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A kind of preparation method of inorganic solid electrolyte membrane/electrode composite material

An inorganic electrolyte and inorganic solid technology, which is used in the manufacture of electrolyte batteries, electrolyte layer coatings, non-aqueous electrolyte batteries, etc., can solve the problems of unsuitability for continuous, large-scale production, low production efficiency, and high equipment requirements, and achieve film Good effect, uniform thickness, simple preparation and operation

Active Publication Date: 2016-02-24
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] For the film-forming methods of inorganic solid electrolyte materials in the prior art (such as high-pressure pressing, magnetron sputtering and laser pulse deposition, etc.), there are poor film-forming effects, high requirements for equipment, low production efficiency, and are not suitable for continuous and large-scale production. However, the object of the present invention is to provide a method for preparing an inorganic solid electrolyte membrane / electrode composite material with stable and compact solid electrolyte membrane and good electrochemical performance. The method is simple to operate, mild in conditions and high in production efficiency. High, easy to realize industrial production

Method used

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Experimental program
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Effect test

Embodiment 1

[0018] Step 1: Synthesis of sulfide (Li 8 P 2 S 9 ) Inorganic solid electrolyte, according to P 2 S 5 : Li 2 Ratio of S=25:75 (molar ratio) Weigh raw materials, grind and mix in an argon glove box. Put the uniformly mixed raw materials into a quartz tube furnace for sintering to obtain Li 8 P 2 S 9 powder (such as figure 1 shown in a). The sintering temperature is 550°C, and the sintering time is 12h.

[0019] The second step: prepare electrolyte ink, weigh 1.5gLi 8 P 2 S 9 Powder, dissolve the powder in 5mL N,N-dimethylformamide dispersant, add 0.6g polyvinylidene fluoride binder, ultrasonic frequency 50KHz, ultrasonic time 8min, get the suspension and let it stand for 120min to get the upper layer uniformly dispersed Post-stabilized inks (such as figure 1 shown in b).

[0020] The third step: inkjet coating to prepare all-solid-state lithium-ion batteries, weigh a certain amount of electrolyte ink, add it to the printer ink cartridge, and print directly on the...

Embodiment 2

[0022] Use 6g of the same electrolyte powder as in Example 1, dissolve the powder in 3mL of tetrahydrofuran dispersant, add 0.2g of polyvinylidene fluoride binder, ultrasonic frequency 100KHz, ultrasonic time 10min, obtain a suspension and let it stand for 120min to obtain the upper layer Stable ink after even dispersion. pre-prepared with LiMn 2 o 4 As the active material, polyvinylidene fluoride is used as the binder of the positive electrode sheet. The electrolyte ink is sprayed on the positive electrode sheet, and the drying temperature is 100 ° C for 12 hours to obtain a dense and uniform electrolyte membrane with a thickness of about 60 μm. The electrolyte membrane / Electrode composite material, assembled into a button battery, after 100 cycles at 25°C and 1C, the charging specific capacity is 120mAhg -1 , the specific discharge capacity is 118mAhg -1 , Coulombic efficiency is 98.3%.

Embodiment 3

[0024] The first step: the inorganic solid electrolyte was synthesized by high-energy ball milling, and lithium sulfide and phosphorus sulfide were mixed according to the stoichiometric ratio in the glove box to control the Li 2 S:P 2 S 5 =3:1 molar ratio mixed, sealed into a ball mill jar full of argon atmosphere. Use a planetary ball mill for mixing. In order to obtain the best results, the large ball is used to counterweight and smash the sample and disperse the small ball. Agate balls of three sizes (d=10mm)×6 / grain and small (d=6mm)×20 / grain are used together, and 2g of sulfide powder material obtained by proportioning and weighing and agate balls of three different sizes are added into a ball mill for dry grinding. The ball milling parameters are set to a speed of 200rmin -1 , the ball milling time is 12h, and Li 8 P 2 S 9 powder.

[0025] Weigh 3g of the inorganic electrolyte powder, dissolve the powder in 3mL of anhydrous hydrazine dispersant, add 0.3g of polye...

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Abstract

The invention discloses a method for preparing an inorganic solid electrolyte membrane / electrode composite material. The method is to disperse an inorganic solid electrolyte powder material and a binder in a solvent by ultrasonic waves to form a stable dispersion system. After standing still, take the upper layer The clear solution is added to the printer ink cartridge, printed onto the electrode sheet by inkjet, or directly coated on the electrode sheet, dried, and an inorganic solid electrolyte film layer is formed on the electrode sheet, that is, a stable, dense, and electrochemical performance is obtained. The electrolyte / electrode composite material of a good inorganic solid electrolyte membrane layer; the method is simple in operation, mild in conditions, high in production efficiency, and easy to realize industrial production.

Description

technical field [0001] The invention relates to a preparation method of an inorganic solid electrolyte membrane / electrode composite material, belonging to the field of lithium batteries. Background technique [0002] Lithium-ion batteries have the advantages of high working voltage, high energy density, small size, and no memory effect, making them one of the energy sources with the most development potential. At present, it has been used in many fields such as military defense, electric vehicles, portable digital equipment, etc., and the requirements for its performance are getting higher and higher. Inorganic all-solid-state lithium-ion batteries have high safety performance and energy density, and are one of the most potential battery systems in the future energy field. The film formation and battery preparation of inorganic electrolytes are currently mainly achieved by high-pressure pressing, magnetron sputtering, and laser pulse deposition. However, these methods requi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/058
CPCH01M4/0407H01M10/0525H01M10/058Y02E60/10Y02P70/50
Inventor 刘晋刘业翔朱凯张锦林月
Owner CENT SOUTH UNIV
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