Background
Because lithium batteries have the advantages of high energy density, long service life, low self-discharge and the like, the lithium batteries are increasingly widely applied to the fields of consumer electronics, electric vehicles, energy storage and the like. However, the lithium ion battery has the performance which can not reach the expected index in the using or storing process, such as capacity attenuation, liquid leakage, even failure phenomena of smoking, fire, thermal runaway, even explosion and the like, and especially is a safety problem, so that a lot of problems are brought to the application of the lithium ion battery, and especially, huge risks and pressure are brought to further expanding the application, such as electric vehicles, energy storage power stations and the like.
Commercial lithium batteries mostly adopt liquid electrolytes containing flammable organic solvents, so that safety risks exist, and development of all-solid-state lithium batteries is one of feasible ways for improving the safety of the batteries. Solid electrolytes are non-volatile, and generally non-flammable, relative to liquid electrolytes; can keep stable in a wider temperature range; some solid electrolytes have a wide electrochemical window, which is beneficial for increasing the energy density of the battery. However, when the temperature rises to a certain degree, the stability of the solid electrolyte itself may also change, and particularly when the negative electrode uses metallic lithium (or sodium) or the battery is in a high SOC state, the metal may react with some solid electrolyte membranes violently, and the result that the diaphragm is broken and the positive and negative electrodes are short-circuited to cause severe thermal runaway also exists. At present, no device and method for measuring the membrane rupture temperature of the solid electrolyte or the composite solid electrolyte membrane are provided.
Disclosure of Invention
In view of this, the utility model aims at providing a solid state electrolyte membrane performance test device that is convenient, easy to operate, and the suitability is strong, adopts this device can realize the test of solid state electrolyte membrane at broad temperature range (130 ℃ -350 ℃) rupture of membranes temperature.
In order to achieve the above purpose, the technical scheme of the utility model is realized like this:
a solid electrolyte membrane rupture temperature testing device comprises an upper peripheral shell, a lower peripheral shell, a first plug body, a second plug body and a conductive column, wherein a cavity is formed in the lower peripheral shell, a first gasket, a solid electrolyte membrane and the first plug body are sequentially placed in the cavity from bottom to top, the upper end of the first plug body extends out of the lower peripheral shell for a certain distance, the second plug body is inserted at the upper end of the first plug body, the upper peripheral shell is detachably connected to the outside of the second plug body, the upper end of the upper peripheral shell is connected with a first conductive signal column, the lower end of the lower peripheral shell is connected with a second conductive signal column, the first plug body and the second plug body are of a straight-tube structure penetrating through from top to bottom, the second gasket and the conductive column are sequentially placed in the first plug body from bottom to top, the upper end face of the conductive column is in contact with the upper peripheral shell, the lower peripheral shell, the first plug body, the second plug body, The second gasket is made of a conductive material; the side wall of the lower peripheral shell is provided with a small hole, a thermocouple is arranged in the hole, and the thermocouple main body is arranged in the side wall of the lower peripheral shell.
Furthermore, the outer side of the second plug body is provided with external threads, the inner side of the upper peripheral shell is provided with internal threads, and the upper peripheral shell is connected with the second plug body through threads.
Further, the inner diameter of the second plug body is the same as the outer diameter of the first plug body, and the outer diameter of the second plug body is the same as the inner diameter of the upper peripheral shell.
Further, the upper peripheral shell and the lower peripheral shell are both made of stainless steel sheets.
Further, the first plug body and the second plug body are made of stainless steel, gold, silver, platinum or carbon materials.
Further, the first gasket and the second gasket are stainless steel sheets or gold sheets or silver sheets or platinum sheets or carbon sheets, and if the first gasket and the second gasket are stainless steel sheets, platinum, gold or carbon is sprayed on the surfaces of the first gasket and the second gasket.
Further, the conductive column, the first conductive signal column and the second conductive signal column are made of stainless steel, gold, silver, platinum or carbon.
Compared with the prior art, solid state electrolyte membrane rupture of membranes temperature testing arrangement have following advantage: the testing temperature range of the membrane breaking temperature of the solid electrolyte membranes of different types is 130-350 ℃; the surface of the gasket used by the device is sprayed with platinum or gold or carbon, so that the problem of high solid-solid interface impedance of the solid electrolyte membrane in contact with the gasket is solved; this device is provided with the second cock body and goes up peripheral casing, screws up whole device through the external screw thread of the second cock body and the internal thread of going up peripheral casing, has guaranteed the leakproofness of device, avoids the device to break damage under the high temperature.
