JPWO2021023513A5 - - Google Patents

Description

On the side of the throttle 38 opposite the mass spectrometer, ie to the left of the throttle 38 in the drawing, the pressure in lines 26, 30, 32, 36 is, for example, 5 mbar. In this case, viscous flow conditions prevail and the measurement gas will diffuse in the residual gas along this distance, leading to time delays. The diffusion distance from connection point 40 of connection line 26 and vacuum line 21 in FIG. .
In addition, this invention includes the following contents as a mode of implementation.
[Aspect 1]
A method for airtightness testing of a subject (14) in which a liquid (12) is enclosed, comprising:
the subject has an internal pressure below atmospheric pressure;
The method includes:
inserting the subject (14) into a test chamber (16);
evacuating the test chamber (16) to a pressure below the internal pressure of the subject (14);
without externally delivering a carrier gas to the test chamber, along with gas components desorbed from the walls of the test chamber and portions of the liquid leaking from the subject through leaks in the subject; aspirating from the test chamber;
conveying the aspirated residual gas component along with the portion of the liquid that has leaked from the subject to a detector (28);
detecting with a detector (28) the portion of the liquid (12) that has leaked through a leak in the subject (14);
method including.
[Aspect 2]
A method according to claim 1, characterized in that said conveyed portion of said liquid (12) is molecular particles in a vaporized state.
[Aspect 3]
3. Method according to claim 1 or 2, characterized in that said liquid (12) has a vapor pressure of less than 500 mbar at room temperature.
[Aspect 4]
4. The method of any one of aspects 1-3, wherein the subject (14) is a battery and the liquid is an electrolyte.
[Aspect 5]
Method according to any one of aspects 1 to 4, characterized in that said test chamber (16) is a rigid test chamber or a film chamber.
[Aspect 6]
A method according to any one of aspects 1 to 5, characterized in that said detector (28) comprises a selective sensor applied to said portion of said liquid to be detected.
[Aspect 7]
A method according to aspect 6, characterized in that said detector (28) is a gas detector, such as a mass spectrometer, a gas chromatograph, an infrared absorption detector, or a detector comprising a chemical or semiconductor sensor. how to.
[Aspect 8]
The method of any one of aspects 1-7, wherein said detector (28) operates in a vacuum system having a pressure lower than said pressure in said test chamber (16). .
[Aspect 9]
9. A method according to any one of aspects 1 to 8, wherein the detected portion of the gas component and the liquid is detected by the detector (28) only when a predetermined pressure limit is reached in the test chamber. ).
[Aspect 10]
A method according to claim 9, characterized in that said pressure limit is in the range 2 mbar to 100 mbar, preferably less than 10 mbar.
[Aspect 11]
11. A method according to aspect 9 or 10, wherein said detector is connected to said test chamber (16) via a valve (V2), said valve being closed at the start of evacuation of said test chamber, said pressure A method characterized in that it is opened only when a limit value is reached.
[Aspect 12]
12. The method of any one of aspects 1-11, wherein the subject (14) is flushed with a flushing gas after being inserted into the test chamber (16).
[Aspect 13]
13. The method of any one of aspects 1-12, wherein said portion of said liquid (12) leaking from said subject (14) is detected by said detector (28) for a period of time before said portion is detected by said detector (28). and accumulating in said test chamber (16) or connecting line.
[Aspect 14]
14. The method of any one of aspects 1-13, wherein a test leak containing a test liquid is inserted into the test chamber (16) before the subject (14) is inserted into the test chamber (16). and calibrating the detector with the test leak by evacuating the test chamber and detecting with the detector (28) the portion of the liquid that leaks through the test leak. A method characterized by
[Aspect 15]
15. A method according to any one of aspects 1 to 14, wherein a gas already contained in said subject (14) when said subject is inserted into said test chamber (16), said leak detection A method characterized in that there is no gas used as a test gas for