CN116559039A - Gas barrier property testing system and testing method - Google Patents

Abstract

The application provides a gas barrier property test system and a test method, which relate to the technical field of film performance test. The pressure difference on the two sides of the sample can be changed from the pressure difference between the pressure and the high vacuum degree in the traditional mode to the pressure difference between the pressure and the low vacuum degree, so that the risk of physical damage of the sample is reduced, the reliability of the gas barrier property test is improved, and the method is particularly suitable for high-temperature aging test in a water vapor environment.

Description

Gas barrier property testing system and testing method

Technical Field

The application relates to the technical field of film performance testing, in particular to a gas barrier property testing system and a testing method.

Background

In the technical fields of electronics, food packaging, etc., electronic parts or foods wrapped inside a film are easily corroded by water and oxygen in the air, so that the film needs to have high water vapor barrier property and oxygen barrier property. In the development process of the film packaging structure or before the product shipment, the water-oxygen barrier property test is required to determine whether the water-oxygen barrier property of the film meets the specification.

According to different principles, the existing water-oxygen barrier property test of film samples can be roughly classified into an isobaric method and a differential pressure method.

The isobaric method is generally to introduce a gas to be detected to be blocked on one surface (hereinafter, also referred to as a supply side) of a sample, introduce an inert gas into the other surface (hereinafter, also referred to as a permeation side) of the sample, and flow the inert gas, wherein the supply side and the permeation side of the sample are maintained at substantially the same pressure (generally, atmospheric pressure), and the inert gas is used as a carrier gas to bring the gas to be detected permeated through the sample into a detection device together to measure the content of the gas to be detected permeated through the sample. Among these, the isobaric method has the advantages that: the pressure on both the supply side and the permeate side is substantially the same, and the sample is not prone to physical defects such as glass. Whereas the isobaric method has the disadvantage that: the detection device needs to have the capability of analyzing a large amount of detection target components in the carrier gas at a high level, however, such a high-sensitivity gas analysis technique is difficult to implement at present. Moreover, since the carrier gas generally contains impurities such as water vapor and oxygen before being introduced into the detection device, this may cause a decrease in detection sensitivity and accuracy.

The differential pressure method generally involves inputting a gas supply having a certain pressure and mixed with a gas to be detected (for example, when a water vapor barrier property test is performed, the gas to be detected is water vapor, the gas supply is a dry gas such as nitrogen gas) to one surface of a sample, forming a vacuum transmission side chamber on the other surface of the sample, and introducing the gas to be detected, which has passed through the sample, into a detection device to measure the gas content of the transmitted sample. The pressure difference method has the advantages that the detection device (such as a mass spectrometer) can detect the object to be detected in the permeation side in a high vacuum state, the sensitivity is high, and the test accuracy can be ensured. The pressure difference method has the following defects: in the test process, because the supply side and the permeation side in the test sample have a large pressure difference, the test sample is easy to have physical defects such as stripping and the like, the phenomenon is that physical damages such as indentation and cracks appear on the test sample, and the gas to be detected easily passes through the test sample from the physical damages, so that the test is invalid.

The problem that the test specimen is susceptible to physical damage is more remarkable when subjected to an aging test in a water vapor environment. For example, in order to test the aging performance of the encapsulation film in the organic electronics field at 85 ℃/85% RH state, the test specimen needs to be warmed to 85 ℃, and the humidity (RH) in the supply side environment needs to be maintained at 85%. Because the gas at the supply side has higher concentration and the sample is in a heating state, the sample is more easily affected by the pressure difference, and is more easily subjected to physical damage, so that the test is invalid.

Disclosure of Invention

In summary, the technical problem to be solved by the present application is to provide a new gas barrier property testing system.

The technical scheme adopted for solving the technical problems is as follows:

in a first aspect, the present application provides a gas barrier testing system comprising:

a support body defining a first cavity having a first opening for interfacing with the supply side chamber with each other;

the first flexible film is combined on the end face of the first opening to close the first opening, the surface of the first flexible film, which is opposite to the supporting body, forms a sample bearing surface for bearing a sample, and the second flexible film extends into the first cavity; the space between the first flexible membrane and the second flexible membrane forms a buffer chamber which is in a closed shape and has adjustable pressure, and the space of the first cavity on one side of the second flexible membrane, which is opposite to the buffer chamber, forms a permeation side chamber.