Detailed Description
It should be noted that, in the present invention, the embodiments and features of the embodiments may be combined with each other without conflict.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are used merely for convenience of description and for simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be construed as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The present invention will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
As shown in fig. 1-2, a solid electrolyte membrane rupture temperature testing device includes an upper peripheral casing 2, a lower peripheral casing 1, a first plug 4, a second plug 5 and a conductive post 9, wherein a cavity is formed in the lower peripheral casing 1, a first gasket 6, a solid electrolyte membrane 7 and the first plug 4 are sequentially placed in the cavity from bottom to top, the upper end of the first plug 4 extends out of the lower peripheral casing 1 by a distance, the second plug 5 is inserted into the upper end of the first plug 4, the upper peripheral casing 2 is detachably connected to the outside of the second plug 5, the upper end of the upper peripheral casing 2 is connected to a first conductive signal post 10, the lower end of the lower peripheral casing 1 is connected to a second conductive signal post 11, and an electrical signal is transmitted out through the second conductive signal post 11.
The first plug body 4 and the second plug body 5 are both vertical cylindrical structures which penetrate through from top to bottom, a second gasket 8 and a conductive column 9 are sequentially placed in the first plug body 4 from bottom to top, the upper end face of the conductive column 9 is in contact with the upper peripheral shell 2, and the upper peripheral shell 2, the lower peripheral shell 1, the first plug body 4, the second plug body 5, the first gasket 6 and the second gasket 8 are all made of conductive materials; the side wall of the lower peripheral shell 1 is provided with a small hole, a thermocouple 3 is arranged in the hole, and the main body of the thermocouple 3 is arranged in the side wall of the lower peripheral shell 1. The temperature inside the shell is measured only by communicating the position of the side wall opening with the inside of the shell.
The outside of the second plug body 5 is provided with external threads, the inside of the upper peripheral shell 2 is provided with internal threads, and the upper peripheral shell 2 is connected with the second plug body 5 through threads.
The inner diameter of the second plug body 5 is the same as the outer diameter of the first plug body 4, and the outer diameter of the second plug body 5 is the same as the inner diameter of the upper peripheral shell 2.
The upper peripheral shell 2 and the lower peripheral shell 1 are both made of stainless steel sheets.
The first plug body 4 and the second plug body 5 are made of stainless steel, gold, silver, platinum or carbon materials.
The first gasket 6 and the second gasket 8 are stainless steel sheets or gold sheets or silver sheets or platinum sheets or carbon sheets, and if the stainless steel sheets are stainless steel sheets, platinum or gold or carbon is sprayed on the surfaces of the stainless steel sheets.
The conductive column 9, the first conductive signal column 10, and the second conductive signal column 11 are made of stainless steel, gold, silver, platinum, or carbon.
During the use, first gasket 6 is placed by lower up in proper order to inside cavity, solid electrolyte membrane 7, first cock body 4, second gasket 8 and leading electrical pillar 9 are placed by lower up in proper order to first cock body 4 is inside, place second cock body 5 afterwards, and second cock body 5 inserts first cock body 4 upper end, goes up outside peripheral casing 2 closes second cock body 5 soon, when the screw is screwed, guarantees the leakproofness of device, avoids the device to break under high temperature and damages. At this time, the upper peripheral housing 2 is in contact with the conductive post 9. And transmits the electrical signal out through the first conductive signal post 10.
The solid electrolyte membrane may be a polymer electrolyte such as PEO or an inorganic solid electrolyte such as an inorganic oxide, an inorganic sulfide, but is not limited thereto.
The test method comprises the following steps:
setting the initial temperature of a thermostat to be 100 ℃;
secondly, putting a solid electrolyte sample to be tested into the device, and then putting the solid electrolyte sample into a drying oven;
connecting the first conductive signal column 10 and the second conductive signal column 11 with two electrodes of a resistance instrument respectively, and connecting a thermocouple with a temperature acquisition recorder;
starting a temperature acquisition recorder and a resistance meter, simultaneously recording the temperature and the resistance, and recording a value every 5 s;
controlling the constant temperature box to slowly heat up at the heating rate of 1-5 ℃/min until reaching a target temperature value;
sixthly, the temperature and the resistance value recorded in the fourth step are plotted, the resistivity is continuously reduced along with the increase of the temperature, when the temperature is increased to a certain temperature, the resistance is rapidly increased due to the melting/cracking of the solid electrolyte membrane 7, and the temperature point or the temperature interval at which the resistance value is suddenly increased is taken as the membrane rupture temperature (T) of the solid electrolyte membraneb)。
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.