CN107611338A - The preparation method of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property - Google Patents

The preparation method of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property Download PDF

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Publication number
CN107611338A
CN107611338A CN201710745118.0A CN201710745118A CN107611338A CN 107611338 A CN107611338 A CN 107611338A CN 201710745118 A CN201710745118 A CN 201710745118A CN 107611338 A CN107611338 A CN 107611338A
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China
Prior art keywords
snap
check
electrical property
beaker
type cell
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CN201710745118.0A
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Chinese (zh)
Inventor
王凤
邱平
马延会
邹积英
温炜炜
张红意
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Jinchuan Lanzhou Science And Technology Park Co Ltd
Jinchuan Group Co Ltd
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Jinchuan Lanzhou Science And Technology Park Co Ltd
Jinchuan Group Co Ltd
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Priority to CN201710745118.0A priority Critical patent/CN107611338A/en
Publication of CN107611338A publication Critical patent/CN107611338A/en
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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Abstract

The preparation method of the invention for disclosing Snap-type cell positive slurry used in a kind of check and evaluation material electrical property, 1)Positive electrode, conductive agent, binding agent and solvent are weighed respectively;2)Batch mixing:Positive electrode, conductive agent, binding agent, the solvent weighed up is poured into 50mL beakers or conical flask, and the material in beaker or conical flask is tentatively stirred with glass bar;3)Magnetic agitation heats, and completes to obtain anode sizing agent after the completion of heating stirring, can be come into operation after cooling.Beneficial effect is:Preparing slurry using this method only needs a small amount of material to reach the purpose that battery material detects.It is less to be related to equipment, process is simple, easily operated, and cost is relatively low, puts and ends to waste, economic and environment-friendly, convenient and safe.

