CN109704303A - A kind of compound biomass carbon material and its preparation and the application in lithium selenium cell coated separator - Google Patents
A kind of compound biomass carbon material and its preparation and the application in lithium selenium cell coated separator Download PDFInfo
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- CN109704303A CN109704303A CN201811465566.6A CN201811465566A CN109704303A CN 109704303 A CN109704303 A CN 109704303A CN 201811465566 A CN201811465566 A CN 201811465566A CN 109704303 A CN109704303 A CN 109704303A
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Abstract
The invention discloses a kind of compound biomass carbon materials and its preparation and the application in lithium selenium cell coated separator, belong to electrochemical energy storage technical field.At room temperature, biological material is immersed in Ni-acetate solution, it is freeze-dried to obtain composite biomass carbon materials material precursor；Then composite biomass material precursor is carbonized in tube furnace, obtained product carries out obtaining compound biomass carbon material after washing is dry.This composite material is applied in the diaphragm modification of lithium selenium cell, shuttle of more selenides between battery plus-negative plate can be effectively inhibited, makes battery that there is higher actual specific capacity, improves the coulombic efficiency and cycle performance of battery.
Description
Technical field
The invention belongs to lithium selenium cell technical field, in particular to a kind of compound biomass carbon material and its preparation and
Application in lithium selenium cell coated separator, the especially application in lithium selenium cell diagram modification.
Background technique
With the prosperity and development of global economy, the gradually quickening of process of industrialization, the energy problem that 21st century faces
Also increasingly severe, the exploitation of novel renewable energy has been very urgent, while environmental problem has become the whole mankind and faces
Challenge, seek the common recognition that novel green energy storage means early have become the whole mankind.Between past more than two decades, lithium ion battery is ground
Study carefully and obtain immense success with industrialization, the extensive use of lithium ion battery changes energy market ecology.
Due to the limitation of conventional lithium ion battery theoretical specific capacity, the matter to battery such as electric car, portable intelligent equipment
To measure specific capacity and volume and capacity ratio more stringent requirements are proposed, and researchers urgently find more height ratio capacity, high-energy density
Battery system.Lithium selenium cell is a kind of energy storage device that the work of polyelectron principle of oxidation and reduction occurs based on selenium and lithium, reason
It is 678mAh/g, theoretical volumetric capacity 3254mAh/cm by specific discharge capacity3, thus be considered as a kind of promising height
Specific energy secondary cell system.However, volume change in the anode there are active material utilizations low, charge and discharge process
Greatly, cyclical stability be deteriorated, coulombic efficiency it is low from and electronic conductivity and ion transportation it is relatively low the problems such as, these are asked
Topic has seriously affected the chemical property of lithium selenium cell.
As market puts forward higher requirements energy storage, attention of the secondary lithium selenium cell by researchers, 2012
Year Ali Abouimrane and Khalil Amine seminar is published in the research paper on J.Am.Chem.Soc. and reports for the first time
Under room temperature elemental selenium as a positive electrode active material the application in serondary lithium battery and sode cell system (J.Am.Chem.Soc.,
2012,134,4505-4508).Hereafter, lithium selenium cell causes the interest of researchers, and relevant research is successively on periodical
Report.Therefore lithium selenium cell becomes concerned high-energy density secondary battery system.For lithium selenium cell chemical property
It is promoted, using the conducting matrix grain of biomass carbon material, the abundant advantages such as hole and high-specific surface area, as lithium selenium cell material
The carrier of material, oneself is considered as a kind of effective scheme for improving lithium selenium cell chemical property.Using the life of low cost, source green
Substance replace traditional chemical reagent as carbon source and screen simple technique can be effectively reduced preparation cost, expansion biomass
The application potential of base carbon material meets environmental-friendly theory.
Summary of the invention
The purpose of the present invention is to provide a kind of compound biomass carbon material preparation methods, it is intended to provide a kind of with rich
Rich hole, high-specific surface area, satisfactory electrical conductivity composite biomass carbon material.
