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Preparation method of composite solid electrolyte

A solid electrolyte and preparation process technology, which is applied in the field of composite solid electrolyte preparation to achieve uniform deposition, low electronic conductivity, and ease of volume effect.

Pending Publication Date: 2022-07-01
WUHAN MARINE ELECTRIC PROPULSION RES INST CHINA SHIPBUILDING IND CORP NO 712 INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, numerous research works have shown that the problem of lithium dendrites still exists in solid-state batteries, and in some solid-state electrolytes with ultra-high mechanical strength, the speed of dendrite growth piercing the electrolyte is faster than in liquid batteries, which shows that Mechanical strength is not the only factor affecting dendrite problems

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  • Preparation method of composite solid electrolyte

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Embodiment 1

[0027] refer to figure 1 As shown, the present invention discloses a method for preparing a composite solid-state electrolyte that inhibits the growth of lithium dendrites. The steps are as follows:

[0028] (1) The surface treatment of the electrolyte is carried out by a laser cleaning method, and the solid electrolyte is cleaned by a high-energy nanosecond laser.

[0029] (2) Put the solid electrolyte into the quartz tube of the plasma-enhanced chemical vapor deposition device, and evacuate the quartz tube to 4Pa.

[0030] (3) Turn on the heating, heat from room temperature to 750°C, the heating rate is 2°C / min, and the temperature is kept for 4h.

[0031] (4) A mixture of nitrogen, hydrogen and methane (flow ratio 2:1:1) was introduced, and the pressure and temperature in the tube were 50pa. The hydrogen flow was 10 mL / min.

[0032] (5) Turn on the radio frequency plasma source and slowly adjust the high power to 300W. Growth time was controlled within 30 minutes.

[0...

Embodiment 2

[0042] A preparation method of a composite solid electrolyte of the present embodiment, the steps are as follows:

[0043] (1) The surface of the electrolyte is treated by a laser cleaning method, and the solid electrolyte is cleaned by a high-energy nanosecond laser.

[0044] (2) Put the solid electrolyte into the quartz tube of the plasma-enhanced chemical vapor deposition device, and evacuate the quartz tube to 5Pa.

[0045] (3) Turn on the heating, heat from room temperature to 800°C, the heating rate is 3°C / min, and the temperature is kept for 5h.

[0046] (4) A mixture of nitrogen, hydrogen and methane (flow ratio 2:1:1) was introduced, and the pressure and temperature in the tube were 50pa. The hydrogen flow was 15 mL / min.

[0047] (5) Turn on the radio frequency plasma source and slowly adjust the high power to 200W. Growth time was controlled within 60 minutes.

[0048] (6) Turn off the radio frequency plasma, stop feeding hydrogen and methane, keep feeding nitrog...

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Abstract

The invention discloses a preparation method of a composite solid electrolyte for inhibiting growth of lithium dendrites, which comprises the following steps of: heating a solid electrolyte in a plasma enhanced chemical vapor deposition device, introducing a mixed gas of nitrogen, hydrogen and methane to start a radio frequency plasma source, stopping introducing hydrogen and methane after closing radio frequency plasma, and cooling to room temperature to obtain the composite solid electrolyte for inhibiting growth of lithium dendrites. The method comprises the following steps: introducing nitrogen, cooling, taking out a sample, selecting a pure copper target, pre-sputtering to clean the surface of the target, mixing nitrogen and argon by adopting a direct current sputtering mode, preparing the sample and metal lithium into a symmetrical battery after the growth reaction is finished, and reacting the sample with Li < + > to generate Li3N and copper nanoparticles in the charging and discharging process, the copper nanoparticles which are well dispersed form a uniform electric field at an interface, and graphene is used as a three-dimensional structure interface of the substrate, has a high specific surface area and a porous structure, and can also effectively reduce the current density and relieve the volume effect, so that metal lithium is uniformly deposited, and the growth of lithium dendrites is effectively inhibited.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, and relates to a preparation method of a composite solid electrolyte for inhibiting the growth of lithium dendrites. Background technique [0002] Due to their high mechanical strength, solid-state electrolytes are considered to be an important approach to solve the dendrite problem in Li metal anodes. However, numerous research works have shown that the problem of lithium dendrites still exists in solid-state batteries, and in some solid-state electrolytes with ultra-high mechanical strength, dendrite growth pierces the electrolyte faster than in liquid batteries, indicating that Mechanical strength is not the only factor that affects dendrite problems. The core is to control the deposition behavior of lithium ions. [0003] Three-dimensional graphene has high external / internal surface area, high mechanical stress, and the three-dimensional interface formed by the three-dimension...

Claims

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Application Information

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IPC IPC(8): H01M10/0562
CPCH01M10/0562Y02E60/10
Inventor 王磊张祥功张明陶园学赵权吴骐
Owner WUHAN MARINE ELECTRIC PROPULSION RES INST CHINA SHIPBUILDING IND CORP NO 712 INST
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