Description

The preparation method of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property
Technical field
The invention belongs to lithium-ion button battery production field, is related to lithium ion used in a kind of check and evaluation material electrical property The method that button cell makes anode sizing agent.
Background technology
Lithium-ion button battery is simple and convenient due to assembling, and involved raw material and equipment is less, and cost is relatively low, detects Journey is also relatively quick, efficient, and therefore, button cell turns into the Main Means of lithium ion battery electrode material electrical performance evaluation at present. Detain the anode sizing agent dispensing in electric assembling process and account for key effect, influence of the blank preparation technicses to battery performance is very big, right and wrong Often important link., need to be by positive active material used in lithium-ion button battery, conductive agent, viscous in the preparation of anode sizing agent Knot agent and solvent mix by a certain percentage, prepare key and are to be uniformly dispersed, modest viscosity.But the raw material phase being related to due to button electricity To less, there is no special small-sized off-the-shelf hardware to sell in terms of slurry preparation, each research unit is mostly using homemade simple Coating experimental provision detain the preparation of electric anode sizing agent.The raw material proportioning being related to when prepared by slurry is also uneven, involved And equipment and equipment be also all not quite similar.Some units cause the slurry prepared because material and pulping equipment are less supporting Far more than the amount needed for actual film-making, so, remaining slurry would have to directly outwell, and causes unnecessary material Waste.In addition, carry out to carry out being equipped with excessive PVDF binding agents during slurry preparation every time temporarily, pole piece again will be surplus after preparing Remaining slurry material is outwelled, and is not only added time cost simultaneously and is caused material waste, and all without will slurry when mostly prepared by slurry Material heating, causes slurry each component to bond bad, pole piece shedding, the decarburization of preparation, so as to influence the performance of made battery.Alright Slurry manufacture craft, it should be while properties of product are lifted, reduce the time in the cost and production process of raw material as far as possible Cost.
The content of the invention
The present invention seeks to propose that a kind of cost is low and timesaving check and evaluation material electrical property used in Snap-type cell positive The preparation method of slurry.
The technical solution adopted by the present invention is:The system of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property Preparation Method, step are:1)Weigh:Positive electrode, conductive agent, binding agent and solvent, wherein positive electrode, conduction are weighed respectively Agent, the quality of binding agent are not higher than 10g, and positive electrode, conductive agent, the mass ratio of binding agent are 80~92:4~10:4~9, Solvent load is 1.1~1.3 times of positive active material, conductive agent and binding agent gross mass;
2)Batch mixing:Positive electrode, the conductive agent weighed up, which pours into, to be cleaned and in the beaker or conical flask dried, beaker or conical flask Capacity is 50mL, then the binding agent weighed up, solvent are poured into the beaker or conical flask, with glass bar by beaker or conical flask Material tentatively stir;
3)Stirring:Beaker or conical flask opening aluminium foil are covered and be put on magnetic force heating stirrer, beaker after preliminary stirring Or magneton is put into conical flask, it is with fixture that beaker or conical flask is stable, open magnetic force heating stirrer, adjustment stirring frequency and Heating-up temperature, the time that magnetic force heating stirrer is opened is recorded, magnetic force heating stirrer power supply, thing are closed after the completion of heating stirring Material stirring is completed to obtain anode sizing agent, can be come into operation after cooling.
The positive electrode is at least one of ternary material, cobalt acid lithium, LiFePO4, LiMn2O4, nickel cobalt lithium aluminate.
The conductive agent is selected from least one of acetylene black, superfine carbon black, CNT.
The binding agent is Kynoar(PVDF), the solvent is 1-METHYLPYRROLIDONE(NMP).
Further, the Kynoar(PVDF)For solubilizer 1-METHYLPYRROLIDONE(NMP)Prepare, and fill in advance Sealed in dark glass bottle standby.
Preferably, the mass ratio of the Kynoar and 1-METHYLPYRROLIDONE is 1:9.The positive electrode is in gained Mass percentage content in anode sizing agent is 80%~93%;Mass percent of the conductive agent in gained anode sizing agent contains Measure as 4%~10%;Mass percentage content of the binding agent in gained anode sizing agent is 3%~10%.
Preferably, mass percentage content of the conductive agent in gained anode sizing agent is 7%~10%.
Step 3)Middle stirring frequency is 120r/min, and the temperature that slurry heats when preparing is 40~55 DEG C, during heating stirring Between be 0.5~2h.Preferably, heating-up temperature is 50 DEG C, and the heating stirring time is 1h.
The beneficial effects of the invention are as follows:Preparing slurry using this method only needs a small amount of material to reach battery material The purpose of detection.It is less to be related to equipment, process is simple, easily operated, and cost is relatively low, puts and ends to waste, economic and environment-friendly, convenient peace Entirely.In addition binding agent can save the time for individually preparing binding agent again, improve operating efficiency again to prepare in advance.The present invention In pulping process by the way of heating, abundant quickly bonding, the pole piece of preparation for being advantageous to each component in slurry are processed It is good without demoulding, decarburization phenomenon, processing characteristics in journey.The slurry prepared with the pulping process of the present invention is processed into group after positive plate The button cell detection data of dress almost approach with full battery, can be widely used in the small tests such as major colleges and universities, scientific research institutions Room and factory laboratory.
