CN104409728A - Method for preparing tin-carbon anode/lithium iron phosphate cathode lithium ion battery based on 3D printing technology - Google Patents
Method for preparing tin-carbon anode/lithium iron phosphate cathode lithium ion battery based on 3D printing technology Download PDFInfo
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Abstract
The invention relates to a method for preparing a tin-carbon anode/lithium iron phosphate cathode lithium ion battery based on a 3D printing technology. The method mainly contains the following steps: a tin-carbon nanomaterial and lithium iron phosphate are respectively dissolved in respective solutions to prepare each electrode printing ink; and then, by a 3D printing technology, an electrode structure is printed by using the tin-carbon material as an anode and the lithium iron phosphate as a cathode; and finally, the prepared electrode is transferred to a glove box filled with argon so as to complete packaging of the 3D combined electrode lithium ion battery. The method for preparing the tin-carbon anode/lithium iron phosphate cathode lithium ion battery mainly based on the 3D printing technology has characteristics of novel preparation method and simple technology. The prepared electrode material has advantages of large specific surface area, high energy density, good conductivity and the like. The method provided by the invention has a huge application potential in the field of high-performance lithium ion batteries.
Description
Technical field
The invention belongs to the combination of 3D technology and new forms of energy nm regime, relate to a kind of method preparing tin carbon anode/lithiated-iron-phosphate cathode lithium ion battery based on 3D printing technique.
Background technology
Along with the exhaustion day by day of traditional energy, lithium rechargeable battery represents as new forms of energy thus receives and pays close attention to widely.Simultaneously lithium ion battery is as the main power source of mobile communication equipment with mancarried electronic aid, has the advantages such as output voltage is higher, without memory, high-energy-density and become the focus studied both at home and abroad due to it.But the problem such as tradition is not high based on the lithium ion battery ubiquity specific area of plane electrode, energy storage density is limited, electrode polarization is serious.
In recent years along with the rise of nanometer technology and 3D printing technique, nanometer technology and 3D printing technique are extended to military affairs, electronics, medical science, biological, the fields such as new forms of energy, especially novel 3D prints the appearance of integrated lithium ion battery, effectively achieve the effective integration of lithium ion battery anode and cathode and package system thereof, revolutionize conventional planar electrode type lithium ion battery structure, this will substantially increase the ratio of active material in battery electrode material, shorten the migration distance in lithium ion charge and discharge process, thus substantially increase lithium ion diffusion rate and mobility.
Print in Study on Li-ion batteries at novel 3D, now successfully develop and be anode with spinel type lithium titanate nano material, take lithium iron phosphate nano material as the novel 3D electrode lithium ion battery of negative electrode.But due to the electronic conductivity of lithium titanate material itself and ionic conductivity bad, problem and the defects such as so the lithium ion battery made exists, capacity attenuation is very fast, cycle performance is poor, specific energy density is not high.
Summary of the invention
For shortcomings and deficiencies of the prior art, the invention provides a kind of method preparing tin carbon anode/lithiated-iron-phosphate cathode lithium ion battery based on 3D printing technique.This method is mainly dissolved into respectively in respective solution with tin carbon nanometer material, LiFePO4 respectively and prepares each printing electrode ink, recycling 3D printing technique, prepare with tin carbon nanometer material for anode, LiFePO4 is the 3D structure electrode lithium ion battery of cathode material.Electrode material prepared by the method has the advantages such as specific area is large, energy density is high, anode and cathode electrode spacing is little.These all will greatly improve lithium ion diffusion velocity in-between the electrodes, and then improve its ion and electronic conductivity, therefore, have huge application potential in high performance lithium ion battery field.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method preparing tin carbon anode/lithiated-iron-phosphate cathode lithium ion battery based on 3D printing technique, it is characterized in that: print using tin carbon as anode material, using LiFePO4 as cathode material with 3D printing technique, finally prepare NEW TYPE OF COMPOSITE lithium ion battery by encapsulation again.
