CN107634225A - A kind of Dual-ion cell preparation method using hard carbon positive electrode - Google Patents
A kind of Dual-ion cell preparation method using hard carbon positive electrode Download PDFInfo
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- CN107634225A CN107634225A CN201710772100.XA CN201710772100A CN107634225A CN 107634225 A CN107634225 A CN 107634225A CN 201710772100 A CN201710772100 A CN 201710772100A CN 107634225 A CN107634225 A CN 107634225A
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- positive electrode
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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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a kind of Dual-ion cell preparation method using hard carbon positive electrode, methods described comprises the following steps：Presoma dewater treatment first；Then the presoma after dewater treatment carries out high temperature cabonization processing, obtains hard carbon positive electrode；Then mixing carbon negative pole material is prepared；Metal salt electrolyte is prepared again；Hard carbon positive electrode, mixing carbon negative pole material and metal salt electrolyte are finally assembled into Dual-ion cell.The present invention directly carries out high temperature cabonization to presoma and handles to obtain hard carbon material, preparation method is simple, raw material are easy to get, production cost is low, and hard carbon material maintains the original pattern feature of predecessor, and the load capacity of anion increases considerably in positive electrode in charging process, improve the specific capacity of Dual-ion cell, the hard carbon material safety of preparation, its Dual-ion cell prepared environmental protection, is easy to reclaim.
Description
Technical field
The present invention relates to Dual-ion cell technical field, more particularly to a kind of Dual-ion cell using hard carbon positive electrode
Preparation method.
Background technology
Lithium ion battery (LIBs) is higher than energy, good cycle, is achieved in consumer electronics field application huge
Success, but lithium ion battery cost is high, while prices of raw materials height is limited to, the current cost of lithium ion battery reduces space
It is limited.In order to reduce cost, the battery of a variety of high-energy-densities is developed, wherein emerging double ion electricity recent years
Pond is exactly one of them.
There was only Li between the both positive and negative polarity of lithium ion battery+It is different to participate in reaction, during the charging of Dual-ion cell,
Anion migrates in the presence of electric field to positive pole, is embedded among anode structure, and cation migrates to negative pole, is embedded into negative pole
Among, the process of electric discharge then in contrast, the ion abjection in positive pole and negative pole, returns in electrolyte, recovers the dense of electrolyte
Degree.The quantity of anion insertion positive electrode directly affects Dual-ion cell capacity, the positive pole that Dual-ion cell uses at present
Material is mainly graphite material, and gap is smaller between layers for graphite positive electrode, and its highest theoretical capacity only has 106mA h
g-1；Graphite positive electrode only provides 60-70mA h g in lithium Dual-ion cell practical application-1The specific capacity of left and right.Cause
This, Dual-ion cell capacity need to be improved.
The content of the invention
To solve the problems such as current Dual-ion cell provides relatively low specific capacity using graphite positive electrode, the present invention provides
A kind of Dual-ion cell preparation method using hard carbon positive electrode.
In order to solve the above technical problems, the technical solution adopted in the present invention is：A kind of pair using hard carbon positive electrode
Ion battery preparation method, methods described comprise the following steps：
Presoma dewater treatment；
Presoma after dewater treatment carries out high temperature cabonization processing, obtains hard carbon positive electrode；
Prepare mixing carbon negative pole material；
Prepare metal salt electrolyte；
Hard carbon positive electrode, mixing carbon negative pole material and metal salt electrolyte are assembled into Dual-ion cell.
Further, the presoma be in plant, biomass class, high polymer material class, fossil fuel class etc. extremely
Few one kind；The plant presoma be potato, corncob cellulose, taro, sweet potato, cassava, at least one of pumpkin, the macromolecule
Material precursor is pyrroles, PVC, PET, PEN, EN at least one, it is further preferred that the fossil fuel presoma is coal
At least one of slag, acetylene black.
Further, the high temperature cabonization processing is under nitrogen protection atmosphere, to preceding at a high temperature of 700-1200 DEG C
Drive body and carry out carbonization treatment 2-24h.
Further, the method for preparing mixing carbon negative pole material is to enter two or more carbon materials by a certain percentage
Row mixing, then grinds 10-15h, then be warming up under protective gas atmosphere with 2-5 DEG C of heating rate under exhausted water environment
80-150 DEG C, then constant temperature processing 10-20h, obtains mixing carbon negative pole material.
Further, the carbon material is graphene, graphene oxide, graphite, graphite powder, nano-graphite, nano-graphite
Powder, CNT, active powdered carbon, expanded graphite, expanded graphite alkene, three-dimensional grapheme, carbon black, soft carbon, at least the one of graphite nodule
Kind.
