CN109817954A - A kind of 3-D ordered multiporous carbon embeds the preparation method of oxide material - Google Patents
A kind of 3-D ordered multiporous carbon embeds the preparation method of oxide material Download PDFInfo
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- CN109817954A CN109817954A CN201910234698.6A CN201910234698A CN109817954A CN 109817954 A CN109817954 A CN 109817954A CN 201910234698 A CN201910234698 A CN 201910234698A CN 109817954 A CN109817954 A CN 109817954A
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- mixed solution
- ethanol
- tannin
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses the preparation methods that a kind of 3-D ordered multiporous carbon embeds oxide material, it is characterized in that: the preparation method is divided into two steps: (1) A Polystyrene Spheres Template being impregnated in tannin-transition metal ions mixed solution, construct metal-polyphenol mixture network of three-dimensional interpenetrating；(2) by the A Polystyrene Spheres Template after dipping it is vacuum dried and heat treatment, obtain 3-D ordered multiporous carbon embed oxide.3-D ordered multiporous carbon, which embeds oxide, makes the transmission isotropism of electronics and ion, and polarization problem when it is used as lithium ion battery negative material can be effectively suppressed, and improves high rate performance；3-D ordered multiporous carbon is crushed caused by can also alleviating oxide in charge and discharge process due to bulk effect, improves the cyclical stability of electrode material.This method have many advantages, such as preparation is simple, the period is short, without complicated special equipment, it is easy to accomplish large-scale industrial production.
Description
Technical field
The invention belongs to lithium cell cathode material and its preparation technical fields, and in particular to using polystyrene spheres as mould
Plate, the 3-D ordered multiporous carbon that tannin-transition metal ions mixture is presoma to prepare embed the preparation of oxide material
Method.
Background technique
Lithium ion battery specific capacity is big, stability is good, is widely used in the fields such as portable device as mobile power source.Stone
Ink is the negative electrode material of current commercial li-ion battery, but its lithium storage content is only 372 mAh g-1, it is limited in other necks
The application in domain.(Shang H, Zuo Z, Li L, et al. Ultrathin Graphdiyne Nanosheets Grown
In Situ on Copper Nanowires and Their Performance as Lithium-ion Battery
Anodes[J]. Angewandte Chemie International Edition, 2018, 57(3):774-778. Li
H, Wang Z, Chen L, et al. Research on Advanced Materials for Li-ion Batteries
[J] Advanced Materials, 2009,21 (45): 4593-4607.) there is transition metal oxide theoretical storage lithium to hold
Measure height (400 ~ 1100 mAh g-1), the advantages that preparation is simple, rich content, be potential negative electrode of lithium ion battery material of new generation
Expect (Jiang J, Li Y, Liu J, et al. Recent Advances in Metal Oxide-based
Electrode Architecture Design for Electrochemical Energy Storage[J]. Advanced
Materials, 2012,24 (38): 5166-5180.).However, transition metal oxide (MxOy) in electric conductivity it is poor, and
During charge and discharge cycles, there are significant bulk effect, cause its high rate performance poor, cyclical stability is bad.(Li M,
Du H , Kuai L , et al. Scalable Dry Production Process of a Superior 3D Net‐
Like Carbon‐Based Iron Oxide Anode Material for Lithium‐Ion Batteries[J].
Angewandte Chemie, 2017, 129(41):12649. Zheng M , Tang H , Li L , et al.
