CN110497595A - A kind of preparation method of the 3D printing silk material of solid electrolyte - Google Patents

A kind of preparation method of the 3D printing silk material of solid electrolyte Download PDF

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Publication number
CN110497595A
CN110497595A CN201910645436.9A CN201910645436A CN110497595A CN 110497595 A CN110497595 A CN 110497595A CN 201910645436 A CN201910645436 A CN 201910645436A CN 110497595 A CN110497595 A CN 110497595A
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preparation
printing
silk material
solid electrolyte
powder
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CN201910645436.9A
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李庆棠
朱鹏博
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Beijing Aerospace Xinfeng Machinery Equipment Co Ltd
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Beijing Aerospace Xinfeng Machinery Equipment Co Ltd
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Priority to CN201910645436.9A priority Critical patent/CN110497595A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/05—Filamentary, e.g. strands
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
    • B29C64/30—Auxiliary operations or equipment
    • B29C64/307—Handling of material to be used in additive manufacturing
    • B29C64/314—Preparation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • 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
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • B29C2948/9259—Angular velocity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Dispersion Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Optics & Photonics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

A kind of preparation method of the 3D printing silk material of solid electrolyte, it is characterized in that, include the following steps, step 1, the composition of 3D printing silk material persursor material are as follows: lithium trifluoromethanesulp,onylimide, the polyethylene oxide of molecular weight 300,000 and with vinylidene fluoride-hexafluoropropylene copolymer, 3 components are dusty material, and taking mass ratio is 5:13~16:3~6；The present invention substitutes existing solid electrolyte artificial chemistry method, preparation efficiency, technology stability is substantially improved, while reducing the chemical poisoning risk in preparation process.Engineering technology basis is established for the large-scale promotion application of all-solid-state battery.