Optionally, in some embodiments of the present application, the film thickness of the first flexible film is greater than the film thickness of the second flexible film, and/or the film thickness of the second flexible film is 40 to 400um.

Optionally, in some embodiments of the present application, the support includes a first sub-support and a second sub-support, the first sub-support defining the first opening and having a first sub-cavity, the second sub-support having a second sub-cavity, the first sub-support and the second sub-support interfacing with each other such that the first sub-cavity and the second sub-cavity are in communication and at least partially form the first cavity, the second flexible membrane being sandwiched between the first sub-support and the second sub-support.

Alternatively, in some embodiments of the present application, the first flexible film has an air permeability of 0.1 to 10cm ³ /(m ³ 24 h.bar), the second flexible film having an air permeability of 0.1 to 10cm ³ /(m ³ 24 h.bar); and/or the number of the groups of groups,

the material of the first flexible film is at least one selected from polyimide, polyamide, polycarbonate, polyether ether ketone, polyether sulfone, polyamide imide, polyethylene, polypropylene, polyethylene terephthalate, polyethylene naphthalate, polyvinyl chloride, polyvinylidene chloride, polyacrylonitrile, polystyrene, polyphenylene sulfide, polytetrafluoroethylene and polyhexamethylene adipamide, and the material of the second flexible film is at least one selected from polyimide, polyamide, polycarbonate, polyether ether ketone, polyether sulfone, polyamide imide, polyethylene, polypropylene, polyethylene terephthalate, polyethylene naphthalate, polyvinyl chloride, polyvinylidene chloride, polyacrylonitrile, polystyrene, polyphenylene sulfide, polytetrafluoroethylene and polyhexamethylene adipamide.

Optionally, in some embodiments of the present application, the support further includes a first support portion disposed between the first flexible film and the second flexible film, the first support portion having a first support surface covered by the first flexible film, and a first channel extending from the first support surface and communicating with the buffer chamber is formed on the first support portion; and/or

The support body also comprises a second support part arranged on one side of the second flexible film, which is opposite to the buffer chamber, the second support part is provided with a second support surface covered by the second flexible film, and a second channel which extends from the second support surface and is communicated with the transmission side chamber is formed on the second support part.

Optionally, in some embodiments of the present application, the method further includes:

a supply body defining a supply-side chamber;

the gas generating device to be detected is at least provided with a detection gas branch which is in butt joint with the buffer chamber so as to provide the gas to be detected for the buffer chamber;

the pressure supply gas generating device is provided with at least a first gas supply branch which is in butt joint with the buffer chamber so as to supply pressure supply gas to the buffer chamber, thereby adjusting the pressure in the chamber at the supply side;

the vacuum generating device is provided with at least a first vacuum branch which is in butt joint with the permeation side cavity;

the detection device is used for detecting the content of the gas to be detected in the permeation side cavity.

Optionally, in some embodiments of the present application, the gas generating device to be detected further has a second gas supply branch that interfaces with the buffer chamber, and the vacuum generating device further has a second vacuum branch that interfaces with the buffer chamber.

Optionally, in some embodiments of the present application, the supply body defines a second opening in communication with the supply-side chamber, the supply body has at least a testing position and a sample-changing position with respect to the support body, the supply body and the support body in the testing position are in abutment, and the second opening and the first opening are brought into abutment with each other such that the supply body and the support body clamp a sample on the sample-bearing surface, and the supply body and the support body in the sample-changing position are separated to reveal the sample-bearing surface.

Optionally, in some embodiments of the present application, the gas barrier testing system includes a test seat, the test seat defines an external chamber having at least a closed state, the support body and the supply body are connected to the test seat, the support body defines a portion of the first opening, the portion of the supply body defining the second opening extends into the external chamber, and the vacuum generating device further has at least a third vacuum branch abutting against the external chamber.