Hierarchically Nanostructured Transition Metal Oxides for Lithium-Ion
Batteries [J] Advanced Science, 2018,5:1700592.).Using carbon material to MxOyCarry out coating decoration
It is to improve MxOyEffective ways.Currently, having developed the two-dimensional M of a peacekeepingxOy/ carbon composite electrode material (Ko S, Lee J
I, Yang H S, et al. Mesoporous CuO Particles Threaded with CNTs for High-
Performance Lithium-ion Battery Anodes[J]. Advanced Materials, 2012, 24(32):
4451-4456. Wang B, Wu X L, Shu C Y, et al. Synthesis of CuO/Graphene
Nanocomposite as a High-performance Anode Material for Lithium-ion Batteries
[J]. Journal of Materials Chemistry, 2010, 20(47):10661-10664. Ren M, Yang M,
Liu W, et al. Ultra-small Fe3O4 nanocrystals decorated on 2D graphene
nanosheets with excellent cycling stability as anode materials for lithium
ion batteries[J]. Electrochimica Acta, 2016, 194: 219-227. Ming H, Zhou H,
Zhu X, et al. Advanced Metal Oxide@ Carbon Nanotubes for High‐Energy Lithium‐
Ion Full Batteries [J] Energy Technology, 2018,6 (4): 766-772.) however, a peacekeeping two
The charge transmission for tieing up electrode material has anisotropy, and material has polarization problem on certain dimension always.(Amin R,
Maier J, Balaya P, et al. Ionic and Electronic Transport in Single
Crystalline LiFePO4 Grown by Optical Floating Zone Technique[J]. Solid State
Ionics, 2008, 179(27):1683-1687. Lytle J C, Yan H, Ergang N S, et al.
Structural and Electrochemical Properties of Three-dimensionally Ordered
Macroporous Tin Oxide Films[J]. Journal of Materials Chemistry, 2004, 14(10):
1616-1622. Arthur T S, Bates D J, Nicolas C, et al. Three-dimensional
Electrodes and Battery Architectures [J] MRS Bulletin, 2011,36 (7): 523-531.)
The effective way to solve the above problems be developed as electrode material have 3-D ordered multiporous carbon embed oxide material.
Summary of the invention
The present invention provides a kind of 3-D ordered multiporous carbon for preparing being simple and efficient to embed oxide material method, i.e., with poly-
Styrene ball is template, Baybery tannin-Cu2+Mixture is presoma, and after thermally treated, it is embedded to prepare 3-D ordered multiporous carbon
Oxide material.3-D ordered multiporous carbon can effectively strengthening electronic and lithium ion transport dynamics, the body of effective buffer oxide
Product effect, to obtain high circulation stability and high rate performance.
Technical solution of the present invention is divided into two steps: (1) A Polystyrene Spheres Template being impregnated in tannin-mistake
It crosses in metallic ion mixed liquor, constructs metal-polyphenol mixture network of three-dimensional interpenetrating；(2) by the polystyrene after dipping
Ball template is vacuum dried and is heat-treated, and obtains 3-D ordered multiporous carbon and embeds oxide material.
Further, the A Polystyrene Spheres Template is styrene after emulsion polymerization, is made through high speed centrifugation.
Further, the tannin is Baybery tannin.
Further, the transition metal ions is Cu2+。
Further, the Cu2+From nitrate trihydrate copper.
Further, the step (1) specifically: A Polystyrene Spheres Template is impregnated in Baybery tannin-Cu2+Ethanol/water
In mixed solution.
Further, the Baybery tannin-Cu2+Ethanol/water mixed solution is Baybery tannin and nitrate trihydrate copper dissolution
It is obtained in the sonicated 10-20 min of ethanol/water mixed solution.
Further, the Baybery tannin-Cu2+In ethanol/water mixed solution, the quality of Baybery tannin and nitrate trihydrate copper
Than for 1:1,1:2 or 2:1.
Further, the Baybery tannin-Cu2+In ethanol/water mixed solution, the volume ratio of ethanol/water mixed solution is
1:1。
Further, the A Polystyrene Spheres Template and Baybery tannin mass ratio are 1:1.
Further, A Polystyrene Spheres Template vacuum drying temperature≤80 DEG C in the step (2) after dipping, when dry
Between 2-3 hours.
Further, the heat treatment method in the step (2) are as follows: the A Polystyrene Spheres Template after drying is placed in tubular type
In furnace, in N2Under atmosphere, 500 DEG C are warming up to the heating rate of 5 DEG C/min, keeps 2h.
3-D ordered multiporous carbon obtained by the present invention, which embeds oxide material, can be used as lithium ion battery negative material.