Description

A kind of preparation method of the 3D printing silk material of solid electrolyte
Technical field
The present invention is a kind of preparation method of the 3D printing silk material of solid electrolyte, is related to a kind of lithium ion solid electrolyte The preparation method of 3D printing silk material, prepared silk material are used for the preparation of lithium ion solid electrolyte.
Background technique
With advances in technology with the development of society, the key that energy problem has become the sustainable development of the relationship whole world is asked Topic.Immense pressure in terms of energy and environment to find and develop novel green renewable energy urgently appointing as society Business.
Solid lithium battery is as a kind of novel battery structure, in recent years by many concerns.Such battery not only has Higher energy density, while there is excellent thermal stability, chemical stability and mechanical stability, and not will cause electrolyte It is the problems such as leakage, highly-safe.
The fabricating technology of all-solid-state battery is still in the stage of fumbling at present, and process flow is usually by positive electrode Film forming is respectively applied with solid electrolyte, then together by the two rolling, bottom is bonded lithium foil, and rolling forms battery again.Therefore Cell manufacturing process is cumbersome and the degree of automation is low, and manufacturing cycle is longer；Meanwhile the use of solid electrolyte is to electrolyte inside Object phase distributing homogeneity and its solid-solid interface wetability between electrode propose harsh technique requirement, work hand-manipulated Skill poor controllability reduces battery performance stability；In addition, the acetonitrile solvent largely used in preparation is toxic, to operator Member has certain actual bodily harm.Therefore it needs to change existing all-solid-state battery preparation process at present, solve the above problems.
3D printing technique is as a kind of novel material preparation technology, and atomization degree is high, strong flexibility.This research Wish to develop a kind of novel solid electrolyte material, by the optimization on existing formula, be allowed to be suitable for 3D printing technique, To which 3D printing technique is embedded into the preparation process flow of all-solid-state battery, simplification of flowsheet, lifting process dynamicization journey Degree and stability.
Summary of the invention
The purpose of the present invention is developing a kind of solid electrolyte 3D printing silk material preparation method, it is good to obtain printing technology Solid electrolyte silk material.
A kind of preparation method of the 3D printing silk material of solid electrolyte, which is characterized in that include the following steps,
Step 1, the composition of 3D printing silk material persursor material are as follows: lithium trifluoromethanesulp,onylimide, molecular weight 300,000 it is poly- Ethylene oxide and with vinylidene fluoride-hexafluoropropylene copolymer, 3 components are dusty material, and taking mass ratio is 5:13~16:3 ~6；
Step 2,3D printing silk material persursor material preparation, by the polyethylene oxide powder of load weighted molecular weight 300,000 It is placed in uncovered beaker, adds load weighted vinylidene fluoride-hexafluoropropylene copolymer powder, stirred using blender, make two Person uniformly mixes ten minutes；Bis trifluoromethyl sulfimide lithium powder is weighed again to be put into same uncovered beaker, is then added The ratio of dehydrated alcohol, dehydrated alcohol and powder mixture is 5ml/g~6ml/g, is persistently stirred 20 minutes, is made using blender Bis trifluoromethyl sulfimide lithium powder is dissolved in dehydrated alcohol, while making polyethylene oxide and vinylidene-hexafluoro Propylene is well dispersed in dehydrated alcohol；After the completion of stirring, solution is heated up between 45~55 DEG C, dehydrated alcohol is slowly steamed It does and obtains blocky solid content, then solid content is sufficiently sheared, is dried in vacuo, it is final to obtain particulate electrolytic matter 3D printing presoma Material；
Step 3, silk material preparation: sending graininess persursor material into screw extruder, carries out blending throwing, and screw rod squeezes Machine revolving speed 100r/min~120r/min out, 200 DEG C~220 DEG C of throwing temperature, molding equipment internal vacuum is lower than 0.02MPa is mounted at outlet of extruder by one, linear velocity and the consistent filament winding machine of screw extruder extruded velocity, will Silk material is coiled, and is used for subsequent solid electrolyte 3D printing.
Wherein, in step 1, lithium trifluoromethanesulp,onylimide, the polyethylene oxide of molecular weight 300,000 and with vinylidene- Hexafluoropropylene copolymer, most preferably taking mass ratio is 5:15:4.
The present invention substitutes existing solid electrolyte artificial chemistry method, preparation efficiency, technology stability is substantially improved, together When reduce chemical poisoning risk in preparation process.Engineering technology is established for the large-scale promotion application of all-solid-state battery Basis.
Specific embodiment:
A kind of preparation method of the 3D printing silk material of solid electrolyte, which is characterized in that include the following steps,
Step 1, the composition of 3D printing silk material persursor material are as follows: lithium trifluoromethanesulp,onylimide, molecular weight 300,000 it is poly- Ethylene oxide and with vinylidene fluoride-hexafluoropropylene copolymer, 3 components are dusty material, and taking mass ratio is 5:13~16:3 ~6；
Step 2,3D printing silk material persursor material preparation, by the polyethylene oxide powder of load weighted molecular weight 300,000 It is placed in uncovered beaker, adds load weighted vinylidene fluoride-hexafluoropropylene copolymer powder, stirred using blender, make two Person uniformly mixes ten minutes；Bis trifluoromethyl sulfimide lithium powder is weighed again to be put into same uncovered beaker, is then added The ratio of dehydrated alcohol, dehydrated alcohol and powder mixture is 5ml/g~6ml/g, is persistently stirred 20 minutes, is made using blender Bis trifluoromethyl sulfimide lithium powder is dissolved in dehydrated alcohol, while making polyethylene oxide and vinylidene-hexafluoro Propylene is well dispersed in dehydrated alcohol；After the completion of stirring, solution is heated up between 45~55 DEG C, dehydrated alcohol is slowly steamed It does and obtains blocky solid content, then solid content is sufficiently sheared, is dried in vacuo, it is final to obtain particulate electrolytic matter 3D printing presoma Material；
