CN102931437A - Production method of foamed nickel growth based lithium ion battery with graphene serving as negative pole - Google Patents
Production method of foamed nickel growth based lithium ion battery with graphene serving as negative pole Download PDFInfo
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- CN102931437A CN102931437A CN2012104474402A CN201210447440A CN102931437A CN 102931437 A CN102931437 A CN 102931437A CN 2012104474402 A CN2012104474402 A CN 2012104474402A CN 201210447440 A CN201210447440 A CN 201210447440A CN 102931437 A CN102931437 A CN 102931437A
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Abstract
The invention discloses a production method of a foamed nickel growth based lithium ion battery with graphene serving as a negative pole. In the current, silicon substrate, titanium substrate, tin substrate and transition metal metallic oxide serves as negative poles of lithium ion batteries, and the problems that cycling stability is poor and serious volume effects appear during lithium intercalating and removing exist. A chemical vapor deposition technology is used firstly, multiple layers of graphene grows on the foamed nickel, the graphene is punched into a circular negative thin sheet in a certain size through a sheet-punching machine, a supporting body, the circular negative pole thin sheet, a membrane, a circular positive pole thin sheet and a supporting body are placed inside a battery casing sequentially, the battery casing and a cover are pressed by a sheet-pressing machine, and the production process of the lithium ion battery is completed. The batter is mature in process, easy to produce, high in battery energy intensity, capable of achieving the charge and discharge performance and the service life and easy to popularize and utilize industrially.
Description
Technical field
The invention belongs to technical field of new energies, the main description utilized grow multi-layer graphene and be prepared into that energy storage density height, charge-discharge performance are excellent, the process of the lithium ion battery that has extended cycle life of nickel foam in chemical vapor deposition unit.
Background technology
Lithium ion battery is a kind of rechargeable battery, and it mainly relies on lithium ion to move work between positive pole and negative pole.Traditionally, lithium ion enters the process of positive electrode embedding, and the process of leaving is taking off embedding; Lithium ion enters the process of negative material inserting, and the process of leaving is slotting taking off.
The operating voltage of monomer lithium ion battery is 3.2V up to 3.7～3.8V(LiFePO4), Ni-Cd, Ni-H battery 3 times, the actual specific energy that can reach at present is about 555Wh/kg, be that material can reach the above specific capacity of 150mAh/g (3～4 times to Ni-Cd, 2～3 times to Ni-MH), close to about 88% of its theoretical value.General lithium ion battery discharges and recharges all and can reach more than 500 times, even more than 1000 times, can the reaching more than 2000 times of LiFePO4, and for the electrical equipment of low discharging current, the useful life of battery is with the competitiveness of times Electronating device.The self-discharge rate of lithium ion battery storage after 1 month that is full of electricity under the room temperature is about 2%, is significantly less than 25～30% of Ni-Cd, 30～35% of Ni, MH.Lithium ion battery 1C 30 minute volumes that charge can reach more than 80% of nominal capacity, and the ferrophosphorus battery can reach 10 minutes and is charged to 90% of nominal capacity now.The effect of its septation is isolation battery core positive and negative plate, to prevent that rolling up the direct contact of core inner positive and negative plate causes short circuit; From microcosmic angle, membrane surface is network structure, and usually arranged dividing of PP, PE, also has PE, PP to be combined with each other.
For the lithium ion battery of material with carbon element as negative pole, when battery is charged, there is lithium ion to generate on the positive pole of battery, the lithium ion of generation arrives negative pole through electrolyte movement.And be layer structure as the carbon of negative pole, and it has a lot of micropores, and the lithium ion that reaches negative pole just is embedded in the micropore of carbon-coating, and the lithium ion of embedding is more, and charging capacity is higher.Equally, when battery is discharged (we use the process of battery), the lithium ion that is embedded in the negative pole carbon-coating is deviate from, and it is anodal to move back again.It is more to return anodal lithium ion, and discharge capacity is higher.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, it is the lithium ion battery manufacture method of negative pole that a kind of Graphene based on the nickel foam growth is provided.