Embodiment
Embodiment 1
(1)Tertiary cathode material LiNi5Co2Mn3O2, conductive agent acetylene black, binding agent PVDF mass ratioes be 85:8:7, claim respectively Measure LiNi5Co2Mn3O2Material 2.55g, acetylene black 0.24g, binding agent 2.1g, solvent 4g, wherein binding agent PVDF quality are dense Spend for 10%.Tertiary cathode material and acetylene black poured into after weighing up one clean in advance and beaker that the capacity dried is 50mL or In conical flask, then the solvent NMP weighed up and binding agent PVDF poured into beaker or conical flask.With glass bar by beaker or taper Mixture in bottle tentatively stirs, then gently inserts the small magneton of wash clean in advance in beaker or conical flask.It is to be confirmed After all materials are put well, beaker or conical flask opening aluminium foil are covered and are positioned over magnetic force heating stirrer centre, used Fixture on puddle support is steady by beaker or taper bottle clip.It is then turned on magnetic force heating stirrer, stirring frequency 120r/min, slurry The temperature that material heats when preparing is 40~55 DEG C, the time that record magnetic force heating stirrer is opened, power supply is closed after one hour, starched Material stirring is completed.It can be used to make button cell after cooling down Deng material oar.
Embodiment 2
(2)Cobalt acid lithium, conductive agent superfine carbon black, binding agent mass ratio are 90:6:4, cobalt acid lithium material 2.7g, ultra-fine is weighed respectively Carbon black 0.18g, binding agent 2g and solvent 4g, wherein binding agent PVDF mass concentration are that 6% (binding agent is PVDF solubilizers NMP It is configured in advance, actually the amount containing PVDF is 1.2g in 2gPVDF binding agents).Cobalt acid lithium material and superfine carbon black fall after weighing up Entering one, wash clean and the capacity dried are then the solvent NMP and binding agent that will be weighed up in 50mL beaker or conical flask in advance PVDF is poured into beaker or conical flask.Mixture in beaker or conical flask is tentatively stirred with glass bar, then will gently be carried The small magneton of preceding wash clean is inserted in beaker or conical flask.After all materials to be confirmed are put well, by beaker or conical flask opening Covered with aluminium foil and be positioned over magnetic force heating stirrer centre, it is with the fixture on puddle support that beaker or taper bottle clip is steady.So Magnetic force heating stirrer, stirring frequency 120r/min are opened afterwards, and the temperature that slurry heats when preparing is 40~55 DEG C, records magnetic The time that power heating stirrer is opened, power supply is closed after 1.5 hours, slurry agitation is completed.It can be used to after being cooled down Deng material oar Make button cell.
Embodiment 3
(3)LiMn2O4 active material, conductive agent acetylene black, binding agent mass ratio are 88:8:4, LiMn2O4 activity material is weighed respectively Material, acetylene black, PVDF binding agents and nmp solvent 2.64g, 0.24g, 2g, 3.6g, wherein binding agent PVDF mass concentration are 6% (Binding agent is prepared in advance with solvent NMP, and actually the amount containing PVDF is 1.2g in 2gPVDF binding agents.Although having used solvent, But quantity of solvent is seldom, to soak slurry effect it is limited, so again individually addition solvent NMP, can so allow material into Slurry).LiMn2O4 active material and acetylene black are poured into after weighing up in the beaker or conical flask for shifting to an earlier date wash clean and drying, then will be claimed Good solvent NMP and binding agent PVDF is poured into beaker or conical flask.With glass bar by the beginning of the mixture of prefabricated slurry in container Step stirs, then gently inserts the small magneton that the capacity of wash clean in advance is 50mL in beaker or conical flask.Institute to be confirmed After thering is material to put well, beaker or conical flask opening aluminium foil are covered and are positioned over magnetic force heating stirrer centre, with stirring The fixture mixed on frame is steady by beaker or taper bottle clip.It is then turned on magnetic force heating stirrer, stirring frequency 120r/min, slurry The temperature heated during preparation is 40~55 DEG C, the time that record magnetic force heating stirrer is opened, power supply, slurry is closed after one hour Stirring is completed.It can be used to make button cell after cooling down Deng material oar.
Embodiment 4
(4)Lithium nickel cobalt dioxide active material, conductive agent CNT, binding agent mass ratio are 92:4:4, lithium nickel cobalt dioxide is weighed respectively Material, CNT, binding agent and solvent 2.76g, 0.12g, 2g, 3.8g, wherein binding agent PVDF mass concentration are 6%.Nickel Cobalt acid lithium active material and CNT pour into beaker or the taper that wash clean and the capacity dried are 50mL in advance after weighing up In bottle, then the solvent NMP weighed up and binding agent PVDF poured into beaker or conical flask.With glass bar by beaker or conical flask Mixture tentatively stir, then gently the small magneton of wash clean in advance is inserted in beaker or conical flask.It is to be confirmed all After material is put well, beaker or conical flask opening aluminium foil are covered and are positioned over magnetic force heating stirrer centre, with stirring Fixture on frame is steady by beaker or taper bottle clip.It is then turned on magnetic force heating stirrer, stirring frequency 120r/min, slurry system The temperature heated when standby is 40~55 DEG C, the time that record magnetic force heating stirrer is opened, closes power supply after two hours, slurry stirs Mix and complete.It can be used to make button cell after cooling down Deng material oar.