The present invention also provides the compound biomass carbon materials described in one kind in lithium selenium cell diagram modification field
Using passing through modification of the composite biomass carbon material to diaphragm synthesized with the infusion process, freeze-drying, improve lithium selenium
The cycle performance of battery.Diaphragm after modification is able to suppress the shuttle effect of the more selenides of lithium selenium cell, has lithium selenium cell
Higher specific discharge capacity, and the coulombic efficiency of battery can be improved, to improve the whole chemical property of battery.
The present invention will be realized using following technical scheme:
A kind of composite biomass carbon material, it is characterised in that: using the biomass after Ni-acetate solution impregnation, then
Freeze-dried, high-temperature calcination obtains composite biomass carbon material.
The biomass is one or more of radish, wax gourd, mushroom or Pleurotus eryngii.
The preparation method of the composite biomass carbon material, comprising the following steps:
Biomass: being cleaned and is removed surface impurity by step (1), and chopping obtains uniform block A；
Step (2): uniform block A is added in Ni-acetate solution, and blocky B is obtained by filtration in immersion；
Step (3): block B is freeze-dried, and the product obtained after dry is ground, and moves to tubular type atmosphere
In furnace, carries out high-temperature calcination and be carbonized to obtain carbonized product C；
Step (4): carbonized product C is washed, dry, and composite biomass carbon material is obtained after grinding.
Wherein,
Homogeneous bulky object A in step (1), diameter are 0.5cm~1.5cm；
The concentration of Ni-acetate solution is 0.5mol/L~1mol/L in step (2)；
The temperature being freeze-dried in step (3) is -75 DEG C~-20 DEG C, and the time is 15h~42h, and high-temperature calcination temperature is
850 DEG C~900 DEG C, the reaction time is 2h~6h；
Carbonized product C milling time is 30min~50min in step (4)；Drying temperature is 60 DEG C~110 DEG C.
A kind of lithium selenium cell diaphragm, comprising: base layer and the modified coatings coated on base layer side, the modified coatings
Composite biomass carbon material more than including.
The base layer is membrane for polymer, and membrane for polymer is polypropylene diaphragm, polyethylene diagrams, polypropylene/poly-
One or more of ethylene/polypropylene three-layer coating or nonwoven cloth diaphragm, membrane for polymer is with a thickness of 16 μm~30 μm；
Modified coatings comprising composite biomass carbon material are with a thickness of 18 μm~40 μm.
A kind of preparation method of lithium selenium cell diaphragm, which is characterized in that composite biomass carbon material is prepared into compound life
Composite biomass carbon material slurry is coated on side and the drying of base layer by substance carbon material slurry, uniform in membrane surface
Form modified coatings；Modified coatings with a thickness of 2 μm~10 μm.
Composite biomass carbon material is mixed with conductive agent Super P and binder 7~8:1 in mass ratio~2:1, is added
Solvent；It obtains that slurry is coated in membrane surface after uniformly mixed slurry after ball milling, it is dry；
The solvent is one of water, ethyl alcohol, ethylene glycol or methyl pyrrolidone solvent or a variety of；
The binder is Kynoar, completes one of sodium carboxymethylcellulose pyce or butadiene-styrene latex or a variety of；
It is described to be applied to dipping film, spin-coating, scraper film, curtain coating film, simple tension or bidirectional extending method
In any one；
It is that 6h~for 24 hours is dried in vacuo in 40 DEG C~60 DEG C environment that the drying, which is in temperature,.
A kind of application of lithium selenium cell diaphragm, the diaphragm are used for electrochemical energy storage field.Again when assembled battery, battery
Modified coatings side in diaphragm is close to cell positive material.
Beneficial effects of the present invention are as follows:
1, the raw material sources used in the present invention are extensive, and low in cost, stable process conditions are reliable, entire process flow letter
It is single easy, it is suitble to large-scale industrial production.
2, the present invention selects biomass as main study subject.The large specific surface area of biomass carbon is applied to lithium selenium electricity
On the diaphragm of pond, the carbon barrier layer with multiple cavernous structure is formed, adsorbable battery makes in the more lithium selenides of reduzate of electric discharge
The active material of battery is maximally utilized.