Manufacture method of the present invention may further comprise the steps:
Step 1: nickel foam is distinguished ultrasonic cleaning 10～40 minutes successively in deionized water, acetone and ethanol.
Step 2: utilize high pure nitrogen with nickel foam dry up and drying left standstill 5～10 minutes, nickel foam is put into the CVD device, utilize high-power vacuum pump with the vacuum degree control in the reaction chamber at 2～3mTorr.
Step 3: pass into the hydrogen of 5～35sccm as reducibility gas, the control reacting furnace was increased to 800～1100 ℃ in 50 minutes.
Step 4: keep CVD device hot operation 40～140 minutes, and in reaction chamber, pass into the methane of 50～250sccm as carbon-source gas.
Step 5: the control reacting furnace was down to normal temperature in 5～10 minutes, take out the nickel foam of the multi-layer graphene of having grown.
Step 6: will having grown with sheet-punching machine, to be die-cut into diameter be that 10～15 millimeters, thickness are 10～20 microns thin rounded flakes for the nickel foam of multi-layer graphene, as the negative pole of lithium ion battery.
Step 7: battery case is lain in a horizontal plane in the glove box that is full of argon gas, with the nickel foam thin rounded flakes of supporter and the step 6 successively stable battery case inside that is placed on, and evenly drip the il electrolyte of 0.1～0.5ml at sheet surface, so that thin slice and support physical efficiency and the complete applying of battery case energy.
Step 8: will be of a size of the surface that 15～20 millimeters lithium ion battery separator is placed on the nickel foam thin slice, and notice that barrier film can not contact with battery case.
Step 9: the il electrolyte of dripping 0.1～0.5ml at the lithium ion battery separator surface uniform, be that 10～15 millimeters, thickness are that 20～200 microns circular positive wafer thin is placed on membrane surface with diameter, and place another supporter on positive wafer thin, use il electrolyte that battery case inside is full of and the block of the battery case that closes, utilize tablet press machine pressing lithium ion battery to finish manufacturing process.
In the such scheme, the described battery case of step 7 and step 9 is Al alloy shell, nickel plating iron-clad or aluminum plastic film, supporter is the inert conductors such as foam gold, foam platinum or nickel foam, and il electrolyte is for being dissolved in the lithium perchlorate (LiClO in the ethylene carbonate (EC)
4), lithium hexafluoro phosphate (LiPF
6) or LiBF4 (LiBF
4); The described lithium ion battery separator of step 8 and step 9 is polyethylene film, polypropylene screen, polyvinylidene fluoride film or cellulose composite membrane; The described lithium ion cell positive thin slice of step 9 is LiMn2O4 sheet, cobalt acid lithium sheet, LiFePO4 sheet or nickle cobalt lithium manganate sheet.
Beneficial effect of the present invention: the Graphene based on the nickel foam growth provided by the invention is the lithium ion battery of negative pole, technical maturity is made simply, and energy content of battery density is high, can realize the remarkable lifting of charge-discharge performance and cycle life, be easy to industry and promote the use of.
Description of drawings
Fig. 1 is the SEM image of the multi-layer graphene take nickel foam as substrate grown.
Fig. 2 is the Raman collection of illustrative plates of the multi-layer graphene take nickel foam as substrate grown.
Fig. 3 is the lithium ion battery structure schematic diagram of negative pole for the Graphene based on the nickel foam growth.
Fig. 4 is capacity and the energy conversion efficiency result schematic diagram of lithium ion battery under the different cycle-indexes.
Fig. 5 is the charging and discharging curve of the 1st～4 circulation of lithium ion battery.
Fig. 6 is the charging and discharging curve of lithium ion battery the 4th, the 25th time, the 50th time, the 75th time and the 100th time circulation.
Embodiment
The invention will be further described below in conjunction with accompanying drawing.