Claims (10)

  1. A kind of 1. preparation method of Snap-type cell positive slurry used in check and evaluation material electrical property, it is characterised in that:1)Weigh: Positive electrode, conductive agent, binding agent and solvent, wherein positive electrode, conductive agent, the quality of binding agent is weighed respectively to be not higher than 10g, positive electrode, conductive agent, the mass ratio of binding agent are 80~92:4~10:4~9, solvent load be positive active material, 1.1~1.3 times of conductive agent and binding agent gross mass;
    2)Batch mixing:Positive electrode, the conductive agent weighed up, which pours into, to be cleaned and in the beaker or conical flask dried, beaker or conical flask Capacity is 50mL, then the binding agent weighed up, solvent are poured into the beaker or conical flask, with glass bar by beaker or conical flask Material tentatively stir;
    3)Stirring:Beaker or conical flask opening aluminium foil are covered and be put on magnetic force heating stirrer, beaker after preliminary stirring Or magneton is put into conical flask, it is with fixture that beaker or conical flask is stable, open magnetic force heating stirrer, adjustment stirring frequency and Heating-up temperature, the time that magnetic force heating stirrer is opened is recorded, magnetic force heating stirrer power supply, thing are closed after the completion of heating stirring Material stirring is completed to obtain anode sizing agent, can be come into operation after cooling.
  2. 2. the preparation side of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property according to claim 1 Method, it is characterised in that:The positive electrode be ternary material, cobalt acid lithium, LiFePO4, LiMn2O4, in nickel cobalt lithium aluminate extremely Few one kind.
  3. 3. the preparation side of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property according to claim 1 Method, it is characterised in that:The conductive agent is selected from least one of acetylene black, superfine carbon black, CNT.
  4. 4. the preparation method of Snap-type cell positive slurry used in check and evaluation material electrical property according to claim 1, its It is characterised by:The binding agent is Kynoar, and the solvent is 1-METHYLPYRROLIDONE.
  5. 5. the preparation side of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property according to claim 4 Method, it is characterised in that:The Kynoar is that solubilizer 1-METHYLPYRROLIDONE is prepared in advance, and loaded in dark glass bottle Seal standby.
  6. 6. the preparation side of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property according to claim 5 Method, it is characterised in that:The mass ratio of the Kynoar and 1-METHYLPYRROLIDONE is 1:9.
  7. 7. the preparation side of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property according to claim 1 Method, it is characterised in that:Mass percentage content of the positive electrode in gained anode sizing agent is 80%~93%;The conduction Mass percentage content of the agent in gained anode sizing agent is 4%~10%;Quality of the binding agent in gained anode sizing agent Degree is 3%~10%.
  8. 8. the preparation side of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property according to claim 7 Method, it is characterised in that:Mass percentage content of the conductive agent in gained anode sizing agent is 7%~10%.
  9. 9. the preparation side of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property according to claim 1 Method, it is characterised in that:Step 3)Middle stirring frequency is 120r/min, and the temperature that slurry heats when preparing is 40~55 DEG C, heating Mixing time is 0.5~2h.
  10. 10. the preparation side of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property according to claim 9 Method, it is characterised in that:Heating-up temperature is 50 DEG C, and the heating stirring time is 1h.
CN201710745118.0A 2017-08-25 2017-08-25 The preparation method of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property Pending CN107611338A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3951921A1 (en) * 2020-08-05 2022-02-09 SK Innovation Co., Ltd. Fabrication method of positive electrode for secondary battery and secondary battery including the positive electrode

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105932273A (en) * 2016-05-29 2016-09-07 合肥国轩高科动力能源有限公司 Preparation method for cathode slurry of lithium ion battery
CN106058252A (en) * 2016-08-17 2016-10-26 江苏金坛绿能新能源科技有限公司 Lithium ion battery cathode slurry and preparation method thereof
CN106299269A (en) * 2016-08-18 2017-01-04 山东精工电子科技有限公司 A kind of lithium ion battery anode glue size preparation method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105932273A (en) * 2016-05-29 2016-09-07 合肥国轩高科动力能源有限公司 Preparation method for cathode slurry of lithium ion battery
CN106058252A (en) * 2016-08-17 2016-10-26 江苏金坛绿能新能源科技有限公司 Lithium ion battery cathode slurry and preparation method thereof
CN106299269A (en) * 2016-08-18 2017-01-04 山东精工电子科技有限公司 A kind of lithium ion battery anode glue size preparation method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3951921A1 (en) * 2020-08-05 2022-02-09 SK Innovation Co., Ltd. Fabrication method of positive electrode for secondary battery and secondary battery including the positive electrode

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