Wherein, the preparation method of tin carbon anode ink and lithiated-iron-phosphate cathode ink is as follows:
1) 3-5g tin carbon is joined in the first mixed solution of the glycerol of 100-120mL deionized water and 30-50mL; 2-4g LiFePO4 is joined in the second mixed solution of the glycerol of 60-100mL deionized water and 30-50mL, the first suspension-turbid liquid and the second suspension-turbid liquid can be obtained respectively;
2) the first suspension-turbid liquid and the second suspension-turbid liquid are at room temperature distinguished ball milling 20-30h, and the material that will obtain centrifugal 3-10min respectively, its medium speed is 3500-4000rpm; By the solution centrifugal 1.5-3h again obtained after centrifugal, rotating speed is 2500-3500rpm;
3) the two kinds of materials above-mentioned centrifugal filtration collected be distributed to glycerine, 3.5% water hydroxypropyl cellulose and 3% water hydroxyethylcellulose in;
4) the stanniferous carbon anode mixture of result homogeneous is made up of the glycerol of 27% glycerine, 20%-30%, the water hydroxypropyl cellulose of 9%, the water hydroxyethylcellulose of 1% and deionized water; Being made up of the glycerol of 25% glycerine, 22%-34%, the water hydroxypropyl cellulose of 9%, the water hydroxyethylcellulose of 1% and deionized water containing phosphonic acids iron lithium cathode mix of homogeneous;
5), subsequently after strong stirring 1-3h and evaporating solvent, under normal temperature, natural evaporation to quality becomes original 50-70%, can obtain required tin carbon anode marking ink and lithiated-iron-phosphate cathode marking ink respectively.
Printing before electrode by 3D technology, specification be in 15 × 10mm substrate of glass by the gold of printing and electron beam coating technique formation rule to electrode, as respectively as the negative electrode of lithium ion battery and anode current collector.
Anode and cathode ink material is placed on respectively 2-5mL to inject in micro-nozzle, by control jet pipe spray ink flow successively print comb teeth-shaped anodic-cathodic.
After battery structure has printed, in tube furnace, 500-700oC will be heated under argon shield condition, and be incubated 2h.
After utilizing poly methyl methacrylate plastic plate and dimethyl silicone polymer fluid sealant to be sealed by coaxial electrode surrounding materials along glass substrate; transfer in glove box; electrolyte is instilled under argon shield; to cover above it with poly methyl methacrylate plastic plate and dimethyl silicone polymer fluid sealant and seal again after complete wetting, namely obtaining required lithium ion battery.
The present invention mainly prepares the method for tin carbon anode/lithiated-iron-phosphate cathode lithium ion battery based on 3D printing technique, have preparation method's novelty, the simple feature of technique; Prepared electrode material has the advantages such as specific area is large, energy density is high, electric conductivity is good.Huge application potential is had in high performance lithium ion battery field.
Accompanying drawing explanation
Fig. 1 is Structure of the cathode and the anode comb assembling structure (for four layers, in fact can multilayer) that 3D printing technique prints
Fig. 2 is the electrode structure (comprising package casing) of the final lithium ion battery that 3D printing technique prints.
Embodiment
The present invention aims to provide a kind of method being prepared the lithium ion battery of tin carbon anode and lithiated-iron-phosphate cathode by 3D printing technique, existing by reference to the accompanying drawings and concrete execution mode illustrate.
Embodiment 1
1) tin carbon nanometer dispersion of materials prepared by 3g is taken in the first mixed solution of the glycerol of 100mL deionized water and 30mL; Taking LiFePO4 prepared by 2g is distributed in the second mixed solution of the glycerol of 60mL deionized water and 30mL, can obtain the first suspension-turbid liquid and the second suspension-turbid liquid respectively.
2) the first suspension-turbid liquid and the second suspension-turbid liquid are at room temperature distinguished ball milling 20h, then respectively by twice centrifuging process.First time is centrifugal is centrifugal 3min under 3500rpm rotating speed, to remove large aggregate; Second time is the solution centrifugal 1.5h again will obtained after centrifugal at 2500rpm, to collect fine particle.