Embodiment 1:
At first nickel foam is distinguished ultrasonic cleaning 30 minutes successively in deionized water, acetone and ethanol, and drying left standstill 5 minutes to utilize high pure nitrogen to dry up nickel foam also; Then nickel foam is put into the CVD device, utilize high-power vacuum pump with the vacuum degree control in the reaction chamber about 3mTorr, pass into the hydrogen of 15sccm as reducibility gas, the control reacting furnace was increased to 1000 ℃ in 50 minutes, keep CVD device hot operation 60 minutes, and in reaction chamber, pass into the methane of 150sccm as carbon-source gas; Then control reacting furnace and be down to normal temperature in 10 minutes, taking out the nickel foam of the multi-layer graphene of having grown and with sheet-punching machine it being die-cut into diameter is that 10 millimeters, thickness are 15 microns thin rounded flakes 4, as the negative pole of lithium ion battery; Secondly aluminum alloy battery shell 7 is lain in a horizontal plane in the glove box that is full of argon gas, be successively stable aluminum alloy battery shell 7 inside that are placed on of 10 millimeters circular foam platinum supporter 5 and circular negative pole thin slice 4 with diameter, and drip the lithium hexafluorophosphate electrolyte solution 6 of 0.2ml at circular negative pole thin slice 4 surface uniforms, the polyethylene barrier film 3 that is of a size of 15 millimeters is placed on the surface of circular negative pole thin slice 4, keeps barrier film not contact with battery case; Drip at last the lithium hexafluorophosphate electrolyte solution 6 of 0.2ml at polyethylene barrier film 3 surface uniforms, be that 10 millimeters, thickness are that 100 microns circular LiMn2O4 thin slice 2 is placed on polyethylene barrier film 3 surfaces with diameter, and place another foam platinum supporter 1 on circular LiMn2O4 thin slice, use lithium hexafluorophosphate electrolyte solution 6 that battery case 7 inside are full of and the block of the battery case that closes, utilize tablet press machine pressing lithium ion battery to finish manufacturing process.Wherein, grown multi-layer graphene the local SEM figure of nickel foam as shown in Figure 1; The Raman collection of illustrative plates of multi-layer graphene as shown in Figure 2; The lithium ion battery structure schematic diagram as shown in Figure 3; Under the different cycle-indexes capacity of lithium ion battery and energy conversion efficiency result schematic diagram as shown in Figure 4, capacity of lithium ion battery can reach 1000mAh/g, 100 times circulation self-energy conversion efficiency can reach 98%; The charging and discharging curve of lithium ion battery the 1st～4 time circulation as shown in Figure 5, the charging and discharging curve repeatability is very good, and the cycle charging excellent performance of lithium ion battery is described; The charging and discharging curve of lithium ion battery the 4th, the 25th time, the 50th time, the 75th time and the 100th circulation as shown in Figure 6, the curve that discharges and recharges for the 100th time is almost consistent with the 4th charging and discharging curve, and lithium ion battery stability excellence be described.
Embodiment 2:
At first nickel foam is distinguished ultrasonic cleaning 10 minutes successively in deionized water, acetone and ethanol, and drying left standstill 5 minutes to utilize high pure nitrogen to dry up nickel foam also; Then nickel foam is put into the CVD device, utilize high-power vacuum pump with the vacuum degree control in the reaction chamber about 2mTorr, pass into the hydrogen of 5sccm as reducibility gas, the control reacting furnace was increased to 800 ℃ in 50 minutes, keep CVD device hot operation 40 minutes, and in reaction chamber, pass into the methane of 50sccm as carbon-source gas; Then control reacting furnace and be down to normal temperature in 5 minutes, taking out the nickel foam of the multi-layer graphene of having grown and with sheet-punching machine it being die-cut into diameter is that 10 millimeters, thickness are 10 microns thin rounded flakes 4, as the negative pole of lithium ion battery; Secondly nickel-clad iron battery case 7 is lain in a horizontal plane in the glove box that is full of argon gas, be successively stable nickel-clad iron battery case 7 inside that are placed on of 10 millimeters circular nickel foam supporter 5 and circular negative pole thin slice 4 with diameter, and drip the lithium perchlorate electrolyte 6 of 0.1ml at circular negative pole thin slice 4 surface uniforms, the polypropylene diaphragm 3 that is of a size of 15 millimeters is placed on the surface of circular negative pole thin slice 4, keeps barrier film not contact with battery case; Drip at last the lithium perchlorate electrolyte 6 of 0.1ml at polypropylene diaphragm 3 surface uniforms, be that 15 millimeters, thickness are that 20 microns circular cobalt acid lithium thin slice 2 is placed on polypropylene diaphragm 3 surfaces with diameter, and place another nickel foam supporter 1 on circular cobalt acid lithium thin slice, use lithium perchlorate electrolyte 6 that battery case 7 inside are full of and the block of the battery case that closes, utilize tablet press machine pressing lithium ion battery to finish manufacturing process.