Further, the metal salt electrolyte is lithium fluoride (or sodium, potassium), lithium hexafluoro phosphate (or sodium, potassium), tetrafluoro boron
One kind in sour lithium (or sodium, potassium), lithium perchlorate (or sodium, potassium).
From the above-mentioned description to structure of the present invention, compared to the prior art, the invention has the advantages that：
1st, the present invention directly handles to obtain hard carbon material to presoma progress high temperature cabonization, and preparation method is simple, raw material
It is easy to get, production cost is low, the hard carbon material safety of preparation so that its Dual-ion cell prepared environmental protection, is easy to reclaim.
2nd, hard carbon material prepared by the present invention maintains the original pattern feature of predecessor, and layer structure is unordered irregular,
The gap length of interlayer differs, and many interlamellar spacings are more than graphite layers away from so that anion in positive electrode in charging process
Load capacity increase considerably, so as to improve the specific capacity of Dual-ion cell, while anion can also be substantially completely in electric discharge
Deintercalation, it is unattenuated by long-term circulation volume so that Dual-ion cell cycle life overlength.
Brief description of the drawings
The accompanying drawing for forming the part of the application is used for providing a further understanding of the present invention, schematic reality of the invention
Apply example and its illustrate to be used to explain the present invention, do not form inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 is a kind of flow chart of Dual-ion cell preparation method using hard carbon positive electrode of the invention；
Fig. 2 is the TEM figures and SEM figures for the hard carbon positive electrode that the embodiment of the present invention 1 provides；
Fig. 3 is charging and discharging curve figure of the lithium Dual-ion cell of the offer of the embodiment of the present invention 1 under 1A/g current densities；
Fig. 4 is long-term charge and discharge cycles of the lithium Dual-ion cell of the offer of the embodiment of the present invention 1 under 1A/g current densities
Curve map；
Fig. 5 is the TEM figures and SEM figures for the hard carbon positive electrode that the embodiment of the present invention 2 provides；
Fig. 6 is charging and discharging curve figure of the sodium Dual-ion cell of the offer of the embodiment of the present invention 2 under 1A/g current densities；
Fig. 7 is long-term charge and discharge cycles of the sodium Dual-ion cell of the offer of the embodiment of the present invention 2 under 1A/g current densities
Curve map；
Fig. 8 is charge and discharge cycles of the sodium Dual-ion cell of the offer of the embodiment of the present invention 2 under 100mA/g current density
Curve map.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
With reference to figure 1, a kind of Dual-ion cell preparation method using hard carbon positive electrode, methods described includes following step
Suddenly：
S101, presoma dewater treatment, the presoma are plant, biomass class, high polymer material class, fossil fuel
At least one of class etc.；The plant presoma is potato, corncob cellulose, taro, sweet potato, cassava, pumpkin etc., the high score
Sub- material precursor is pyrroles, PVC, PET, PEN, EN etc., it is further preferred that the fossil fuel presoma is cinder, second
Acetylene black etc.；
S102, the presoma after dewater treatment carry out high temperature cabonization processing, obtain hard carbon positive electrode, the high temperature cabonization
Handle as under nitrogen protection atmosphere, carbonization treatment 2-24h is carried out to presoma at a high temperature of 700-1200 DEG C；
S103, mixing carbon negative pole material is prepared, the method for preparing mixing carbon negative pole material is by two or more carbon
Material is mixed by a certain percentage, and 10-15h is then ground under exhausted water environment, then with 2-5 DEG C under protective gas atmosphere
Heating rate is warming up to 80-150 DEG C, then constant temperature processing 10-20h, obtains mixing carbon negative pole material, the carbon material is graphite
Alkene, graphene oxide, graphite, graphite powder, nano-graphite, Nano graphite powder, CNT, active powdered carbon, expanded graphite, expansion
Graphene, three-dimensional grapheme, carbon black, soft carbon, graphite nodule etc.；
S104, prepares metal salt electrolyte, and the metal salt electrolyte is lithium fluoride (or sodium, potassium etc.), lithium hexafluoro phosphate
One kind in (or sodium, potassium etc.), LiBF4 (or sodium, potassium etc.), lithium perchlorate (or sodium, potassium etc.)；
S105, hard carbon positive electrode, mixing carbon negative pole material and metal salt electrolyte are assembled into Dual-ion cell.
The present invention directly carries out high temperature cabonization to presoma and handles to obtain hard carbon material, and preparation method is simple, and raw material are easy
, production cost is low, the hard carbon material safety of preparation so that its Dual-ion cell prepared environmental protection, is easy to reclaim；What is prepared is hard
Carbon material maintains the original pattern feature of predecessor, and layer structure is unordered irregular, and the gap length of interlayer differs, and a lot
Interlamellar spacing be more than graphite layers away from so that the load capacity of anion increases considerably in positive electrode in charging process, so as to carry
The specific capacity of high Dual-ion cell, at the same electric discharge when anion can also substantially completely deintercalation, do not waned by long-term circulation volume
Subtract so that Dual-ion cell cycle life overlength.