In a second aspect, the present application provides a gas barrier testing method employing the gas barrier testing system of the first aspect, comprising the steps of:

disposing a sample on a sample-bearing surface;

adjusting the pressure of the buffer chamber to enable the buffer chamber to have a first vacuum degree, and adjusting the pressure of the transmission side chamber to enable the transmission side chamber to have a second vacuum degree, wherein the first vacuum degree is smaller than the second vacuum degree;

Introducing gas to be detected into the supply side chamber so that the pressure in the supply side chamber is higher than that in the buffer chamber;

and determining the content of the gas to be detected in the permeation side cavity.

Optionally, in some embodiments of the present application, adjusting the pressure of the permeate side chamber to provide the permeate side chamber with a second vacuum level includes:

the pressure of the permeation side chamber is adjusted through the dry pump so that the permeation side chamber has a third vacuum degree, and the pressure of the permeation side chamber is adjusted through the cold pump so that the permeation side chamber is changed from the third vacuum degree to a second vacuum degree, wherein the third vacuum degree is smaller than the second vacuum degree.

Optionally, in some embodiments of the present application, the test method further includes, before testing the sample, the steps of:

adjusting the pressure of the permeation side chamber so that the permeation side chamber has a second vacuum degree;

introducing a gas to be detected with preset content into the permeation side cavity, and determining the corrected detection content of the gas to be detected in the permeation side cavity;

obtaining an error proportional relation between the preset content and the corrected detected content according to the preset content and the corrected detected content;

wherein, confirm the content of waiting to detect the gas in permeating the side cavity, include:

determining the actual detection content of the gas to be detected in the permeation side cavity;

And determining the content of the gas to be detected in the permeation side cavity according to the actual detection content and the error proportion relation.

In conclusion, due to the adoption of the technical scheme, the application at least comprises the following beneficial effects:

the application provides a gas barrier property test system, mainly defines a buffer chamber that is closed shape and pressure adjustable through setting up first flexible membrane and second flexible membrane in the first cavity of support to make first cavity be in the space that the second flexible membrane is in back to buffer chamber one side constitutes and sees through the side cavity, and part waits to detect gaseous invasion to see through in the side cavity in proper order through sample, first flexible membrane and second flexible membrane in order, in order to be detected. When the test is performed, the pressure difference on two sides of the sample can be changed from the pressure difference between the pressure and the high vacuum degree in the traditional mode to the pressure difference between the pressure and the low vacuum degree, so that the risk of physical damage of the sample is reduced, the reliability of the gas barrier test is improved, and meanwhile, the high vacuum degree can still be maintained through the side chamber, so that the requirement on a detection device is reduced, and the device is particularly suitable for high-temperature aging test under a water vapor environment.

Drawings

For a clearer description of an embodiment of the present application, reference will be made to the accompanying drawings of embodiments, which, as will become apparent, relate only to some embodiments of the present application and are not limiting of the present application, wherein:

FIG. 1 is a schematic structural view of a sample supporting structure in example 1 according to the present invention;

FIG. 2 is a schematic view showing the structure of the sample support structure and the cooperation of the supply body in example 1 according to the present invention;

FIG. 3 is a schematic top view of a first support and a first channel thereof on a sample support structure according to embodiment 1 of the present invention;

FIG. 4 is a schematic view showing the structure of the test seat, the sample supporting structure and the feeder according to the embodiment 2 of the present invention;

FIG. 5 is a schematic diagram showing piping connection of the gas barrier test system in example 2 according to the present invention;

FIG. 6 is a flow chart of the test method in example 1 according to the present invention;

FIG. 7 is a schematic diagram of a further refinement of the test method of example 1 according to the present invention;

fig. 8 is a schematic diagram of a further refinement of the test method in example 1 provided by the present invention.

Reference numerals illustrate:

100-support, 101 a-first sub-support, 101 b-second sub-support, 110-first flexible membrane, 110 a-sample support surface, 120-second flexible membrane, 130-buffer chamber, 140-permeate side chamber, 150-first support, 150 a-first channel, 160-second support, 160 a-second channel, 170-buffer joint, 180-connector

200-a supply body, 210-a supply side chamber;

300-test seat, 300 a-seat body, 300 b-movable cover, 310-external chamber;

400-a gas generating device to be detected, 410-a detection gas branch;

500-a gas supply generating device, 510-a first gas supply branch, 520-a second gas supply branch;

600-vacuum generating device, 610-first vacuum branch, 620-second vacuum branch, 630-third vacuum branch;

700-detecting device;

810-first switch valve, 820-second switch valve, 830-third switch valve, 840-fourth switch valve, 850-fifth switch valve, 860-sixth switch valve;

900-sample.