Embodiment 3:
At first nickel foam is distinguished ultrasonic cleaning 40 minutes successively in deionized water, acetone and ethanol, and drying left standstill 10 minutes to utilize high pure nitrogen to dry up nickel foam also; Then nickel foam is put into the CVD device, utilize high-power vacuum pump with the vacuum degree control in the reaction chamber about 2mTorr, pass into the hydrogen of 35sccm as reducibility gas, the control reacting furnace was increased to 1100 ℃ in 50 minutes, keep CVD device hot operation 140 minutes, and in reaction chamber, pass into the methane of 250sccm as carbon-source gas; Then control reacting furnace and be down to normal temperature in 10 minutes, taking out the nickel foam of the multi-layer graphene of having grown and with sheet-punching machine it being die-cut into diameter is that 15 millimeters, thickness are 20 microns thin rounded flakes 4, as the negative pole of lithium ion battery; Secondly plastic-aluminum battery case 7 is lain in a horizontal plane in the glove box that is full of argon gas, be successively stable plastic-aluminum battery case 7 inside that are placed on of 15 millimeters circular foam gold supporter 5 and circular negative pole thin slice 4 with diameter, and drip the LiBF4 electrolyte 6 of 0.5ml at circular negative pole thin slice 4 surface uniforms, the Kynoar barrier film 3 that is of a size of 20 millimeters is placed on the surface of circular negative pole thin slice 4, keeps barrier film not contact with battery case; Drip at last the LiBF4 electrolyte 6 of 0.5ml at polyethylene barrier film 3 surface uniforms, be that 15 millimeters, thickness are that 200 microns circular nickle cobalt lithium manganate thin slice 2 is placed on Kynoar barrier film 3 surfaces with diameter, and place another foam gold supporter 1 on circular LiMn2O4 thin slice, use LiBF4 electrolyte 6 that battery case 7 inside are full of and the block of the battery case that closes, utilize tablet press machine pressing lithium ion battery to finish manufacturing process.
Embodiment 4:
At first nickel foam is distinguished ultrasonic cleaning 30 minutes successively in deionized water, acetone and ethanol, and drying left standstill 5 minutes to utilize high pure nitrogen to dry up nickel foam also; Then nickel foam is put into the CVD device, utilize high-power vacuum pump with the vacuum degree control in the reaction chamber about 3mTorr, pass into the hydrogen of 25sccm as reducibility gas, the control reacting furnace was increased to 1035 ℃ in 50 minutes, keep CVD device hot operation 90 minutes, and in reaction chamber, pass into the methane of 120sccm as carbon-source gas; Then control reacting furnace and be down to normal temperature in 10 minutes, taking out the nickel foam of the multi-layer graphene of having grown and with sheet-punching machine it being die-cut into diameter is that 10 millimeters, thickness are 15 microns thin rounded flakes 4, as the negative pole of lithium ion battery; Secondly aluminum alloy battery shell 7 is lain in a horizontal plane in the glove box that is full of argon gas, be successively stable aluminum alloy battery shell 7 inside that are placed on of 10 millimeters circular nickel foam supporter 5 and circular negative pole thin slice 4 with diameter, and drip the lithium perchlorate electrolyte 6 of 0.3ml at circular negative pole thin slice 4 surface uniforms, the cellulose composite diaphragm 3 that is of a size of 15 millimeters is placed on the surface of circular negative pole thin slice 4, keeps barrier film not contact with battery case; Drip at last the lithium perchlorate electrolyte 6 of 0.2ml at polyethylene barrier film 3 surface uniforms, be that 10 millimeters, thickness are that 100 microns circular LiFePO4 thin slice 2 is placed on polyethylene barrier film 3 surfaces with diameter, and place another nickel foam supporter 1 on circular LiFePO4 thin slice, use lithium perchlorate electrolyte 6 that battery case 7 inside are full of and the block of the battery case that closes, utilize tablet press machine pressing lithium ion battery to finish manufacturing process.
