All-solid-state battery reaction chamber for in-situ XRD and Raman test and test method

Abstract

The invention belongs to the technical field of batteries, and particularly relates to an all-solid-state battery reaction chamber for in-situ XRD and Raman test and a test method. The solid-state battery reaction chamber comprises a working electrode cover, a solid-state battery mold shell and a counter electrode holder which are sequentially connected from top to bottom; the working electrode cover comprises a cover body and a working electrode lead, the working electrode lead is connected with the cover body, and the cover body is provided with a test window for XRD test or Raman test; the solid-state battery mold shell is provided with a concave mold cavity, and a positive electrode, an electrolyte and a negative electrode of a solid-state battery can be assembled; and a metal rod matched with the concave mold cavity is arranged on the counter electrode holder, and an electrode outgoing line is arranged in the lower part of the counter electrode holder. The preparation method has the advantages of simplicity, rapidness, compact structure, small size, good equipment universality and reusability; and the obtained spectrum has the characteristics of high signal-to-noise ratio, low off-axis error, no impure phase peak interference, uniform working electrode current density, accurate test potential, high capacity retention ratio in long circulation and the like.

Description

technical field

[0001] The invention belongs to the technical field of batteries, and in particular relates to an all-solid-state battery reaction chamber and a testing method for in-situ XRD and Raman testing. Background technique

[0002] With the continuous deepening of research on lithium-ion batteries, new materials and systems such as NCM (ternary), NCA, hard carbon, SiO, silicon carbon, and lithium anodes continue to emerge. It is of great significance to optimize the design of positive and negative electrode materials to study the phase and structure evolution of related positive and negative electrode materials during the charge and discharge process.

[0003] At present, it is of great significance to use non-flammable inorganic solid-state electrolytes to replace flammable and explosive commercial electrolytes to realize high-safety lithium battery designs. On the one hand, the sulfide system Li with high conductivity 2 S-P 2 S 5 Based on the binary system (su...

Examples

Embodiment 1

[0061] In situ XRD detection of solid-state battery assembly

[0062] like Figure 2-3 As shown, put the upper mold core 1 into the die cavity 2 of the solid-state battery mold case 2, and then add 80mg Li to the die cavity 6 P.S. 5 C1, put the pressure ring 3 on the counter electrode seat 4, and then put the counter electrode seat 4 into the die cavity of the solid-state battery mold case 2. The solid battery mold equipped with the upper mold core 1 and the counter electrode holder 4 is placed in the inner cavity of the hydraulic press, and the solid electrolyte is pressed into thin sheets under a pressure of 2 MPa.

[0063] like Figure 3-4 As shown, carefully remove the counter electrode holder 4, and put 10mg composite positive electrode material (LiCoO 2 with Li 6 P.S. 5 Cl mass ratio 7:3) was added into the die cavity of the solid-state battery mold shell 2, evenly filled on the surface of the electrolyte, and the electrode pressure ring 5 was put on the counter el...

Embodiment 2

[0068] In situ XRD detection of solid-state battery assembly

[0069] Put the upper mold core 1 into the die cavity of the solid-state battery mold case 2, and then add 80mgLi 10 GeP 2 S 12 , put the pressure ring 3 on the counter electrode seat 4, and then put the counter electrode seat 4 into the die cavity of the solid state battery mold case 2. The solid battery mold equipped with the upper mold core 1 and the counter electrode holder 4 is placed in the inner cavity of the hydraulic press, and the solid electrolyte is pressed into thin sheets under a pressure of 2 MPa.

[0070] Carefully take off the opposite electrode seat 4, put 10mg composite positive electrode material (LiCoO 2 with Li 10 GeP 2 S 12 mass ratio 7:3) into the die cavity of the solid-state battery mold case 2, evenly spread on the surface of the electrolyte, put the electrode pressure ring 5 on the counter electrode seat 4, and then under the pressure of 8Mpa, the positive electrode material and the...