Detailed Description

The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all, of the embodiments of the present application. Based on the embodiments herein, all other embodiments that a person skilled in the art would obtain without making any inventive effort are within the scope of protection of the present application.

In the description of the present application, it should be understood that the terms "center," "longitudinal," "transverse," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate an orientation or positional relationship based on that shown in the drawings, merely for convenience of description and to simplify the description, and do not indicate or imply that the devices or elements referred to must have a unique orientation, be configured and operated in a particular orientation, and thus should not be construed as limiting the present application. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or the inclusion of a number of indicated features. Thus, a feature defining "a first" or "a second" may include, either explicitly or implicitly, one or more features. In the description of the present application, the meaning of "a plurality" is two or more unless explicitly defined otherwise.

In the application, the term "exemplary" is used to mean "serving as an example, instance, or illustration. Any embodiment described herein as exemplary is not necessarily to be construed as preferred or advantageous over other embodiments. The following description is presented to enable any person skilled in the art to make and use the application. In the following description, details are set forth for purposes of explanation. It will be apparent to one of ordinary skill in the art that the present application may be practiced without these specific details. In other instances, well-known structures and processes have not been shown in detail to avoid obscuring the description of the present application with unnecessary detail. Thus, the present application is not intended to be limited to the embodiments shown, but is to be accorded the widest scope consistent with the principles disclosed herein.

Example 1

The main body of this embodiment is a sample supporting structure of a gas barrier test system. The gas barrier test system used in this embodiment is specifically a water vapor barrier test system. It should be noted that the sample supporting structure provided in this embodiment is not limited to application to the water vapor barrier test system, and may be used in other gas barrier test systems such as an oxygen barrier test system.

Referring to fig. 1 and 2, in this embodiment, the sample supporting structure specifically includes:

a support body 100, the support body 100 defining a first cavity having a first opening for interfacing with the supply side chamber 210;

a first flexible film 110 and a second flexible film 120, the first flexible film 110 being bonded on the first opening end face to close the first opening, a surface of the first flexible film 110 facing away from the support 100 constituting a sample-carrying surface 110a for carrying the sample 900, the second flexible film 120 extending into the first cavity; the space between the first flexible membrane 110 and the second flexible membrane 120 forms a buffer chamber 130 with a closed shape and adjustable pressure, and the space of the first cavity on the side of the second flexible membrane 120 opposite to the buffer chamber 130 forms a transmission side chamber 140.

The support 100 refers to a component for carrying the sample 900, and the first flexible film 110 is combined on an end surface of the first opening of the support 100 to close the first opening, so that the first flexible film 110 cooperates with the support 100 to separate two isolated spaces, namely a space outside the first flexible film 110 and a space inside the first cavity, respectively, and the second flexible film 120 extends into the first cavity to separate the first cavity into two spaces. The space outside the first flexible film 110 constitutes a supply-side chamber 210 for introducing water vapor having a certain pressure and a certain content. Since the pressure of the buffer chamber 130 defined by the first flexible film 110 and the second flexible film 120 and the inner wall of the first cavity is adjustable, when the test is performed, the buffer chamber 130 and the supply side chamber 210 can have a certain pressure difference, the buffer chamber 130 and the transmission side chamber 140 can also have a certain pressure difference, the buffer chamber 130 can be in a state of lower vacuum degree by pressure adjustment, and the transmission side chamber 140 can be in a state of higher vacuum degree. At this time, the pressure difference is formed in a gradient stepwise manner along the direction from the supply side chamber 210 to the buffer chamber 130 to the permeation chamber, and the pressure difference is formed in the supply side chamber 210, the buffer chamber 130, and the permeation chamber. Further, the gas to be detected, i.e., the water vapor, sequentially permeates the sample 900, the first flexible film 110 and the second flexible film 120 and gradually enters the permeation-side chamber 140 with higher vacuum degree, and is detected by the detection device 700, so as to evaluate the water vapor barrier property of the sample 900.