Claims (6)
1. the Graphene based on the nickel foam growth is the lithium ion battery manufacture method of negative pole, it is characterized in that the method may further comprise the steps:
Step 1: nickel foam is distinguished ultrasonic cleaning 10～40 minutes successively in deionized water, acetone and ethanol;
Step 2: utilize high pure nitrogen with nickel foam dry up and drying left standstill 5～10 minutes, nickel foam is put into the CVD device, utilize high-power vacuum pump with the vacuum degree control in the reaction chamber at 2～3mTorr;
Step 3: pass into the hydrogen of 5～35sccm as reducibility gas, the control reacting furnace was increased to 800～1100 ℃ in 50 minutes;
Step 4: keep CVD device hot operation 40～140 minutes, and in reaction chamber, pass into the methane of 50～250sccm as carbon-source gas;
Step 5: the control reacting furnace was down to normal temperature in 5～10 minutes, take out the nickel foam of the multi-layer graphene of having grown;
Step 6: will having grown with sheet-punching machine, to be die-cut into diameter be that 10～15 millimeters, thickness are 10～20 microns thin rounded flakes for the nickel foam of multi-layer graphene, as the negative pole of lithium ion battery;
Step 7: battery case is lain in a horizontal plane in the glove box that is full of argon gas, with the nickel foam thin rounded flakes of supporter and the step 6 successively stable battery case inside that is placed on, and evenly drip the il electrolyte of 0.1～0.5ml at sheet surface, so that thin slice and support physical efficiency and the complete applying of battery case;
Step 8: will be of a size of the surface that 15～20 millimeters lithium ion battery separator is placed on the nickel foam thin slice, and keep barrier film not contact with battery case;
Step 9: the il electrolyte of dripping 0.1～0.5ml at the lithium ion battery separator surface uniform, be that 10～15 millimeters, thickness are that 20～200 microns circular positive wafer thin is placed on membrane surface with diameter, and place another supporter on positive wafer thin, use il electrolyte that battery case inside is full of and the block of the battery case that closes, utilize tablet press machine pressing lithium ion battery, finish manufacturing process.
2. lithium ion battery manufacturing process according to claim 1, it is characterized in that: described battery case is Al alloy shell, nickel plating iron-clad or aluminum plastic film.
3. lithium ion battery manufacturing process according to claim 1 is characterized in that: described supporter is foam gold, foam platinum or nickel foam.
4. lithium ion battery manufacturing process according to claim 1, it is characterized in that: described il electrolyte is lithium perchlorate, lithium hexafluoro phosphate or the LiBF4 that is dissolved in the ethylene carbonate.
5. lithium ion battery manufacturing process according to claim 1, it is characterized in that: described lithium ion battery separator is polyethylene film, polypropylene screen, polyvinylidene fluoride film or cellulose composite membrane.
6. lithium ion battery manufacturing process according to claim 1 is characterized in that: described lithium ion cell positive thin slice is LiMn2O4 sheet, cobalt acid lithium sheet, LiFePO4 sheet or nickle cobalt lithium manganate sheet.
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| CN103794793A (en) * | 2014-01-22 | 2014-05-14 | 东莞市万丰纳米材料有限公司 | Positive and negative material for preparing lithium battery from continuous-phase spongy graphene as well as preparation method of material |
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| CN110752373A (en) * | 2019-10-28 | 2020-02-04 | 北京科技大学 | High-performance liquid metal battery negative current collector and preparation method thereof |
| CN110752373B (en) * | 2019-10-28 | 2021-06-15 | 北京科技大学 | High-performance liquid metal battery negative current collector and preparation method thereof |
| CN111604072A (en) * | 2020-05-15 | 2020-09-01 | 桂林电子科技大学 | Nano particle-graphene-foam nickel composite material with bionic structure and preparation method thereof |
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