CN104409728B - 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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- CN104409728B CN104409728B CN201410237602.9A CN201410237602A CN104409728B CN 104409728 B CN104409728 B CN 104409728B CN 201410237602 A CN201410237602 A CN 201410237602A CN 104409728 B CN104409728 B CN 104409728B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention 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, it is related to one kind and stannum carbon is prepared based on 3D printing technique
The method of anode/lithiated-iron-phosphate cathode lithium ion battery.
Background technology
With the increasingly depleted of traditional energy, lithium rechargeable battery represents as new forms of energy thus receiving extensive pass
Note.Lithium ion battery is as the main power source of mobile communication equipment and mancarried electronic aid simultaneously, because it has output voltage
The advantages such as higher, without memory, high-energy-density and become the focus of domestic and international research.But the lithium based on plane electrode for the tradition
The problems such as ion battery generally existing specific surface area is not high, energy storage density is limited, electrode polarization is serious.
Recently as the rise of nanotechnology and 3D printing technique, nanotechnology and 3D printing technique have been extended to army
The fields such as thing, electronics, medical science, biology, new forms of energy, the appearance of the integrated lithium ion battery of especially new 3D printing, effectively realize
The effective integration of lithium ion battery anode and cathode and its package system, revolutionizes conventional planar electrode type lithium ion battery knot
Structure, this will substantially increase the ratio of active substance in battery electrode material, shortens the migration in lithium ion charge and discharge process
Distance, thus substantially increase lithium ion diffusion rate and mobility.
In terms of new 3D printing Study on Li-ion batteries, successfully develop with spinel type lithium titanate nano material
For anode, the new 3D electrode lithium ion battery with lithium iron phosphate nano material as negative electrode.But due to lithium titanate material itself
Electronic conductivity and ionic conductivity bad, so the lithium ion battery made exists, capacity attenuation is very fast, cycle performance is poor,
The problems such as specific energy density is high and defect.
Content of the invention
For shortcomings and deficiencies of the prior art, the invention provides a kind of based on 3D printing technique prepare stannum carbon anode/
The method of lithiated-iron-phosphate cathode lithium ion battery.This method is mainly molten respectively with tin carbon nanometer material, LiFePO4 respectively
Solution prepares each printing electrode ink in respective solution, recycles 3D printing technique, prepares with tin carbon nanometer material as sun
Pole, LiFePO4 is the 3D structure electrode lithium ion battery of cathode material.Electrode material prepared by the method has specific surface
Amass the advantages such as big, energy density is high, anode and cathode electrode spacing is little.These all will greatly improve lithium ion expansion in-between the electrodes
Scattered speed, and then improve its ion and electronic conductivity, therefore, there is huge application to dive in high performance lithium ion battery field
Power.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of method preparing stannum carbon anode/lithiated-iron-phosphate cathode lithium ion battery based on 3D printing technique, its feature exists
In：Printed using stannum carbon as anode material, using LiFePO4 as cathode material with 3D printing technique, finally pass through encapsulation again
Prepare NEW TYPE OF COMPOSITE lithium ion battery.
Wherein, the preparation method of stannum carbon anode ink and lithiated-iron-phosphate cathode ink is as follows：
1）In first mixed solution of glycerol 3-5g stannum carbon being added to 100-120mL deionized water and 30-50mL；
In second mixed solution of glycerol 2-4g LiFePO4 being added to 60-100mL deionized water and 30-50mL, respectively can
Obtain the first suspension and the second suspension；
2）First suspension and the second suspension are distinguished ball milling 20-30h at room temperature, and by the material obtaining respectively from
Heart 3-10min, wherein rotating speed are 3500-4000rpm；The solution recentrifuge 1.5-3h that will obtain after centrifugation, rotating speed is 2500-
3500rpm；
3）Two kinds of materials that above-mentioned centrifugal filtration is collected are distributed to glycerol, 3.5% water hydroxypropyl cellulose and 3%
In water hydroxyethyl cellulose；
4）The stanniferous carbon anode mixture of result homogenizing by 27% glycerol, the glycerol of 20%-30%, 9% water hydroxypropyl fine
Dimension element, 1% water hydroxyethyl cellulose and deionized water composition；The lithium cathode mix of ferrum containing phosphonic acids of homogenizing by 25% glycerol,
The glycerol of 22%-34%, 9% water hydroxypropyl cellulose, 1% water hydroxyethyl cellulose and deionized water composition；
5）Subsequently after strong stirring 1-3h and evaporation solvent, under room temperature, natural evaporation to quality is changed into original 50-70%,
Required stannum carbon anode marking ink and lithiated-iron-phosphate cathode marking ink can be respectively obtained.