Compared with the conventional manner, the scheme provided in this embodiment mainly defines the buffer chamber 130 with adjustable pressure through the first flexible membrane 110 and the second flexible membrane 120, and the pressure difference between the two sides of the sample 900 is changed from the pressure difference between the atmosphere and the high vacuum degree in the conventional manner to the pressure difference between the atmosphere and the low vacuum degree, so that the risk of physical damage of the sample 900 is reduced, the reliability of the gas barrier test is improved, and the method is particularly suitable for the high-temperature aging test in the water vapor environment. Meanwhile, compared with the solution that only reduces the vacuum degree of the transmission side chamber 140, in the solution provided in the embodiment, the transmission side chamber 140 can still maintain a higher vacuum degree, thereby reducing the specification requirements for the detection device.

Here, the gas rarefaction degree in the vacuum state is referred to as a vacuum degree, and the vacuum degree is mainly used to describe the pressure condition in the chamber, and the vacuum degree is generally expressed by a pressure value (unit is Pa, mbar,1 mbar=100 Pa, for example). The rarefaction of the gas, the smaller the pressure value, and the higher the vacuum.

In the present embodiment, the supply-side chamber 210 is defined by the supply body 200, and the openings of the supply body 200 and the support body 100 are aligned with each other, but the present invention is not limited thereto. The supply body 200 and the supply-side chamber 210 defined by the same may be deformed by an practitioner without affecting the purpose of the invention.

In this embodiment, the support body 100 is formed with a buffer joint 170 communicating with the buffer chamber 130 for connecting with a pressure adjusting device, so that the pressure adjusting device adjusts the pressure in the buffer chamber 130. The practitioner may also adjust the pressure within the buffer chamber 130 in other ways, as this application is not particularly limited.

Regarding the connection manner of the first flexible film 110 and the second flexible film 120, in the present embodiment, the first flexible film 110 is directly adhered to the end face of the first opening in the support 100. While the second flexible membrane 120 extends into the support 100, if the second flexible membrane 120 is arranged with its edges glued to the inner wall of the first cavity, the second flexible membrane 120 has a certain risk of detachment under a higher pressure difference, so referring again to fig. 1, in this embodiment the support 100 comprises a first sub-support 101a and a second sub-support 101b, the first sub-support 101a defining a first opening and having a first sub-cavity, the second sub-support 101b having a second sub-cavity, the first sub-support 101a and the second sub-support 101b being fixedly butted against each other such that the first sub-cavity and the second sub-cavity are in communication and at least partly constitute the first cavity, the second flexible membrane 120 being clamped between the first sub-support 101a and the second sub-support 101 b. By providing the support body 100 separately, connection reliability of the second flexible film 120 can be ensured. Here, the support 100 is not limited to include only two sub-supports 100, and the operator may select the number of sub-supports included in the support 100 according to his own needs without affecting the purpose of the invention, but the two sub-supports 100 holding the second flexible film 120 at least partially define the first cavity regardless of the number of sub-supports included in the support 100.

As for the materials, the first flexible film 110 and the second flexible film 120 described hereinabove may be made of a polymer material as shown in the present embodiment. When the first flexible film 110 and the second flexible film 120 are made of a polymer material, the materials of the first flexible film 110 and the second flexible film 120 include, but are not limited to: any one of polyimide, polyamide, polycarbonate, polyetheretherketone, polyethersulfone, polyamideimide, polyethylene, polypropylene, polyethylene terephthalate, polyethylene naphthalate, polyvinyl chloride, polyvinylidene chloride, polyacrylonitrile, polystyrene, polyphenylene sulfide, polytetrafluoroethylene, polyhexamethylene adipamide, or a combination thereof.

When the water vapor transmission rate of the first flexible film 110 and the second flexible film 120 is lower than that of the sample 900, the water vapor content entering the transmission side chamber 140 is reduced, which increases the testing difficulty. Therefore, in the present embodiment, the water vapor permeability of the first flexible film 110 and the second flexible film 120 is configured to be 1 to 10 g/(m) ² 24 h). At the first flexibilityWhen the membrane 110 and the second flexible membrane 120 have the above-mentioned range of water vapor transmittance, the water vapor transmittance is generally several orders of magnitude higher than that of the sample 900, that is, most of the water vapor penetrating through the sample 900 enters the permeation side chamber 140 through the first flexible membrane 110 and the second flexible membrane 120, so as to reduce the testing difficulty.