3) the two kinds of materials above-mentioned centrifugal filtration collected be distributed to glycerine, 3.5% water hydroxypropyl cellulose and 3% water hydroxyethylcellulose in.The stanniferous carbon anode mixture of homogeneous by 27% glycerine, 20% glycerol, the water hydroxypropyl cellulose of 9%, the water hydroxyethylcellulose of 1% and deionized water form (mass percent); Homogeneous containing phosphonic acids iron lithium cathode mix by 25% glycerine, 22% glycerol, the water hydroxypropyl cellulose of 9%, the water hydroxyethylcellulose of 1% and deionized water form (mass percent).Subsequently after strong stirring 1h and evaporating solvent, under normal temperature, natural evaporation to quality becomes original 50%, can obtain required tin carbon anode marking ink and lithiated-iron-phosphate cathode marking ink respectively.
4) printing before electrode by 3D technology, specification be in 15 × 10mm substrate of glass by the gold of printing and electron beam coating technique formation rule to electrode, as respectively as the negative electrode of lithium ion battery and anode current collector.Anode and cathode ink material is placed on respectively in injection micro-nozzle (3mL), by control jet pipe spray ink flow successively print comb teeth-shaped anodic-cathodic, as in Fig. 1: 1 is anode, and 2 is negative electrode.After battery structure has printed, in tube furnace, 500 will be heated under argon shield condition
oc, and be incubated 2h.
5) after utilizing PMMA (polymethyl methacrylate) plastic plate and PDMS (dimethyl silicone polymer) fluid sealant to be sealed by coaxial electrode surrounding materials along glass substrate; transfer in glove box; electrolyte is instilled under argon shield; to cover above it with PMMA plastic plate and PDMS fluid sealant and seal again after complete wetting; namely required lithium ion battery is obtained; as shown in Figure 2; 1 is anode; 2 is negative electrode; 3 is anode gold electrode current collector; 4 is negative electrode gold electrode current collector, and 5 is glass substrate.
Embodiment 2
1) tin carbon nanometer dispersion of materials prepared by 4g is taken in the first mixed solution of the glycerol of 110mL deionized water and 40mL; Taking LiFePO4 prepared by 3g is distributed in the second mixed solution of the glycerol of 80mL deionized water and 40mL, can obtain the first suspension-turbid liquid and the second suspension-turbid liquid respectively.
2) the first suspension-turbid liquid and the second suspension-turbid liquid are at room temperature distinguished ball milling 25h, then respectively by twice centrifuging process.First time is centrifugal is centrifugal 5min under 3800rpm rotating speed, to remove large aggregate; Second time is the solution centrifugal 2h again will obtained after centrifugal at 3000rpm, to collect fine particle.
3) the two kinds of materials above-mentioned centrifugal filtration collected be distributed to glycerine, 3.5% water hydroxypropyl cellulose and 3% water hydroxyethylcellulose in.The stanniferous carbon anode mixture of homogeneous by 27% glycerine, 20% glycerol, the water hydroxypropyl cellulose of 9%, the water hydroxyethylcellulose of 1% and deionized water form (mass percent); Homogeneous containing phosphonic acids iron lithium cathode mix by 25% glycerine, 25% glycerol, the water hydroxypropyl cellulose of 9%, the water hydroxyethylcellulose of 1% and deionized water form (mass percent).Subsequently after strong stirring 2h and evaporating solvent, under normal temperature, natural evaporation to quality becomes original 60%, can obtain required tin carbon anode marking ink and lithiated-iron-phosphate cathode marking ink respectively.
4) printing before electrode by 3D technology, specification be in 15 × 10mm substrate of glass by the gold of printing and electron beam coating technique formation rule to electrode, as respectively as the negative electrode of lithium ion battery and anode current collector.Anode and cathode ink material is placed on respectively in injection micro-nozzle (3mL), by control jet pipe spray ink flow successively print comb teeth-shaped anodic-cathodic, as in Fig. 1: 1 is anode, and 2 is negative electrode.After battery structure has printed, in tube furnace, 600 will be heated under argon shield condition
oc, and be incubated 2h
5) after utilizing PMMA (polymethyl methacrylate) plastic plate and PDMS (dimethyl silicone polymer) fluid sealant to be sealed by coaxial electrode surrounding materials along glass substrate; transfer in glove box; electrolyte is instilled under argon shield; to cover above it with PMMA plastic plate and PDMS fluid sealant and seal again after complete wetting; namely required lithium ion battery is obtained; as shown in Figure 2; 1 is anode; 2 is negative electrode; 3 is anode gold electrode current collector; 4 is negative electrode gold electrode current collector, and 5 is glass substrate.