Before printing electrode with 3D technology, be by printing and electron beam plating in 15 × 10mm substrate of glass in specification
The gold of membrane technology formation rule to electrode, as respectively as the negative electrode of lithium ion battery and anode current collector.
Anode and cathode ink material is individually placed in 2-5mL injection micro-nozzle, by controlling the stream of the sprayed ink of jet pipe
Amount successively prints comb teeth-shaped anodic-cathodic.
Battery structure prints after completing, and being heated to 500-700oC under argon protective condition in tube furnace, and will be incubated
2h.
Using poly methyl methacrylate plastic plate and polydimethylsiloxane fluid sealant along glass substrate by coaxial electrical
After the surrounding materials sealing of pole, transfer in glove box, instill electrolyte under argon protection, use poly- methyl after complete wetting again
Acrylic acid methyl ester. plastic plate and polydimethylsiloxane fluid sealant will cover above it and seal, that is, obtain required lithium-ion electric
Pond.
Present invention is primarily based on the method that 3D printing technique prepares stannum carbon anode/lithiated-iron-phosphate cathode lithium ion battery, tool
There are preparation method novelty, process is simple feature；Prepared electrode material has that specific surface area is big, energy density is high, electric conductivity
Advantage can well be waited.There is huge application potential in high performance lithium ion battery field.
Brief description
Fig. 1 combs assembling structure for the Structure of the cathode and the anode that 3D printing technique prints（Taking four layers as a example, can essentially multilamellar）
The electrode structure of the final lithium ion battery that Fig. 2 prints for 3D printing technique（Including package casing）.
Specific embodiment
The present invention is intended to provide a kind of lithium-ion electric preparing stannum carbon anode and lithiated-iron-phosphate cathode by 3D printing technique
The method in pond, to illustrate in conjunction with accompanying drawing and specific embodiment.
Embodiment 1
1）Weigh 3g preparation tin carbon nanometer material be distributed to 100mL deionized water and 30mL glycerol first mixing
In solution；In the second mixed solution of glycerol that the LiFePO4 weighing 2g preparation is distributed to 60mL deionized water and 30mL,
Can get the first suspension and the second suspension respectively.
2）First suspension and the second suspension are distinguished ball milling 20h at room temperature, then passes through two times centrifugal work respectively
Skill.Centrifugation for the first time is centrifugation 3min under 3500rpm rotating speed, to remove big aggregate；It is will be from 2500rpm for the second time
The solution recentrifuge 1.5h obtaining after the heart, to collect fine particle.
3）Two kinds of materials that above-mentioned centrifugal filtration is collected are distributed to glycerol, 3.5% water hydroxypropyl cellulose and 3%
In water hydroxyethyl cellulose.The stanniferous carbon anode mixture of homogenizing by 27% glycerol, 20% glycerol, 9% water hydroxypropyl fine
Dimension element, 1% water hydroxyethyl cellulose and deionized water composition（Mass percent）；The lithium cathode mix of ferrum containing phosphonic acids of homogenizing
It is made up of 25% glycerol, 22% glycerol, 9% water hydroxypropyl cellulose, 1% water hydroxyethyl cellulose and deionized water（Matter
Amount percentage ratio）.Subsequently after strong stirring 1h and evaporation solvent, under room temperature, natural evaporation to quality is changed into original 50%, you can point
Do not obtain required stannum carbon anode marking ink and lithiated-iron-phosphate cathode marking ink.
4）Before printing electrode with 3D technology, be by printing and electron beam in 15 × 10mm substrate of glass in specification
The gold of coating technique formation rule to electrode, as respectively as the negative electrode of lithium ion battery and anode current collector.By anode and cathode
Ink material is individually placed to inject micro-nozzle（3mL）In, successively print comb by controlling the flow of the sprayed ink of jet pipe
In shape anodic-cathodic, such as Fig. 1：1 is anode, and 2 is negative electrode.Battery structure prints after completing, argon protection in tube furnace
Under the conditions of be heated to 500oC, and it is incubated 2h.
5）Using PMMA (polymethyl methacrylate) plastic plate and PDMS (polydimethylsiloxane) fluid sealant along glass
Glass substrate, by after the sealing of coaxial electrode surrounding materials, is transferred in glove box, is instilled electrolyte, treat to soak completely under argon protection
To be covered above it and seal with PMMA plastic plate and PDMS fluid sealant again after profit, that is, obtain required lithium ion battery, such as Fig. 2
Shown, 1 is anode, and 2 is negative electrode, and 3 is anode gold electrode current collector, and 4 is negative electrode gold electrode current collector, and 5 is glass substrate.