Lithium Dual-ion cell preparation method：
S101, corncob cellulose is cleaned up, carry out dewater treatment and obtain high temperature cabonization presoma；
S102, then the corncob cellulose after dehydration is put into the tube type resistance furnace of nitrogen protection atmosphere, in 1000 DEG C of height
The lower carbonization treatment 3h of temperature, obtains hard carbon positive electrode.
S103, it is 6 by weight by graphene and Nano graphite powder：4 are mixed, and are then ground under exhausted water environment
12h, then 100 DEG C are warming up to 3 DEG C of heating rate under protective gas atmosphere, then constant temperature processing 15h, obtains mixing carbon and bears
Pole material；
S104, prepare 2M lithium hexafluoro phosphates (LiPF6) electrolyte；
S105, lithium Dual-ion cell battery assembling, in ar gas environment (H2O<0.5ppm, O2<It is complete in glove box 0.5ppm)
Into the assembling of lithium Dual-ion cell；
The TEM figures and SEM figures of the hard carbon positive electrode provided from Fig. 2 the present embodiment can be seen that hard carbon material by infinite layers
Shape structure composition, layer structure is clearly demarcated, and layer structure is unordered irregular, and gap length differs and is covered with porous knot between layers
Structure, this can increase considerably PF6- anion is embedded in load capacity, so as to improve the specific capacity of lithium Dual-ion cell.
As shown in Figure 3-4, the electrochemistry of lithium Dual-ion cell is have studied using charging and discharging curve, cyclical stability etc.
Energy.Fig. 4 shows the 10th time, 100 times, the charged/discharged curve map of 300 times, and the discharge capacity of lithium Dual-ion cell is from the 10th
Secondary 122mA h g-1Increase to the 150mA h g of the 300th time-1.Fig. 3 is the length under lithium Dual-ion cell 1A/g high current densities
Phase stable circulation performance, it provides 150mA h g after 350 circulations-1High power capacity, be 2 times of graphite positive electrode,
And discharge capacity has slow growth trend with the increase of cycle-index.Therefore prepared using hard carbon material as positive electrode
Lithium Dual-ion cell has high specific discharge capacity and super good long-term cycle stability energy.Lithium Dual-ion cell is beaten with iron nail
Individual hole, battery remain to lightening LED lamp, illustrate battery still can normal work, show that its is safe to use.
Embodiment 2
Sodium Dual-ion cell preparation method：
S101, corncob cellulose is cleaned up, carry out dewater treatment and obtain high temperature cabonization presoma；
S102, then the corncob cellulose after dehydration is put into the tube type resistance furnace of nitrogen protection atmosphere, in 900 DEG C of high temperature
Lower carbonization treatment 2h, obtains hard carbon positive electrode.
S103, it is 8 by weight by graphene and nano-graphite：2 are mixed, and then grind 12h under exhausted water environment,
100 DEG C are warming up to 3 DEG C of heating rate under protective gas atmosphere again, then constant temperature processing 15h, obtain mixing Carbon anode material
Material.
S104, prepare 3M sodium hexafluoro phosphates (NaPF6) electrolyte.
S105, sodium Dual-ion cell battery assembling, in ar gas environment (H2O<0.5ppm, O2<It is complete in glove box 0.5ppm)
Into the assembling of sodium Dual-ion cell.
The TEM figures of hard carbon positive electrode are provided from Fig. 5 the present embodiment and SEM figures can be seen that hard carbon material by countless stratiforms
Structure composition, layer structure is clearly demarcated, and layer structure is unordered irregular, and gap length differs and is covered with porous knot between layers
Structure, this can increase considerably PF6- anion is embedded in load capacity, so as to improve the specific capacity of sodium Dual-ion cell.
As shown in fig. 6-7, the electrochemistry of sodium Dual-ion cell is have studied using charging and discharging curve, cyclical stability etc.
Energy.Fig. 6 shows the 10th time, 100 times, the charged/discharged curve map of 1000 times, and the discharge capacity of sodium Dual-ion cell is from the 10th
Secondary 107mA h g-1Increase to the 132mA h g of the 100th time-1.Fig. 7 is sodium Dual-ion cell under 1A/g high current densities
Long-term cycle stability energy, its by 700 times circulation after provide 112mA hg-1High power capacity.Therefore hard carbon material is used
The sodium Dual-ion cell prepared as positive electrode has high specific discharge capacity and super good long-term cycle stability energy.
Embodiment 3
Lithium Dual-ion cell preparation method：
S101, pyrroles's high polymer material is cleaned up, carry out dewater treatment and obtain high temperature cabonization presoma；
S102, then pyrroles is put into the tube type resistance furnace of nitrogen protection atmosphere, the carbonization treatment under 1100 DEG C of high temperature
10h, obtain hard carbon positive electrode.