Embodiment 3

[0074] In situ Raman detection of solid-state battery assembly

[0075] Put the upper mold core 1 into the die cavity of the solid-state battery mold case 2, and then add 80mgLi 6 P.S. 5 C1, put the pressure ring 3 on the counter electrode seat 4, and then put the counter electrode seat 4 into the die cavity of the solid-state battery mold case 2. The solid battery mold equipped with the upper mold core 1 and the counter electrode holder 4 is placed in the inner cavity of the hydraulic press, and the solid electrolyte is pressed into thin sheets under a pressure of 2 MPa. Carefully take off the opposite electrode seat 4, put 10mg composite positive electrode material (LiCoO 2 with Li 6 P.S. 5 Cl mass ratio 7:3) was added to the cavity 2 of the die of the shell, evenly filled on the surface of the electrolyte, and the electrode pressure ring 5 was put on the counter electrode seat 4, and then the positive electrode material and the solid electrolyte were tightly pressed und...

technical field

[0001] The invention belongs to the technical field of batteries, and in particular relates to an all-solid-state battery reaction chamber and a testing method for in-situ XRD and Raman testing. Background technique

[0002] With the continuous deepening of research on lithium-ion batteries, new materials and systems such as NCM (ternary), NCA, hard carbon, SiO, silicon carbon, and lithium anodes continue to emerge. It is of great significance to optimize the design of positive and negative electrode materials to study the phase and structure evolution of related positive and negative electrode materials during the charge and discharge process.

[0003] At present, it is of great significance to use non-flammable inorganic solid-state electrolytes to replace flammable and explosive commercial electrolytes to realize high-safety lithium battery designs. On the one hand, the sulfide system Li with high conductivity 2 S-P 2 S 5 Based on the binary system (su...

Examples

Embodiment 1

[0061] In situ XRD detection of solid-state battery assembly

[0062] like Figure 2-3 As shown, put the upper mold core 1 into the die cavity 2 of the solid-state battery mold case 2, and then add 80mg Li to the die cavity 6 P.S. 5 C1, put the pressure ring 3 on the counter electrode seat 4, and then put the counter electrode seat 4 into the die cavity of the solid-state battery mold case 2. The solid battery mold equipped with the upper mold core 1 and the counter electrode holder 4 is placed in the inner cavity of the hydraulic press, and the solid electrolyte is pressed into thin sheets under a pressure of 2 MPa.

[0063] like Figure 3-4 As shown, carefully remove the counter electrode holder 4, and put 10mg composite positive electrode material (LiCoO 2 with Li 6 P.S. 5 Cl mass ratio 7:3) was added into the die cavity of the solid-state battery mold shell 2, evenly filled on the surface of the electrolyte, and the electrode pressure ring 5 was put on the counter el...

Embodiment 2

[0068] In situ XRD detection of solid-state battery assembly

[0069] Put the upper mold core 1 into the die cavity of the solid-state battery mold case 2, and then add 80mgLi 10 GeP 2 S 12 , put the pressure ring 3 on the counter electrode seat 4, and then put the counter electrode seat 4 into the die cavity of the solid state battery mold case 2. The solid battery mold equipped with the upper mold core 1 and the counter electrode holder 4 is placed in the inner cavity of the hydraulic press, and the solid electrolyte is pressed into thin sheets under a pressure of 2 MPa.

[0070] Carefully take off the opposite electrode seat 4, put 10mg composite positive electrode material (LiCoO 2 with Li 10 GeP 2 S 12 mass ratio 7:3) into the die cavity of the solid-state battery mold case 2, evenly spread on the surface of the electrolyte, put the electrode pressure ring 5 on the counter electrode seat 4, and then under the pressure of 8Mpa, the positive electrode material and the...

Embodiment 3

[0074] In situ Raman detection of solid-state battery assembly

[0075] Put the upper mold core 1 into the die cavity of the solid-state battery mold case 2, and then add 80mgLi 6 P.S. 5 C1, put the pressure ring 3 on the counter electrode seat 4, and then put the counter electrode seat 4 into the die cavity of the solid-state battery mold case 2. The solid battery mold equipped with the upper mold core 1 and the counter electrode holder 4 is placed in the inner cavity of the hydraulic press, and the solid electrolyte is pressed into thin sheets under a pressure of 2 MPa. Carefully take off the opposite electrode seat 4, put 10mg composite positive electrode material (LiCoO 2 with Li 6 P.S. 5 Cl mass ratio 7:3) was added to the cavity 2 of the die of the shell, evenly filled on the surface of the electrolyte, and the electrode pressure ring 5 was put on the counter electrode seat 4, and then the positive electrode material and the solid electrolyte were tightly pressed und...

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