Embodiment 2
1）Weigh 4g preparation tin carbon nanometer material be distributed to 110mL deionized water and 40mL glycerol first mixing
In solution；In the second mixed solution of glycerol that the LiFePO4 weighing 3g preparation is distributed to 80mL deionized water and 40mL,
Can get the first suspension and the second suspension respectively.
2）First suspension and the second suspension are distinguished ball milling 25h at room temperature, then passes through two times centrifugal work respectively
Skill.Centrifugation for the first time is centrifugation 5min under 3800rpm rotating speed, to remove big aggregate；It is will be from 3000rpm for the second time
The solution recentrifuge 2h obtaining after the heart, to collect fine particle.
3）Two kinds of materials that above-mentioned centrifugal filtration is collected are distributed to glycerol, 3.5% water hydroxypropyl cellulose and 3%
In water hydroxyethyl cellulose.The stanniferous carbon anode mixture of homogenizing by 27% glycerol, 20% glycerol, 9% water hydroxypropyl fine
Dimension element, 1% water hydroxyethyl cellulose and deionized water composition（Mass percent）；The lithium cathode mix of ferrum containing phosphonic acids of homogenizing
It is made up of 25% glycerol, 25% glycerol, 9% water hydroxypropyl cellulose, 1% water hydroxyethyl cellulose and deionized water（Matter
Amount percentage ratio）.Subsequently after strong stirring 2h and evaporation solvent, under room temperature, natural evaporation to quality is changed into original 60%, you can point
Do not obtain required stannum carbon anode marking ink and lithiated-iron-phosphate cathode marking ink.
4）Before printing electrode with 3D technology, be by printing and electron beam in 15 × 10mm substrate of glass in specification
The gold of coating technique formation rule to electrode, as respectively as the negative electrode of lithium ion battery and anode current collector.By anode and cathode
Ink material is individually placed to inject micro-nozzle（3mL）In, successively print comb by controlling the flow of the sprayed ink of jet pipe
In shape anodic-cathodic, such as Fig. 1：1 is anode, and 2 is negative electrode.Battery structure prints after completing, argon protection in tube furnace
Under the conditions of be heated to 600oC, and it is incubated 2h
5）Using PMMA (polymethyl methacrylate) plastic plate and PDMS (polydimethylsiloxane) fluid sealant along glass
Glass substrate, by after the sealing of coaxial electrode surrounding materials, is transferred in glove box, is instilled electrolyte, treat to soak completely under argon protection
To be covered above it and seal with PMMA plastic plate and PDMS fluid sealant again after profit, that is, obtain required lithium ion battery, such as Fig. 2
Shown, 1 is anode, and 2 is negative electrode, and 3 is anode gold electrode current collector, and 4 is negative electrode gold electrode current collector, and 5 is glass substrate.
Embodiment 3
1）Weigh 5g preparation tin carbon nanometer material be distributed to 120mL deionized water and 50mL glycerol first mixing
In solution；In the second mixed solution of glycerol that the LiFePO4 weighing 4g preparation is distributed to 100mL deionized water and 50mL,
Can get the first suspension and the second suspension respectively.
2）First suspension and the second suspension are distinguished ball milling 30h at room temperature, then passes through two times centrifugal work respectively
Skill.Centrifugation for the first time is centrifugation 10min under 4000rpm rotating speed, to remove big aggregate；It is will in 3500rpm for the second time
The solution recentrifuge 3h obtaining after centrifugation, to collect fine particle.
3）Two kinds of materials that above-mentioned centrifugal filtration is collected are distributed to glycerol, 3.5% water hydroxypropyl cellulose and 3%
In water hydroxyethyl cellulose.The stanniferous carbon anode mixture of homogenizing by 27% glycerol, 20% glycerol, 9% water hydroxy propyl cellulose
Element, 1% water hydroxyethyl cellulose and deionized water composition（Mass percent）；The lithium cathode mix of ferrum containing phosphonic acids of homogenizing by
25% glycerol, 30% glycerol, 9% water hydroxypropyl cellulose, 1% water hydroxyethyl cellulose and deionized water composition（Quality
Percentage ratio）.Subsequently after strong stirring 3h and evaporation solvent, under room temperature, natural evaporation to quality is changed into original 70%, you can respectively
Obtain required stannum carbon anode marking ink and lithiated-iron-phosphate cathode marking ink.