Further, the lithium ion battery negative material is made by following preparation method:
(1) ethanol/water mixed solution is obtained after mixing second alcohol and water by the volume ratio of 1:1；
(2) by mass ratio be 1:1,1:2 or 2:1 Baybery tannin and nitrate trihydrate copper dissolution in ethanol/water mixed solution (1:
1, V/V) Baybery tannin-Cu, is obtained2+Ethanol/water mixed solution；
(3) A Polystyrene Spheres Template is impregnated in Baybery tannin-Cu2+Ethanol/water mixed solution 2-3 hours, wherein polystyrene
Ball template and Baybery tannin mass ratio are 1:1；
(4) then the A Polystyrene Spheres Template after dipping is taken out, is dried in vacuo 3 h under the conditions of 60 DEG C；It again will be after drying
A Polystyrene Spheres Template is placed in tube furnace, in N2Under atmosphere, with 5 DEG C of min-1Heating rate be warming up to 500 DEG C, keep 2h,
Obtained product is 3D Cu2O-CuO@C lithium ion battery negative material.
Baybery tannin used in the method for the present invention is condensed tannin, and structure is more steady compared to hydrolysable tannins
It is fixed, in addition, there are a large amount of ortho position phenolic hydroxyl group, energy and Cu on Baybery tannin2+Stable coordinate bond is formed, so that Cu2+Can and its
Stable bond.Therefore, the material prepared by the present invention has good high rate performance and cyclical stability, and prepares simple, week
Phase is short, energy consumption is small, without complicated special equipment the advantages that, it is easy to accomplish large-scale industrial production.
Detailed description of the invention
Fig. 1 is 3D Cu prepared by collagenous fibres and the embodiment of the present invention 12The X-ray diffraction power spectrum (XRD) of O-CuO@C
Figure.As seen from the figure, 3D Cu2There are Cu in O-CuO@C2O and CuO.
Fig. 2 is 3D Cu prepared by the embodiment of the present invention 12In O-CuO C and the x-ray photoelectron spectroscopy of O element (XPS)
Figure.Wherein figure (a) is 3D Cu2The XPS figure of Cu element, figure (b) are 3D Cu in O-CuO@C2The XPS figure of O element in O-CuO@C,
By the xps energy spectrum figure of Cu and O element it is found that Cu2+It is changed into Cu after thermally treated2O and CuO.
Fig. 3 is 3D Cu prepared by the embodiment of the present invention 12The Raman spectrogram of [email protected] seen from the figure, Baybery tannin passes through
It crosses high temperature cabonization and forms graphitic carbon material.
Fig. 4 is 3D Cu prepared by the embodiment of the present invention 12Scanning electron microscope (SEM) figure of [email protected] can by figure
Know, 3D Cu2O-CuO@C has 3-D ordered multiporous structure.
Fig. 5 is 3D Cu prepared by the embodiment of the present invention 12Transmission electron microscope (TEM) figure of [email protected] can by figure
Know, in 3D Cu2O-CuO@C is 3-D ordered multiporous structure, Cu2O-CuO nano particle is distributed in 3-D ordered multiporous carbon.
Fig. 6 is 3D Cu prepared by the embodiment of the present invention 12The high rate performance of O-CuO@C.
Fig. 7 is 3D Cu prepared by the embodiment of the present invention 22The high rate performance of O-CuO@C.
Fig. 8 is 3D Cu prepared by the embodiment of the present invention 32O-CuO@C is in 0.5 Ag-1Under cyclical stability.
Specific embodiment
The present invention is specifically described below by embodiment, and technical solution of the present invention be not limited to it is set forth below
The specific embodiment of act.