Embodiment 3
1) tin carbon nanometer dispersion of materials prepared by 5g is taken in the first mixed solution of the glycerol of 120mL deionized water and 50mL; Taking LiFePO4 prepared by 4g is distributed in the second mixed solution of the glycerol of 100mL deionized water and 50mL, can obtain the first suspension-turbid liquid and the second suspension-turbid liquid respectively.
2) the first suspension-turbid liquid and the second suspension-turbid liquid are at room temperature distinguished ball milling 30h, then respectively by twice centrifuging process.First time is centrifugal is centrifugal 10min under 4000rpm rotating speed, to remove large aggregate; Second time is the solution centrifugal 3h again will obtained after centrifugal at 3500rpm, to collect fine particle.
3) the two kinds of materials above-mentioned centrifugal filtration collected be distributed to glycerine, 3.5% water hydroxypropyl cellulose and 3% water hydroxyethylcellulose in.The stanniferous carbon anode mixture of homogeneous by 27% glycerine, 20% glycerol, the water hydroxypropyl cellulose of 9%, the water hydroxyethylcellulose of 1% and deionized water form (mass percent); Homogeneous containing phosphonic acids iron lithium cathode mix by 25% glycerine, 30% glycerol, the water hydroxypropyl cellulose of 9%, the water hydroxyethylcellulose of 1% and deionized water form (mass percent).Subsequently after strong stirring 3h and evaporating solvent, under normal temperature, natural evaporation to quality becomes original 70%, can obtain required tin carbon anode marking ink and lithiated-iron-phosphate cathode marking ink respectively.
4) printing before electrode by 3D technology, specification be in 15 × 10mm substrate of glass by the gold of printing and electron beam coating technique formation rule to electrode, as respectively as the negative electrode of lithium ion battery and anode current collector.Anode and cathode ink material is placed on respectively in injection micro-nozzle (3mL), by control jet pipe spray ink flow successively print comb teeth-shaped anodic-cathodic, as in Fig. 1: 1 is anode, and 2 is negative electrode.After battery structure has printed, in tube furnace, 700 will be heated under argon shield condition
oc, and be incubated 2h
5) after utilizing PMMA (polymethyl methacrylate) plastic plate and PDMS (dimethyl silicone polymer) fluid sealant to be sealed by coaxial electrode surrounding materials along glass substrate; transfer in glove box; electrolyte is instilled under argon shield; to cover above it with PMMA plastic plate and PDMS fluid sealant and seal again after complete wetting; namely required lithium ion battery is obtained; as shown in Figure 2; 1 is anode; 2 is negative electrode; 3 is anode gold electrode current collector; 4 is negative electrode gold electrode current collector, and 5 is glass substrate.
Claims (6)
1. prepare the method for tin carbon anode/lithiated-iron-phosphate cathode lithium ion battery based on 3D printing technique for one kind, it is characterized in that: print using tin carbon as anode material, using LiFePO4 as cathode material with 3D printing technique, finally prepare NEW TYPE OF COMPOSITE lithium ion battery by encapsulation again.