Step 3, silk material preparation: sending graininess persursor material into screw extruder, carries out blending throwing, and screw rod squeezes Machine revolving speed 100r/min~120r/min out, 200 DEG C~220 DEG C of throwing temperature, molding equipment internal vacuum is lower than 0.02MPa is mounted at outlet of extruder by one, linear velocity and the consistent filament winding machine of screw extruder extruded velocity, will Silk material is coiled, and is used for subsequent solid electrolyte 3D printing.
Wherein, in step 1, lithium trifluoromethanesulp,onylimide, the polyethylene oxide of molecular weight 300,000 and with vinylidene- Hexafluoropropylene copolymer, most preferably taking mass ratio is 5:15:4.
Specific step is as follows for this method:
(1) precursor preparation
Solid electrolyte presoma includes 3 kinds of material components, the polycyclic oxygen of lithium trifluoromethanesulp,onylimide, molecular weight 300,000 Ethane and with vinylidene fluoride-hexafluoropropylene copolymer, is conduction lithium salts with bis trifluoromethyl sulfimide lithium, polyethylene oxide is Polymer dielectric, vinylidene fluoride-hexafluoropropylene copolymer are reinforcing material, and 3 kinds of materials are dusty material, pass through machinery Mixing, is sufficiently mixed three kinds of materials, form powder-mixed material, lithium salts, polyethylene oxide and biasfluoroethylene-hexafluoropropylene Mass ratio is 5/15/4.Specific steps are successively are as follows: weigh polyethylene oxide powder and are placed in uncovered beaker, add load weighted Vinylidene fluoride-hexafluoropropylene copolymer powder, is stirred using blender, makes the two uniformly mixing ten minutes.Double three are weighed again Methyl fluoride sulfimide lithium powder is put into same uncovered beaker, and dehydrated alcohol, dehydrated alcohol and powder mixture is then added Ratio be 5ml/g, persistently stirred using blender 20 minutes, bis trifluoromethyl sulfimide lithium powder made to be dissolved in nothing In water-ethanol, while it is well dispersed in polyethylene oxide and biasfluoroethylene-hexafluoropropylene in dehydrated alcohol.After the completion of stirring, Solution is warming up between 45~55 DEG C, dehydrated alcohol is slowly evaporated to the blocky solid content of acquisition, then solid content is sufficiently sheared, Vacuum drying, it is final to obtain particulate electrolytic matter 3D printing persursor material.
(2) prepared by silk material
Graininess persursor material is sent into screw extruder, carries out blending throwing, screw extruder revolving speed 100r/min, 200 DEG C of throwing temperature, molding equipment internal vacuum is lower than 0.02MPa, is mounted at outlet of extruder by one, linear velocity With the consistent filament winding machine of screw extruder extruded velocity, silk material is coiled, is used for subsequent solid electrolyte 3D printing.
(3) silk material quality evaluation
The macro microcosmic forming defect situation of material is characterized using electron microscope and Stereo microscope, is surveyed using stress rheometer Viscosity of material is tried, cupping machine test material mechanical property is used.The quality knot obtained by above several characterization test methods Fruit is as follows:
Macroscopic view molding: silk material diameter meets printing and requires within the scope of 1.4-1.7mm, and macroscopic view molding is good, and microscope is seen Examine lower pore-free, crack defect；
Microcosmic molding: under electron microscope observation, the defects of internal object mutually has good uniformity, pore-free, crackle；
Viscosity of material: complex viscosity is to meet 3D printing demand within the scope of 200-250Pas；
Mechanical property: tensile strength maintains an equal level within the scope of 10-12MPa with existing thin-film material tensile strength.
In order to further appreciate that the contents of the present invention, the present invention is described in detail in conjunction with the embodiments.
Embodiment:
(1) precursor preparation
Solid electrolyte presoma includes 3 kinds of material components, the polycyclic oxygen of lithium trifluoromethanesulp,onylimide, molecular weight 300,000 Ethane and with vinylidene fluoride-hexafluoropropylene copolymer, is conduction lithium salts with bis trifluoromethyl sulfimide lithium, polyethylene oxide is Polymer dielectric, vinylidene fluoride-hexafluoropropylene copolymer are reinforcing material, and 3 kinds of materials are dusty material, pass through machinery Mixing, is sufficiently mixed three kinds of materials, form powder-mixed material, lithium salts, polyethylene oxide and biasfluoroethylene-hexafluoropropylene Mass ratio is 5/15/4.Specific steps are successively are as follows: weigh polyethylene oxide powder and are placed in uncovered beaker, add load weighted Vinylidene fluoride-hexafluoropropylene copolymer powder, is stirred using blender, makes the two uniformly mixing ten minutes.Double three are weighed again Methyl fluoride sulfimide lithium powder is put into same uncovered beaker, and dehydrated alcohol, dehydrated alcohol and powder mixture is then added Ratio be 5ml/g, persistently stirred using blender 20 minutes, bis trifluoromethyl sulfimide lithium powder made to be dissolved in nothing In water-ethanol, while it is well dispersed in polyethylene oxide and biasfluoroethylene-hexafluoropropylene in dehydrated alcohol.After the completion of stirring, Solution is warming up between 45~55 DEG C, dehydrated alcohol is slowly evaporated to the blocky solid content of acquisition, then solid content is sufficiently sheared, Vacuum drying, it is final to obtain particulate electrolytic matter 3D printing persursor material.
(2) prepared by silk material
Graininess persursor material is sent into screw extruder, carries out blending throwing, screw extruder revolving speed 100r/min, 200 DEG C of throwing temperature, molding equipment internal vacuum 0.02MPa is mounted at outlet of extruder, linear velocity and spiral shell by one Silk material is coiled by the consistent filament winding machine of bar extruder extruded velocity, is used for subsequent solid electrolyte 3D printing.
(3) silk material quality evaluation
The macro microcosmic forming defect situation of material is characterized using electron microscope and Stereo microscope, is surveyed using stress rheometer Viscosity of material is tried, cupping machine test material mechanical property is used.The quality knot obtained by above several characterization test methods Fruit is as follows:
Macroscopic view molding: silk material diameter meets printing and requires within the scope of 1.4-1.7mm, and macroscopic view molding is good, and microscope is seen Examine lower pore-free, crack defect；
Microcosmic molding: under electron microscope observation, the defects of internal object mutually has good uniformity, pore-free, crackle；Material is viscous Degree: complex viscosity is to meet 3D printing demand within the scope of 200-250Pas；
Mechanical property: tensile strength maintains an equal level within the scope of 10-12MPa with existing thin-film material tensile strength.