It is necessarily pointed out that the present embodiment is served only for, invention is further explained, should not be understood as pair
The limitation of the scope of the present invention some nonessential changes according to what foregoing invention content was done for those skilled in the art
Into with adjustment, be also considered as and be within the scope of the present invention.It is worth noting that 1) number of material used in following embodiment
It is mass parts.2) electrode material prepared by following embodiment is to be assembled into fastening lithium ionic cell to test its battery performance,
The specific assembly method of battery is as follows: the 3-D ordered multiporous carbon of preparation is embedded Cu2O-CuO(Cu2O-CuO@C), conductive agent and
Binder is that 7:2:1 is coated on copper foil after mixing in mass ratio, and working electrode is made after dry；By working electrode, lithium
Piece, diaphragm, electrolyte (using volume ratio for 1:1:1 ethylene carbonate/methyl ethyl carbonate/dimethyl carbonate as the 1.0 of solvent
mol L-1 LiPF6) assembled in the glove box filled with argon gas, it is prepared into CR2032 type button cell；By assembled button
Formula battery is placed on charge-discharge tester (new prestige Neware, CT-3008) and tests its battery performance.
Embodiment 1
1.0 g Baybery tannins (BT) and 2.0 g nitrate trihydrate copper dissolutions are in 20 mL ethanol/water mixed solutions (1:1, V/V).
1.0 g A Polystyrene Spheres Templates (PS ball template) are impregnated in 3 h in above-mentioned solution.Then the PS ball template after dipping is taken out,
3 h are dried in vacuo under the conditions of 60 DEG C.PS ball template after drying is placed in tube furnace, in N2Under atmosphere, with 5 DEG C of min-1
Heating rate be warming up to 500 DEG C, keep 2h.Obtained product is 3D Cu2O-CuO@C lithium ion battery negative material.
As shown in Figure 1,3D Cu2O-CuO@C has Cu2O and CuO typical diffractive peak.
By the xps energy spectrum figure of Cu and O element in Fig. 2 it is found that Cu2+Cu is formd after thermally treated2O and CuO.
From the figure 3, it may be seen that Baybery tannin forms graphitic carbon by high temperature cabonization.
As shown in Figure 4,3D Cu2O-CuO@C is 3-D ordered multiporous structure.
As shown in Figure 5, in 3D Cu2In O-CuO@C, Cu2O-CuO nano particle is distributed in 3-D ordered multiporous structural carbon
On.
By gained 3D Cu2O-CuO@C is assembled into button cell as working electrode, tests it on charge-discharge tester
High rate performance.As shown in fig. 6,3D Cu2O-CuO@C current density be respectively 0.2,0.4,0.6,0.8,1.0,2.0,4.0,
8.0 A g-1When, specific discharge capacity is respectively 493,433,388,355,353,283,231,196,173 mAh g-1。
Embodiment 2
1.0 g Baybery tannins (BT) and 1.0 g nitrate trihydrate copper dissolutions are in 20 mL ethanol/water mixed solutions (1:1, V/V).
1.0 g PS ball templates are impregnated in 3 h in above-mentioned solution.Then the PS ball template after dipping is taken out, vacuum under the conditions of 60 DEG C
Dry 3 h.PS ball template after drying is placed in tube furnace, in N2Under atmosphere, with 5 DEG C of min-1Heating rate be warming up to
500 DEG C, keep 2h.Obtained product is 3D Cu2O-CuO@C lithium ion battery negative material.
By gained 3D Cu2O-CuO@C is assembled into button cell as working electrode, tests it on charge-discharge tester
High rate performance.As shown in fig. 7,3D Cu2O-CuO@C is in 0.2,0.4,0.8,1.0,2.0,4 and 6 Ag-1Current density under, put
Capacitance is respectively up to 511,444,392,371,357,286,233 and 198 mAh g-1。
Embodiment 3
1.0 g Baybery tannins (BT) and 0.5 g nitrate trihydrate copper dissolution are in 20 mL ethanol/water mixed solutions (1:1, V/V).
