to 700 DEG C in the mixed atmosphere of hydrogen and argon gas with the rate of 6 DEG C/min, is cooled to room temperature, selenizing is made
Zinc.Wherein, the volume fraction of hydrogen is 6% in mixed atmosphere.
(3) zinc selenide obtained is anode, aluminium foil as cathode, AlCl using in step (2)3/ [EMIm] Cl is electrolyte dress
It being made into battery to be tested for the property, positive electrode of the zinc selenide as aluminium ion battery, discharge potential platform is 1.8V,
Under the current density of 200mA/g, the material first discharge specific capacity be 166mAh/g, 60 times circulation after there are also 83mAh/g ratio
Capacity.
Embodiment 6
(1) 2g zinc nitrate hexahydrate is dissolved in 80mL methanol, obtains solution A；2.6g methylimidazole is dissolved in 80mL
In methanol, solution B is obtained；Solution A is poured into solution B rapidly, forms reaction solution after stirring evenly, is stood after reacting 15h through being centrifuged
It is precipitated, presoma is made in described be deposited at 60 DEG C after vacuum drying 5h；
(2) presoma and selenium powder 1:4 mixed grinding in mass ratio that obtain in step (1) are placed in tube furnace,
4h is kept the temperature after being warming up to 700 DEG C in the mixed atmosphere of hydrogen and argon gas with the rate of 6 DEG C/min, is cooled to room temperature, selenizing is made
Zinc.Wherein, the volume fraction of hydrogen is 6% in mixed atmosphere.
(3) zinc selenide obtained is anode, aluminium foil as cathode, AlCl using in step (2)3/ [EMIm] Cl is electrolyte dress
It being made into battery to be tested for the property, positive electrode of the zinc selenide as aluminium ion battery, discharge potential platform is 1.8V,
Under the current density of 200mA/g, the material first discharge specific capacity be 162mAh/g, 60 times circulation after there are also 85mAh/g ratio
Capacity.
Embodiment 7
(1) 2g zinc nitrate hexahydrate is dissolved in 80mL methanol, obtains solution A；2.6g methylimidazole is dissolved in 80mL
In methanol, solution B is obtained；Solution A is poured into solution B rapidly, forms reaction solution after stirring evenly, is stood after reacting 26h through being centrifuged
It is precipitated, presoma is made in described be deposited at 60 DEG C after vacuum drying 5h；
(2) presoma and selenium powder 1:4 mixed grinding in mass ratio that obtain in step (1) are placed in tube furnace,
2h is kept the temperature after being warming up to 800 DEG C in the mixed atmosphere of hydrogen and argon gas with the rate of 8 DEG C/min, is cooled to room temperature, selenizing is made
Zinc.Wherein, the volume fraction of hydrogen is 8% in mixed atmosphere.
(3) zinc selenide obtained is anode, aluminium foil as cathode, AlCl using in step (2)3/ [EMIm] Cl is electrolyte dress
It being made into battery to be tested for the property, positive electrode of the zinc selenide as aluminium ion battery, discharge potential platform is 1.8V,
Under the current density of 200mA/g, the material first discharge specific capacity be 173mAh/g, 60 times circulation after there are also 82mAh/g ratio
Capacity.
Embodiment 8
(1) 2g zinc nitrate hexahydrate is dissolved in 90mL methanol, obtains solution A；2.7g methylimidazole is dissolved in 90mL
In methanol, solution B is obtained；Solution A is poured into solution B rapidly, forms reaction solution after stirring evenly, is stood after reacting 30h through being centrifuged
It is precipitated, presoma is made in described be deposited at 60 DEG C after vacuum drying 5h；
(2) presoma and selenium powder 1:4 mixed grinding in mass ratio that obtain in step (1) are placed in tube furnace,
4h is kept the temperature after being warming up to 800 DEG C in the mixed atmosphere of hydrogen and argon gas with the rate of 10 DEG C/min, is cooled to room temperature, selenizing is made
Zinc.Wherein, the volume fraction of hydrogen is 10% in mixed atmosphere.
(3) zinc selenide obtained is anode, aluminium foil as cathode, AlCl using in step (2)3/ [EMIm] Cl is electrolyte dress
It being made into battery to be tested for the property, positive electrode of the zinc selenide as aluminium ion battery, discharge potential platform is 1.8V,
Under the current density of 200mA/g, the material first discharge specific capacity be 163mAh/g, 60 times circulation after there are also 75mAh/g ratio
Capacity.
It, can also be using zinc chloride as raw material in addition to using zinc nitrate hexahydrate as the raw material for preparing zinc selenide in the present invention
Zinc selenide is prepared, equally can be realized identical technical effect.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (10)
1. application of the zinc selenide as aluminium ion cell positive material.
2. application according to claim 1, which is characterized in that the partial size of the zinc selenide is 400-1000nm, is uniformly divided
It dissipates and there is regular morphology.
3. application according to claim 2, which is characterized in that the zinc selenide is prepared by the following method:
(1) soluble zinc salt is dissolved in methanol, obtains solution A；Methylimidazole is dissolved in methanol, solution B is obtained；By institute
It states solution A to pour into the solution B, forms reaction solution after stirring evenly, stand reaction and precipitated, will be made after precipitating drying
Presoma；
(2) it is calcined in the mixed atmosphere of hydrogen and argon gas after mixing the presoma obtained in step (1) with selenium powder.
4. application according to claim 3, which is characterized in that in step (1), the soluble zinc salt is six nitric hydrates
One of zinc or zinc chloride.
5. application according to claim 4, which is characterized in that in step (1), in the reaction solution zinc nitrate hexahydrate with
The mass ratio of methylimidazole is 42-64:34-58.
6. application according to claim 3, which is characterized in that in step (1), the time for standing reaction is 10-
30h。
7. application according to claim 3, which is characterized in that in step (1), the temperature of the drying is less than 90 DEG C.
8. application according to claim 3, which is characterized in that in step (2), the mass ratio 1 of the presoma and selenium powder:
1-4。
9. application according to claim 3, which is characterized in that in step (2), the volume of hydrogen point in the mixed atmosphere
Number is 3-10%.
10. application according to claim 3, which is characterized in that in step (2), the calcining is specifically with 2-10 DEG C/min
Rate be warming up to 400-800 DEG C after keep the temperature 1-4h.
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| CN111180725A (en) * | 2020-01-22 | 2020-05-19 | 河北大学 | Method for preparing aluminum battery anode material by utilizing MOF (metal organic framework) to induce metal selenide |
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| CN114122389A (en) * | 2021-11-26 | 2022-03-01 | 合肥工业大学 | Zinc-manganese selenide solid solution positive electrode material for water-based zinc ion battery and preparation method thereof |
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| CN109360986B (en) | 2020-10-13 |
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