In addition, for the gas barrier property test, after the water vapor or other gas to be detected reaches the saturation state in the first flexible film 110 and the second flexible film 120, more water vapor or other gas to be detected passes through the first flexible film 110 and the second flexible film 120. During the replacement of the sample 900, the first flexible membrane 110 is easily eroded by water vapor in the atmosphere, which affects the detection accuracy, so the membrane thickness of the first flexible membrane 110 needs to be set thicker to reduce the risk of water vapor in the atmosphere entering the buffer chamber 130 or the transmission-side chamber 140.

Whereas in this embodiment the second flexible membrane 120 is shielded from the first flexible membrane 110 and is not substantially in direct contact with the atmosphere. Since the time to reach the saturated state is in positive correlation with the thickness, the film thickness of the second flexible film 120 can be set smaller (for example, 40 to 400 um), and the second flexible film 120 can reach the saturated state faster than the case where the first flexible film 110 and the second flexible film 120 have the same film thickness, thereby reducing the test time.

In addition, as two members butted against each other, a gap must be formed between the first sub-support 101a and the second sub-support 101b, and the second flexible film 120 is disposed in the gap. That is, the side portion of the second flexible film 120 has a possibility of being impregnated with water vapor. In the manner described above, however, setting the film thickness of the second flexible film 120 to be smaller can reduce the possibility of the side of the sample 900 from being impregnated with water vapor, improving the accuracy of measurement.

In this case, when the sample 900 is replaced after one test is completed, the supply-side chamber 210 is generally restored to the atmospheric pressure state from the high pressure state, and if the first flexible membrane 110 and the second flexible membrane 120 have high air permeability (for example, the first flexible membrane 110 and the second flexible membrane 120 are made of porous materials), part of the gas may enter the buffer chamber 130 through the first flexible membrane 110 or enter the permeation-side chamber 140 through the second flexible membrane 120 due to losing the barrier effect of the sample 900, and it is difficult to maintain the vacuum state in the buffer chamber 130 and the permeation-side chamber 140. Therefore, after each test is completed, the buffer chamber 130 and the permeation side chamber 140 need to reestablish the vacuum state, which affects the test efficiency.

Accordingly, in the present embodiment, the air permeability of the first flexible film 110 and the second flexible film 120 is configured to be 0.1 to 10cm ³ /(m ³ 24 h.bar). Under such values, the first flexible membrane 110 and the second flexible membrane 120 have good gas barrier properties, so that when the supply side chamber 210 is in the atmospheric pressure state, the buffer chamber 130 defined by the first flexible membrane 110 and the second flexible membrane 120 and the transmission side chamber 140 defined by the second flexible membrane 120 will not have a larger change in the air pressure or a slower rate of change in the air pressure. Thus, the buffer chamber 130 and the transmission side chamber 140 can be prevented from being set up again to be in a vacuum state after one test is finished, and the test efficiency is improved.

It will be appreciated that the first flexible membrane 110, the second flexible membrane 120, and the sample 900 overlying the sample support surface 110a will deform to some extent under the pressure differential. When the deformation amplitude is large, the first flexible film 110, the second flexible film 120, and the sample 900 are likely to be physically damaged.

Referring to fig. 1 again, in the present embodiment, the support body 100 further includes a first support portion 150 disposed between the first flexible membrane 110 and the second flexible membrane 120, the first support portion 150 has a first support surface covered by the first flexible membrane 110, and a first channel 150a extending from the first support surface and communicating with the buffer chamber 130 is formed on the first support portion 150; the support body 100 further includes a second support portion 160 disposed on a side of the second flexible film 120 facing away from the buffer chamber 130, the second support portion 160 having a second support surface covered by the second flexible film 120, and a second channel 160a extending from the second support surface and communicating with the transmission side chamber 140 being formed on the second support portion 160.