1.0 g PS ball templates are impregnated in 3 h in above-mentioned solution.Then the PS ball template after dipping is taken out, vacuum under the conditions of 60 DEG C
Dry 3 h.PS ball template after drying is placed in tube furnace, in N2Under atmosphere, with 5 DEG C of min-1Heating rate be warming up to
500 DEG C, keep 2h.Obtained product is 3D Cu2O-CuO@C lithium ion battery negative material.
By gained 3D Cu2O-CuO@C is assembled into button cell as working electrode, tests it on charge-discharge tester
Cycle performance.As shown in figure 8,3D Cu2O-CuO@C is in 0.5 Ag-1By 200 times circulation after discharge capacity can stablize ~
576 mAh g-1。
Claims (14)
1. a kind of 3-D ordered multiporous carbon embed oxide material preparation method, it is characterised in that: the preparation method include with
Lower step:
(1) A Polystyrene Spheres Template is impregnated in tannin-transition metal ions mixed solution, constructs the metal-of three-dimensional interpenetrating
Polyphenol mixture network；
(2) by the A Polystyrene Spheres Template after dipping it is vacuum dried and heat treatment, obtain 3-D ordered multiporous carbon embed oxygen
Compound material.
2. according to the method described in claim 1, it is characterized by: the A Polystyrene Spheres Template is styrene through emulsion polymerization
Afterwards, then by high speed centrifugation it is made.
3. according to the method described in claim 1, it is characterized by: the tannin is Baybery tannin.
4. according to the method described in claim 1, it is characterized by: the transition metal ions is Cu2+。
5. according to the method described in claim 4, it is characterized by: the Cu2+From nitrate trihydrate copper.
6. according to the method described in claim 1, it is characterized by: the step (1) specifically: soak A Polystyrene Spheres Template
Stain is in Baybery tannin-Cu2+In ethanol/water mixed solution.
7. according to the method described in claim 6, it is characterized by: the Baybery tannin-Cu2+Ethanol/water mixed solution is
Baybery tannin and nitrate trihydrate copper dissolution are obtained in the sonicated 10-20 min of ethanol/water mixed solution.
8. method according to claim 6 or 7, it is characterised in that: the Baybery tannin-Cu2+Ethanol/water mixed solution
In, the mass ratio of Baybery tannin and nitrate trihydrate copper is 1:1,1:2 or 2:1.
9. method according to claim 6 or 7, it is characterised in that: the Baybery tannin-Cu2+Ethanol/water mixed solution
In, the volume ratio of ethanol/water mixed solution is 1:1.
10. method according to claim 6 or 7, it is characterised in that: the A Polystyrene Spheres Template and Baybery tannin matter
Amount is than being 1:1.
11. according to the method described in claim 1, it is characterized by: the step (2) in dipping after A Polystyrene Spheres Template
Vacuum drying temperature≤80 DEG C, drying time 2-3 hour.
12. according to the method described in claim 1, it is characterized by: heat treatment method in the step (2) are as follows: will dry
A Polystyrene Spheres Template afterwards is placed in tube furnace, in N2Under atmosphere, 500 DEG C are warming up to the heating rate of 5 DEG C/min, is kept
2h。
13. a kind of 3-D ordered multiporous carbon as obtained by claim 1-12 any one the method embeds oxide material
Preparing the purposes in lithium ion battery negative material.
14. purposes according to claim 13, which is characterized in that the lithium ion battery negative material is by following preparation
Method is made:
(1) ethanol/water mixed solution is obtained after mixing second alcohol and water by the volume ratio of 1:1；
(2) by mass ratio be 1:1,1:2 or 2:1 Baybery tannin and nitrate trihydrate copper dissolution in ethanol/water mixed solution (1:
1, V/V) Baybery tannin-Cu, is obtained2+Ethanol/water mixed solution；
(3) A Polystyrene Spheres Template is impregnated in Baybery tannin-Cu2+Ethanol/water mixed solution 2-3 hours, wherein polystyrene
Ball template and Baybery tannin mass ratio are 1:1；
(4) then the A Polystyrene Spheres Template after dipping is taken out, is dried in vacuo 3 h under the conditions of 60 DEG C；It again will be after drying
A Polystyrene Spheres Template is placed in tube furnace, in N2Under atmosphere, with 5 DEG C of min-1Heating rate be warming up to 500 DEG C, keep 2h,
Obtained product is 3D Cu2O-CuO@C lithium ion battery negative material.
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Application publication date: 20190528 |