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A molten salt electrochemical multifunctional in-situ characterization device and its application method

An electrochemical and multi-functional technology, applied in the fields of electrochemical variables of materials, measurement devices, material analysis using radiation, etc. Observation and other issues to achieve the effect of real results, good authenticity and accurate comparison

Active Publication Date: 2022-02-25
UNIV OF SCI & TECH BEIJING +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The technical problem solved by the present invention is that it is difficult to directly observe the electrolysis process in the current high-temperature molten salt environment, and only secondary analysis can be performed. Compared with direct observation and analysis, the research on the high-temperature molten salt electrolysis process has serious lag and inaccuracy , and most of the existing research methods or devices can only achieve in-situ and real-time acquisition of a single information, and cannot achieve in-situ and real-time acquisition of multiple information

Method used

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  • A molten salt electrochemical multifunctional in-situ characterization device and its application method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] A method for using a molten salt electrochemical multifunctional in-situ characterization device, the specific steps are as follows;

[0077] Step 1: Take an equimolar ratio of NaCl and KCl molten salt mixture and place it in a transparent electrolytic cell 2111 with an outer diameter of 10 mm and a wall thickness of 1 mm, place the transparent electrolytic cell 2111 in the optically transparent hearth 211 of the vacuum holding furnace 2 and combine The rotary table 1 is tightly connected; the transparent electrolytic cell 2111 is a quartz tube;

[0078] Step 2: When the vacuum holding furnace 2 is evacuated to 1-10Pa, start to increase the temperature of the transparent electrolytic cell 2111 until the molten salt mixture in the transparent electrolytic cell 2111 is melted and kept at 700°C to obtain a high-temperature melt;

[0079] Step 3: Insert two graphite electrodes into the high-temperature melt by operating the furnace cover 3 and the electrode system 4, and th...

Embodiment 2

[0083] A method for using a molten salt electrochemical multifunctional in-situ characterization device, the specific steps are as follows;

[0084] Step 1: Take Na with a molar ratio of 3:2 2 CO 3 and K 2 CO 3 The molten salt mixture is placed in a transparent electrolytic cell 2111 with an outer diameter of 10 mm and a wall thickness of 1 mm, and the transparent electrolytic cell 2111 is placed in the optically transparent hearth 211 of the vacuum holding furnace 2 and is closely connected with the rotary table 1; the transparent electrolytic cell 2111 is a quartz tube;

[0085] Step 2: When the vacuum holding furnace 2 is evacuated to 1-10 Pa, start to increase the temperature of the transparent electrolytic cell 2111 until the molten salt mixture in the transparent electrolytic cell 2111 is melted and kept at 800°C to obtain a high-temperature melt;

[0086] Step 3: Insert two graphite electrodes into the high-temperature melt by operating the furnace cover 3 and the e...

Embodiment 3

[0090] A method for using a molten salt electrochemical multifunctional in-situ characterization device, the specific steps are as follows;

[0091] Step 1: Take NaCl and AlCl in equimolar ratio 3 The molten salt mixture is placed in a transparent electrolytic cell 2111 with an outer diameter of 10 mm and a wall thickness of 1 mm. The transparent electrolytic cell 2111 is placed in the optically transparent hearth 211 of the vacuum holding furnace 2. There is a glass support rod at the bottom of the transparent electrolytic cell 2111 , the support rod can be directly fixed to the bottom rotary table 1 by mechanical clamping; the transparent electrolytic cell 2111 is a glass tube;

[0092] Step 2: When the vacuum holding furnace 2 is evacuated to 1-10Pa, start to increase the temperature of the transparent electrolytic cell 2111 until the molten salt mixture in the transparent electrolytic cell 2111 is heated to 150°C and kept warm;

[0093]Step 3: insert sheet-shaped metal al...

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Abstract

The embodiment of the present invention discloses a molten salt electrochemical multifunctional in-situ characterization device and its use method, which belong to the technical field of high temperature electrochemical analysis. The device of the invention can simultaneously support in-situ Raman, in-situ optical and in-situ synchrotron radiation scanning in one body, and can realize structural analysis of high-temperature melts, in-situ visualization of electrode three-dimensional morphology, and in-depth and comprehensive understanding of the corresponding evolution. process. The device is specifically composed of a vacuum insulation furnace body and a transparent electrolytic cell. The vacuum insulation furnace body is designed with a concave Raman corner objective lens entrance, an optical visualization window, a supplementary light window, an aluminum foil transmission window, a transparent quartz furnace, and two-stage heating. The resistance wire and other systems realize the above three functions; while the transparent electrolytic cell integrates the furnace tube and the crucible of the conventional vertical resistance furnace, and realizes the connection between the crucible and the rotary table at the bottom of the furnace through processing, and then realizes the test process. The electrolyzer rotates with the rotation of the turntable, and the tomographic picture of the electrode is obtained.

Description

technical field [0001] The invention belongs to the technical field of high-temperature electrochemical analysis, and relates to a molten salt electrochemical multifunctional in-situ characterization device and a use method. Background technique [0002] At present, high-temperature molten salts are widely used in the metallurgical industry due to their wide electrochemical window, high ionic conductivity, and fast electrochemical reaction rate. In addition, its high boiling point and thermal conductivity make high-temperature molten salt play an important role in large-scale energy storage and nuclear industry. [0003] For a long time, analyzing the chemical structure of high-temperature molten salts under different conditions and different components, and revealing the real chemical and electrochemical reaction mechanisms inside the melt under high-temperature environments have always been the focus of research in the field of high-temperature molten salt electrochemistry...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/26G01N21/65G01N21/84G01N23/02
CPCG01N27/26G01N21/65G01N21/84G01N23/02
Inventor 焦树强宋维力焦汉东陈浩森
Owner UNIV OF SCI & TECH BEIJING
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