4）Before printing electrode with 3D technology, be by printing and electron beam in 15 × 10mm substrate of glass in specification
The gold of coating technique formation rule to electrode, as respectively as the negative electrode of lithium ion battery and anode current collector.By anode and cathode
Ink material is individually placed to inject micro-nozzle（3mL）In, successively print comb by controlling the flow of the sprayed ink of jet pipe
In shape anodic-cathodic, such as Fig. 1：1 is anode, and 2 is negative electrode.Battery structure prints after completing, argon protection in tube furnace
Under the conditions of be heated to 700oC, and it is incubated 2h
5）Using PMMA (polymethyl methacrylate) plastic plate and PDMS (polydimethylsiloxane) fluid sealant along glass
Glass substrate, by after the sealing of coaxial electrode surrounding materials, is transferred in glove box, is instilled electrolyte, treat to soak completely under argon protection
To be covered above it and seal with PMMA plastic plate and PDMS fluid sealant again after profit, that is, obtain required lithium ion battery, such as Fig. 2
Shown, 1 is anode, and 2 is negative electrode, and 3 is anode gold electrode current collector, and 4 is negative electrode gold electrode current collector, and 5 is glass substrate.
Claims (1)
1. a kind of based on 3D printing technique prepare stannum carbon anode/lithiated-iron-phosphate cathode lithium ion battery method it is characterised in that：
Printed using stannum carbon as anode material, using LiFePO4 as cathode material, finally again by encapsulation system with 3D printing technique
Standby go out composite lithium ion cell；The method comprises the following steps：
Step S1：Prepare stannum carbon anode ink and lithiated-iron-phosphate cathode ink：
1）In first mixed solution of glycerol 3-5g stannum carbon being added to 100-120mL deionized water and 30-50mL；By 2-
4g LiFePO4 is added in the second mixed solution of the glycerol of 60-100mL deionized water and 30-50mL, respectively obtains
One suspension and the second suspension；
2）First suspension and the second suspension are distinguished ball milling 20-30h at room temperature, and the material obtaining is centrifuged 3- respectively
10min, wherein rotating speed are 3500-4000rpm；The solution recentrifuge 1.5-3h that will obtain after centrifugation, rotating speed is 2500-
3500rpm；
3）Two kinds of materials that above-mentioned centrifugal filtration is collected are distributed to the water hydroxyl of glycerol, 3.5% water hydroxypropyl cellulose and 3%
In ethyl cellulose；
4）The stanniferous carbon anode mixture of result homogenizing includes 27% glycerol, the glycerol of 20%-30%, 9% water hydroxy propyl cellulose
Element, 1% water hydroxyethyl cellulose and deionized water；The phosphoric acid ferrum lithium cathode mix of homogenizing includes 25% glycerol, 22%-34%
Glycerol, 9% water hydroxypropyl cellulose, 1% water hydroxyethyl cellulose and deionized water；
5）Subsequently after strong stirring 1-3h and evaporation solvent, under room temperature, natural evaporation to quality is changed into original 50-70%, you can
Respectively obtain required stannum carbon anode marking ink and lithiated-iron-phosphate cathode marking ink；
Step S2：Before printing electrode with 3D technology, be by printing and electronics in 15 × 10mm substrate of glass in specification
The gold of bundle coating technique formation rule to electrode, as respectively as the negative electrode of lithium ion battery and anode current collector；
Step S3：Anode and cathode ink material is individually placed in 2-5mL injection micro-nozzle, by controlling the sprayed ink of jet pipe
Flow successively prints comb teeth-shaped anodic-cathodic；
Step S4：Battery structure prints after completing, and will be heated to 500-700 in tube furnace under argon protective conditionoC, and protect
Warm 2h；
Step S5：Will be coaxial along glass substrate using poly methyl methacrylate plastic plate and polydimethylsiloxane fluid sealant
After sealing around electrode material, transfer in glove box, instill electrolyte under argon protection, use poly- first after complete wetting again
Base acrylic acid methyl ester. plastic plate and polydimethylsiloxane fluid sealant will cover above it and seal, that is, obtain required lithium ion
Battery.
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| CN201410237602.9A CN104409728B (en) | 2014-05-31 | 2014-05-31 | Method for preparing tin-carbon anode/lithium iron phosphate cathode lithium ion battery based on 3D printing technology |
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| 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 |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101017893A (en) * | 2006-02-08 | 2007-08-15 | 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 |
| CN102054970A (en) * | 2009-11-02 | 2011-05-11 | 五邑大学 | Method for preparing tin-carbon cathode material of lithium ion battery |
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2014
- 2014-05-31 CN CN201410237602.9A patent/CN104409728B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101017893A (en) * | 2006-02-08 | 2007-08-15 | 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 |
| CN102054970A (en) * | 2009-11-02 | 2011-05-11 | 五邑大学 | Method for preparing tin-carbon cathode material of lithium ion battery |
Non-Patent Citations (1)
| Title |
|---|
| "3D Printing of Interdigitated Li-Ion Microbattery Architectures";Ke Sun et al.;《Advanced Materials》;20130617;第25卷(第33期);第4539页左栏第1段-第4541页右栏第1段、实验部分及附图1、附图3b以及附图4a * |
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