3, the lithium selenium cell assembles battery using coated separator, can significantly improve the actual capacity of battery, and circulation is surely
It is qualitative, so that the whole chemical property of battery is had biggish promotion.
Detailed description of the invention
Fig. 1 is lithium selenium cell structural schematic diagram of the present invention；
Fig. 2 is biomass carbon material electron microscope obtained in comparative example 1 of the present invention；
Fig. 3 is composite biomass carbon material electron microscope obtained in comparative example 2 of the present invention；
Fig. 4 is the circulation contrast properties figure of the button cell of assembling of the embodiment of the present invention.
Specific embodiment
In order to make the objectives, technical solutions and advantages of the present invention clearer, combined with specific embodiments below further
Illustrate technical solution of the present invention, these descriptions are merely illustrative, these embodiments are not to be construed as to technical solution
Limitation.
Embodiment 1
260g biomass radish is taken, the homogeneous bulky that diameter is 1cm is cut into, is immersed in the second that concentration is 0.5mol/L
In sour nickel solution, soaking time for 24 hours, by it in -70 DEG C of freeze-drying 12h after filtering, by the biological material after drying in pipe
850 DEG C of carbonization 2h, obtained black powder use deionized water and washes of absolute alcohol three times respectively in formula furnace, and centrifugation drying is ground
30min is ground, composite biomass carbon material is obtained, by obtained composite biomass carbon material and adhesive Kynoar PVDF,
Conductive agent Super P continues grinding until being sufficiently mixed according to mass ratio 8:1:1, and mixed-powder is placed in ball grinder, is added dropwise
Ball grinder is placed on ball milling 2h on planetary ball mill, then the material of ball milling is starched by 2mL N methyl pyrrolidone NMP
Material is applied to 40 DEG C of the side drying of diaphragm with film pulling device, forms the modified coatings with a thickness of 3 μm, and base layer is poly- the third of 20 μm
Alkene polymer layer is punched into the disk that diameter is 16mm to which modified diaphragm be made.
After composite biomass carbon material and selenium powder in mass ratio 4:6 ground and mixed, under conditions of 260 DEG C of closed container
It is heat-treated 12h, the composite material that will be obtained, with adhesive PVDF, conductive agent Super P is uniformly mixed according to mass ratio 7:2:1,
Dropwise addition 2mL NMP is ground to thick be coated uniformly on aluminium foil and is dried to obtain battery pole piece, is then punched into battery pole piece
Diameter is the disk of 12mm.
Using above-mentioned pole piece and modified diaphragm, by modified coatings side in the diaphragm after modification close to cell positive material,
2016 type button cells are assembled into inertia glove box, metal lithium sheet is to electrode, and the electrolyte of use is molten by LiTFSI
Solution is made in the mixed solution of DOL and DME, in electrolyte the concentration of LiTFSI be 1mol/L (in electrolyte, the body of DOL and DME
Product is than being 1:1, and LiTFSI is bis trifluoromethyl sulfonic acid imide li, and DOL is 1,3-dioxolane, and DME is glycol dinitrate
Ether), the battery being assembled into carries out correlated performance test with Wuhan indigo plant electrical measurement test system CT2001A.
Comparative example 1
260g biomass radish is taken, the homogeneous bulky that diameter is 1cm is cut into, by it in -70 DEG C of freeze-drying 12h,
By the biological material after drying, 850 DEG C of carbonization 2h, obtained black powder use deionized water and anhydrous respectively in tube furnace
Ethyl alcohol cleans three times, and 30min is ground in centrifugation drying, obtains common biomass carbon material (Fig. 2 is radish biomass electron microscope).