2. a kind of method preparing tin carbon anode/lithiated-iron-phosphate cathode lithium ion battery based on 3D printing technique according to claim 1, is characterized in that: the preparation method of tin carbon anode ink and lithiated-iron-phosphate cathode ink is as follows:
1) 3-5g tin carbon is joined in the first mixed solution of the glycerol of 100-120mL deionized water and 30-50mL; 2-4g LiFePO4 is joined in the second mixed solution of the glycerol of 60-100mL deionized water and 30-50mL, the first suspension-turbid liquid and the second suspension-turbid liquid can be obtained respectively;
2) the first suspension-turbid liquid and the second suspension-turbid liquid are at room temperature distinguished ball milling 20-30h, and the material that will obtain centrifugal 3-10min respectively, its medium speed is 3500-4000rpm; By the solution centrifugal 1.5-3h again obtained after centrifugal, rotating speed is 2500-3500rpm;
3) the two kinds of materials above-mentioned centrifugal filtration collected be distributed to glycerine, 3.5% water hydroxypropyl cellulose and 3% water hydroxyethylcellulose in;
4) the stanniferous carbon anode mixture of result homogeneous is made up of the glycerol of 27% glycerine, 20%-30%, the water hydroxypropyl cellulose of 9%, the water hydroxyethylcellulose of 1% and deionized water; Being made up of the glycerol of 25% glycerine, 22%-34%, the water hydroxypropyl cellulose of 9%, the water hydroxyethylcellulose of 1% and deionized water containing phosphonic acids iron lithium cathode mix of homogeneous;
5), subsequently after strong stirring 1-3h and evaporating solvent, under normal temperature, natural evaporation to quality becomes original 50-70%, can obtain required tin carbon anode marking ink and lithiated-iron-phosphate cathode marking ink respectively.
3. a kind of method preparing tin carbon anode/lithiated-iron-phosphate cathode lithium ion battery based on 3D printing technique according to claim 2, it is characterized in that: before printing electrode by 3D technology, will specification be in 15 × 10mm substrate of glass by printing and the gold of electron beam coating technique formation rule to electrode, as respectively as the negative electrode of lithium ion battery and anode current collector.
4. a kind of method preparing tin carbon anode/lithiated-iron-phosphate cathode lithium ion battery based on 3D printing technique according to claim 2, it is characterized in that: anode and cathode ink material is placed on respectively 2-5mL and injects in micro-nozzle, by control jet pipe spray ink flow successively print comb teeth-shaped anodic-cathodic.
5. a kind of method preparing tin carbon anode/lithiated-iron-phosphate cathode lithium ion battery based on 3D printing technique according to claim 2, is characterized in that: after battery structure has printed, will be heated to 500-700 in tube furnace under argon shield condition
oc, and be incubated 2h.
6. a kind of method preparing tin carbon anode/lithiated-iron-phosphate cathode lithium ion battery based on 3D printing technique according to claim 2; it is characterized in that: after utilizing poly methyl methacrylate plastic plate and dimethyl silicone polymer fluid sealant to be sealed by coaxial electrode surrounding materials along glass substrate; transfer in glove box; electrolyte is instilled under argon shield; to cover above it with poly methyl methacrylate plastic plate and dimethyl silicone polymer fluid sealant and seal again after complete wetting, namely obtaining required lithium ion battery.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105417833A (en) * | 2015-12-25 | 2016-03-23 | 福州品行科技发展有限公司 | Portable hydrogen-rich water cup having water-purifying and light-reminding functions and use method thereof |
| CN107252707A (en) * | 2017-06-01 | 2017-10-17 | 清华大学深圳研究生院 | A kind of microfluidic system and its preparation technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101017893B (en) * | 2006-02-08 | 2010-05-12 | 深圳市比克电池有限公司 | A tin carbon compound electrode material for lithium ion battery cathode and preparing method |
| CN101202340A (en) * | 2007-12-07 | 2008-06-18 | 广西师范大学 | Tin carbon nanometer compound material for lithium ion battery and method for making same |
| CN102054970B (en) * | 2009-11-02 | 2013-02-13 | 五邑大学 | Method for preparing tin-carbon cathode material of lithium ion battery |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105417833A (en) * | 2015-12-25 | 2016-03-23 | 福州品行科技发展有限公司 | Portable hydrogen-rich water cup having water-purifying and light-reminding functions and use method thereof |
| CN105417833B (en) * | 2015-12-25 | 2018-03-16 | 福州品行科技发展有限公司 | A kind of portable hydrogen-rich cup and its application method with water purification and light prompting function |
| CN107252707A (en) * | 2017-06-01 | 2017-10-17 | 清华大学深圳研究生院 | A kind of microfluidic system and its preparation technology |
| CN107252707B (en) * | 2017-06-01 | 2019-07-05 | 清华大学深圳研究生院 | A kind of microfluidic system and its preparation process |
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