S103, it is 6 by weight by graphene and Nano graphite powder：4 are mixed, and are then ground under exhausted water environment
12h, then 100 DEG C are warming up to 3 DEG C of heating rate under protective gas atmosphere, then constant temperature processing 15h, obtains mixing carbon and bears
Pole material；
S104, prepare 2.5M lithium hexafluoro phosphates (LiPF6) electrolyte；
S105, lithium Dual-ion cell battery assembling, in ar gas environment (H2O<0.5ppm, O2<It is complete in glove box 0.5ppm)
Into the assembling of lithium Dual-ion cell；
Battery charge and discharge under 100mA/g current density is can be seen that from the cyclic curve figure of Fig. 8 lithium Dual-ion cell
Electricity circulation, discharge capacity are up to the h of mA more than 240 g-1。
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (6)
- A kind of 1. Dual-ion cell preparation method using hard carbon positive electrode, it is characterised in that：Methods described includes following step Suddenly：Presoma dewater treatment；Presoma after dewater treatment carries out high temperature cabonization processing, obtains hard carbon positive electrode；Prepare mixing carbon negative pole material；Prepare metal salt electrolyte；Hard carbon positive electrode, mixing carbon negative pole material and metal salt electrolyte are assembled into Dual-ion cell.
- A kind of 2. Dual-ion cell preparation method using hard carbon positive electrode according to claim 1, it is characterised in that：Institute Presoma is stated as at least one of plant, biomass class, high polymer material class, fossil fuel class etc.；The plant forerunner Body be potato, corncob cellulose, taro, sweet potato, cassava, at least one of pumpkin, the high polymer material presoma be pyrroles, PVC, PET, PEN, EN at least one, the fossil fuel presoma are cinder, at least one of acetylene black.
- A kind of 3. Dual-ion cell preparation method using hard carbon positive electrode according to claim 1, it is characterised in that：Institute It is under nitrogen protection atmosphere to state high temperature cabonization processing, and carbonization treatment 2- is carried out to presoma at a high temperature of 700-1200 DEG C 24h。
- A kind of 4. Dual-ion cell preparation method using hard carbon positive electrode according to claim 1, it is characterised in that：Institute The method for preparing mixing carbon negative pole material is stated as two or more carbon materials are mixed by a certain percentage, then in exhausted water ring 10-15h is ground under border, then 80-150 DEG C is warming up to 2-5 DEG C of heating rate under protective gas atmosphere, then constant temperature is handled 10-20h, obtain mixing carbon negative pole material.
- A kind of 5. Dual-ion cell preparation method using hard carbon positive electrode according to claim 4, it is characterised in that：Institute Carbon material is stated as graphene, graphene oxide, graphite, graphite powder, nano-graphite, Nano graphite powder, CNT, activated carbon Powder, expanded graphite, expanded graphite alkene, three-dimensional grapheme, carbon black, soft carbon, at least one of graphite nodule.
- A kind of 6. Dual-ion cell preparation method using hard carbon positive electrode according to claim 1, it is characterised in that：Institute Metal salt electrolyte is stated as lithium fluoride (or sodium, potassium), lithium hexafluoro phosphate (or sodium, potassium), LiBF4 (or sodium, potassium), high chlorine One kind in sour lithium (or sodium, potassium).
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Cited By (7)
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| CN108270006A (en) * | 2018-01-30 | 2018-07-10 | 北京大学 | A kind of sodium base Dual-ion cell |
| CN108448165A (en) * | 2018-03-15 | 2018-08-24 | 北京化工大学 | A kind of Dual-ion cell and preparation method thereof for making cathode using trielement composite material |
| CN108615932A (en) * | 2018-03-30 | 2018-10-02 | 南京大学 | Negative and positive double ion rocking chair type secondary cell and preparation method thereof |
| CN108878774A (en) * | 2018-06-26 | 2018-11-23 | 上海汉行科技有限公司 | A kind of complex carbon material and its preparation method and application |
| CN110474094A (en) * | 2018-05-10 | 2019-11-19 | 福建新峰二维材料科技有限公司 | A kind of potassium double ion capacitor batteries based on mixed electrode |
| CN112552941A (en) * | 2020-12-18 | 2021-03-26 | 袁新华 | Low-resistance biomass carbon material and preparation method thereof |
| CN116072818A (en) * | 2023-02-17 | 2023-05-05 | 大连理工大学 | Soft carbon material anode of double-ion battery and preparation method thereof |
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| CN116072818A (en) * | 2023-02-17 | 2023-05-05 | 大连理工大学 | Soft carbon material anode of double-ion battery and preparation method thereof |
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