The first support portion 150 can effectively support the first flexible film 110 and the sample 900, and avoid the first flexible film 110 and the sample 900 from being deformed substantially. The second supporting portion 160 can effectively support the second flexible film 120 in the same principle, and avoid the second flexible film 120 from being deformed greatly. It should be noted that the above support should not be understood that the first support portion 150 is necessarily subjected to the gravity of the first flexible film 110 or the sample 900, or the second support portion 160 is necessarily subjected to the gravity of the second flexible film 120. The support described herein can be understood as: the supply side chamber 210, the buffer chamber 130, and the permeation side chamber 140 have gradient pressure differences, and the first support 150 and the second support 160 contact each other to cause the sample 900, the first flexible membrane 110, and the second flexible membrane 120 to have a tendency to maintain their original shapes by the pressure differences.

It is understood that an practitioner may set only any one of the first support portion 150 and the second support portion 160 to achieve a technical effect of supporting with respect to the corresponding flexible film. Ideally as demonstrated in this embodiment: the support body 100 has both the first support portion 150 and the second support portion 160.

The structure of the support 100 will be further disclosed below:

referring to fig. 1 and 3, in the present embodiment, the first sub-supporting body 101a and the second sub-supporting body 101b are each in a cylindrical shape with two ends open, and have the same inner diameter and outer diameter, i.e. the wall thicknesses of the first sub-supporting body 101a and the second sub-supporting body 101b are the same. The axial dimension of the first sub-support 101a is approximately 5mm or so, while the axial dimension of the second sub-support 101b is greater than the axial dimension of the first sub-support 101 a. The first sub-support 101a and the second sub-support 101b are bonded and fixed at the portion where the both are abutted, and are subjected to sealing treatment.

The first support 150 is disposed at one end of the first sub-support 101a, specifically, one end defining a first opening, and a first support surface and a first opening end surface on the first support 150 are kept flush to facilitate adhesion of the first flexible film 110 on the first support surface. The second support 160 is disposed at one end of the second sub-support 101b, and a second support surface on the second support 160 is kept flush with the open end surface of the second support 160 to facilitate adhesion of the second flexible film 120 on the second support surface.

In this embodiment, the first channel 150a is a first through hole, and the second channel 160a is a second through hole, where the first through hole and the second through hole are uniformly arranged, and the apertures of the first through hole and the second through hole may be uniform or non-uniform. The practitioner may also provide other shaped passages in place of the first and second through holes described above.

In addition, the second sub-supporting body 101b is fixedly connected or integrally formed with a connecting body 180, and bolt holes are formed in the connecting body 180 so that the entire supporting body 100 can be fixed on other components.

Next, a test method of a gas barrier test system applied to a sample supporting structure according to the present embodiment will be described, and in this embodiment, referring to fig. 6, the test method includes the steps of:

s100, arranging a sample 900 on a sample bearing surface 110 a;

s200, adjusting the pressure of the buffer chamber 130 to enable the buffer chamber 130 to have a first vacuum degree, and adjusting the pressure of the buffer chamber 130 to enable the transmission side chamber 140 to have a second vacuum degree, wherein the first vacuum degree is smaller than the second vacuum degree;

s300, introducing pressure-supplying gas mixed with the gas to be detected and having a preset pressure into the supply side chamber 210 so that the pressure in the supply side chamber 210 is greater than the pressure in the buffer chamber 130;

S400, determining the content of the gas to be detected in the permeation side chamber 140.

According to the testing method provided by the embodiment, the pressure difference of the two sides of the sample 900 is changed from the pressure difference of the pressure and the high vacuum degree in the traditional mode to the pressure difference of the pressure and the low vacuum degree mainly by adjusting the pressure of the buffer chamber 130, so that the risk of physical damage of the sample 900 is reduced, the reliability of the gas barrier test is improved, and the testing method is particularly suitable for high-temperature aging test in a water vapor environment.

It should be noted that the above-mentioned gas supply is mainly used for mixing with the gas to be detected and providing pressure. For example, the dry test method provided in this embodiment is a water vapor barrier test, the gas to be detected is water vapor, and the pressure-supplying gas may be a dry gas such as nitrogen.

In addition, referring to fig. 7, in this embodiment, step S200 is further refined to improve efficiency, specifically, the steps described above: adjusting the pressure of the permeate side chamber 140 so that the permeate side chamber 140 has a second vacuum, comprising:

s210, adjusting the pressure of the permeation side chamber 140 through a dry pump so that the permeation side chamber 140 has a third vacuum degree;

S220, adjusting the pressure of the transmission side chamber 140 through the cold pump so that the transmission side chamber 140 is changed from a third vacuum degree to a second vacuum degree, wherein the third vacuum degree is smaller than the second vacuum degree.