Claims (2)

1. a kind of preparation method of the 3D printing silk material of solid electrolyte, which is characterized in that include the following steps,
Step 1, the composition of 3D printing silk material persursor material are as follows: the polycyclic oxygen of lithium trifluoromethanesulp,onylimide, molecular weight 300,000 Ethane and with vinylidene fluoride-hexafluoropropylene copolymer, 3 components are dusty material, and taking mass ratio is 5:13~16:3~6；
Step 2,3D printing silk material persursor material preparation, the polyethylene oxide powder of load weighted molecular weight 300,000 is placed in In uncovered beaker, load weighted vinylidene fluoride-hexafluoropropylene copolymer powder is added, is stirred using blender, makes the two Even mixing ten minutes；Bis trifluoromethyl sulfimide lithium powder is weighed again to be put into same uncovered beaker, is then added anhydrous The ratio of ethyl alcohol, dehydrated alcohol and powder mixture is 5ml/g~6ml/g, is persistently stirred using blender 20 minutes, makes double three Methyl fluoride sulfimide lithium powder is dissolved in dehydrated alcohol, while making polyethylene oxide and biasfluoroethylene-hexafluoropropylene It is well dispersed in dehydrated alcohol；After the completion of stirring, solution is heated up between 45~55 DEG C, dehydrated alcohol is slowly evaporated and is obtained Blocky solid content is obtained, then solid content is sufficiently sheared, is dried in vacuo, it is final to obtain particulate electrolytic matter 3D printing presoma material Material；
Silk material preparation: graininess persursor material is sent into screw extruder, carries out blending throwing, screw extruder by step 3 Revolving speed 100r/min~120r/min, 200 DEG C~220 DEG C of throwing temperature, molding equipment internal vacuum is lower than 0.02MPa, leads to It crosses one to be mounted at outlet of extruder, linear velocity and the consistent filament winding machine of screw extruder extruded velocity coil silk material Come, is used for subsequent solid electrolyte 3D printing.
2. a kind of preparation method of the 3D printing silk material of solid electrolyte, which is characterized in that in step 1, trimethyl fluoride sulfonyl is sub- Amine lithium, the polyethylene oxide of molecular weight 300,000 and with vinylidene fluoride-hexafluoropropylene copolymer, most preferably taking mass ratio is 5:15:4.
CN201910645436.9A 2019-07-17 2019-07-17 A kind of preparation method of the 3D printing silk material of solid electrolyte Pending CN110497595A (en)

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Publication number Priority date Publication date Assignee Title
CN111326786A (en) * 2020-03-19 2020-06-23 珠海冠宇电池有限公司 Composite solid electrolyte with three-dimensional penetrating structure and all-solid-state lithium ion battery
CN111554975A (en) * 2020-05-11 2020-08-18 珠海冠宇电池股份有限公司 Solid electrolyte, preparation method thereof and lithium ion battery
CN112331912A (en) * 2020-11-09 2021-02-05 贵州梅岭电源有限公司 Preparation method of gel electrolyte

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