After common biomass carbon material and selenium powder 4:6 ground and mixed in mass ratio, under conditions of 260 DEG C of closed container
It is heat-treated 12h, the C/Se material that will be obtained, with adhesive PVDF, conductive agent Super P is uniformly mixed according to mass ratio 7:2:1,
Dropwise addition 2mL NMP is ground to thick be coated uniformly on aluminium foil and is dried to obtain battery pole piece, is then punched into battery pole piece
Diameter is the disk of 12mm, and the load capacity of selenium is 0.8mg/cm2。
Using above-mentioned pole piece and common diaphragm (celgard 2400), 2016 type button electricity are assembled into inertia glove box
Pond, metal lithium sheet are to electrode, and the electrolyte of use is made of the mixed solution that LiTFSI is dissolved in DOL and DME, electrolyte
The concentration of middle LiTFSI is that (in electrolyte, the volume ratio of DOL and DME are 1:1 to 1mol/L, and LiTFSI is bis trifluoromethyl sulfonic acid
Imide li, DOL are 1,3-dioxolane, and DME is glycol dimethyl ether), the battery being assembled into Wuhan indigo plant electrical measurement test system
CT2001A carries out correlated performance test.
Comparative example 2
260g biomass radish is taken, the homogeneous bulky that diameter is 1cm is cut into, is immersed in the second that concentration is 0.5mol/L
In sour nickel solution, soaking time for 24 hours, by its subzero 70 DEG C of freeze-dryings 12h after filtering, by the biological material after drying in pipe
850 DEG C of carbonization 2h, obtained black powder use deionized water and washes of absolute alcohol three times respectively in formula furnace, and centrifugation drying is ground
30min is ground, composite biomass carbon material is obtained, (Fig. 3 is composite biomass carbon material Electronic Speculum to obtained composite biomass carbon material
Figure).
After composite biomass carbon material and selenium powder in mass ratio 4:6 ground and mixed, under conditions of 260 DEG C of closed container
It is heat-treated 12h, the composite material that will be obtained, with adhesive PVDF, conductive agent Super P is uniformly mixed according to mass ratio 7:2:1,
Dropwise addition 2mL NMP is ground to thick be coated uniformly on aluminium foil and is dried to obtain battery pole piece, is then punched into battery pole piece
Diameter is the disk of 12mm.
Using above-mentioned pole piece and common diaphragm (celgard 2400), 2016 type button electricity are assembled into inertia glove box
Pond, metal lithium sheet are to electrode, and the electrolyte of use is made of the mixed solution that LiTFSI is dissolved in DOL and DME, electrolyte
The concentration of middle LiTFSI is that (in electrolyte, the volume ratio of DOL and DME are 1:1 to 1mol/L, and LiTFSI is bis trifluoromethyl sulfonic acid
Imide li, DOL are 1,3-dioxolane, and DME is glycol dimethyl ether), the battery being assembled into Wuhan indigo plant electrical measurement test system
CT2001A carries out correlated performance test.
Fig. 4 is charge and discharge cycles figure of the button cell of assembling under 0.5C multiplying power, statistics indicate that, the compound bio used
Modified diaphragm is not used in matter carbon material, and under 0.5C discharge-rate, initial discharge specific capacity is 570mAh/g, after circulation 100 is enclosed
For 270mAh/g.Although shuttle effect can be inhibited to a certain extent, promote lithium selenium cell capacity, assembled not as good as modified diaphragm
Lithium selenium cell.Using the battery of modified diaphragm under 0.5C discharge-rate, initial discharge specific capacity is 658mAh/g, circulation 100
It is 419mAh/g after circle.The reason is that composite biomass modified diaphragm can exist in the more plasma seleniums for being partially disengaged conductive estimation
It is intercepted before diaphragm, the more selenides during which captured are secondary use, to promote the cycle performance of lithium selenium cell.
Technical solution of the present invention is not limited to examples detailed above, and the other embodiments obtained according to the technique and scheme of the present invention are equal
It should fall into claim of the invention.
Claims (10)
1. a kind of composite biomass carbon material, it is characterised in that: using the biomass after Ni-acetate solution impregnation, passed through after
Freeze-drying, high-temperature calcination obtain composite biomass carbon material.
2. according to claim 1 meet biological material, which is characterized in that the biomass is radish, wax gourd, mushroom
Or one or more of Pleurotus eryngii.
3. preparing the preparation method of composite biomass carbon material described in claim 1, which comprises the following steps:
Biomass: being cleaned and is removed surface impurity by step (1), and chopping obtains uniform block A；
Step (2): uniform block A is added in Ni-acetate solution, and blocky B is obtained by filtration in immersion；
Step (3): block B is freeze-dried, and the product obtained after dry is ground, and moves to tube-type atmosphere furnace
In, it carries out high-temperature calcination and is carbonized to obtain carbonized product C；
Step (4): carbonized product C is washed, dry, and composite biomass carbon material is obtained after grinding.
4. a kind of composite biomass carbon materials preparation method for material according to claim 3, which is characterized in that in step (1)
Even block A, diameter are 0.5cm~1.5cm；
The concentration of Ni-acetate solution is 0.5mol/L~1mol/L in step (2)；
The temperature being freeze-dried in step (3) is -75 DEG C~-20 DEG C, and drying time is 12h~42h, and high-temperature calcination temperature is
850 DEG C~900 DEG C, the reaction time is 2h~6h；
Carbonized product C milling time is 30min~50min in step (4)；Drying temperature is 60 DEG C~110 DEG C.
5. a kind of lithium selenium cell diaphragm characterized by comprising base layer and the modified coatings coated on base layer side, institute
Stating modified coatings includes composite biomass carbon material of any of claims 1 or 2.
6. lithium selenium cell diaphragm according to claim 5, which is characterized in that the base layer is membrane for polymer, is gathered
Conjunction object diaphragm is in polypropylene diaphragm, polyethylene diagrams, polypropylene, polyethylene/polypropylene three-layer coating or nonwoven cloth diaphragm
One or more, membrane for polymer is with a thickness of 16 μm~30 μm.
7. a kind of preparation method of lithium selenium cell diaphragm described in claim 5 or 6, which is characterized in that by composite biomass carbon
Material is prepared into composite biomass carbon material slurry, and composite biomass carbon material slurry is coated on the side of base layer and is done
It is dry, modified coatings are formed uniformly in membrane surface；Modified coatings with a thickness of 2 μm~10 μm.
8. the preparation method of lithium selenium cell diaphragm according to claim 7, which is characterized in that composite biomass carbon material with
Conductive agent Super P and binder 7~8:1 in mass ratio~2:1 mixing, adds solvent；It is obtained after ball milling uniformly mixed
Slurry is coated in membrane surface after slurry, it is dry；
The solvent is one of water, ethyl alcohol, ethylene glycol or methyl pyrrolidone solvent or a variety of；
The binder is Kynoar, completes one of sodium carboxymethylcellulose pyce or butadiene-styrene latex or a variety of；
It is described to be applied in dipping film, spin-coating, scraper film, curtain coating film, simple tension or bidirectional extending method
Any one；
It is that 6h~for 24 hours is dried in vacuo in 40 DEG C~60 DEG C environment that the drying, which is in temperature,.
9. a kind of application of lithium selenium cell diaphragm described in claim 5 or 6, it is characterised in that: the diaphragm is for electrification
Learn energy storage field.
10. the application of lithium selenium cell diaphragm according to claim 9, it is characterised in that: when assembled battery, in battery diaphragm
Modified coatings side close to cell positive material.
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| CN110416479A (en) * | 2019-07-31 | 2019-11-05 | 东华大学 | A kind of multichannel carbide wood interlayer and its preparation and application with orientation |
| CN112688024A (en) * | 2020-12-31 | 2021-04-20 | 界首市天鸿新材料股份有限公司 | Diaphragm material of power lithium battery |
| CN113247867A (en) * | 2020-02-07 | 2021-08-13 | Ii-Vi特拉华有限公司 | Immobilized selenium in porous carbon in the presence of oxygen, method for preparing immobilized selenium and use in rechargeable batteries |
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Application publication date: 20190503 |