The dry pump refers to a dry mechanical pump, oil or other working medium is not contained in the pump cavity, and the dry pump can enable the permeation side cavity 140 to reach a lower vacuum degree faster. The cold pump is referred to as a condensing pump, which can make the permeation-side chamber 140 reach a higher vacuum level faster. The present embodiment combines the use of a dry pump and a cold pump, and has the advantage of faster and more efficient achievement of the target vacuum rate than using only one of the dry pump or the cold pump.

In the present embodiment, the arrangement and connection manner of the dry pump and the cold pump are not particularly limited, so that the dry pump and the cold pump are both communicated with the permeate side chamber 140, and the pressure of the permeate side chamber 140 is adjusted.

In addition, for the permeate side chamber 140, it is kept in a vacuum state during the test phase, that is, there may be a portion of the gas to be detected pumped away by the vacuum pump described above, which may cause errors in the test results.

Therefore, referring to fig. 8, in this embodiment, before testing the sample 900, the testing method further includes the steps of:

S500, adjusting the pressure of the transmission side chamber 140 so that the transmission side chamber 140 has a second vacuum degree;

s600, introducing the gas to be detected with the preset content into the permeation side chamber 140, and determining the corrected detection content of the gas to be detected in the permeation side chamber 140;

s700, obtaining an error proportion relation between the preset content and the corrected detection content according to the preset content and the corrected detection content;

wherein determining the content of the gas to be detected in the permeation side chamber 140 includes:

s410, determining the actual detection content of the gas to be detected in the permeation side chamber 140;

s420, determining the content of the gas to be detected in the permeation side chamber 140 according to the actual detected content and the error proportional relation.

In detail, before the test sample 900 is tested, the state of the permeation side chamber 140 during the test is simulated in step S500, and the gas to be detected with the preset content is directly introduced into the permeation side chamber 140 in step S600, so as to determine the corrected detection content actually detected according to the detection device 700. Ideally, all the gas to be detected that is introduced into the permeate side chamber 140 should be detected by the detecting device 700. However, as described above, there may be a portion of the gas to be detected being pumped away by the vacuum pump, so the preset level is generally greater than the corrected detection level, and the two have an error proportional relationship. This error scaling can characterize the effect of the chamber environment on the detection device 700. Therefore, in the actual test, the content of the gas to be detected in the transmission side chamber 140 can be calculated according to the error proportional relationship and the actual detected content.

Further, with respect to step S300, in the present embodiment, the preset pressure is a high pressure greater than the atmospheric pressure, but this should not be construed as limiting the preset pressure in value. The preset pressure may be any pressure greater than the pressure in the buffer chamber 130 to meet the requirements of different tests.

Example 2

The main body of the embodiment is a gas barrier property test system, in particular to a water vapor barrier property test system. The gas barrier property test system provided in the present embodiment is not limited to the water vapor barrier property test system, and may be another gas barrier property test system such as an oxygen barrier property test system.

Referring to fig. 4 and 5, in the present embodiment, the gas barrier testing system includes:

a sample support structure as described in example 1;

a supply body 200, the supply body 200 defining a supply-side chamber 210;

the gas-to-be-detected generating device 500, the gas-to-be-detected generating device 500 having at least a detection gas branch 410 in communication with the supply-side chamber 210 to supply the gas to be detected to the supply-side chamber 210;

a pressure-supplying gas generating device having at least a first gas supply branch 510 butted with the supply-side chamber 210 to supply pressure-supplying gas to the supply-side chamber 210, thereby adjusting the pressure of the gas in the supply-side chamber 210;

The vacuum generating device 600, the vacuum generating device 600 has at least a first vacuum branch 610 abutting against the transmission side chamber 140;

the detection device 700, the detection device 700 is used for detecting the content of the gas to be detected in the permeation side chamber 140.

The supply body 200 is mainly used for defining a supply side chamber 210, the gas generating device 500 to be detected is mainly used for generating gas to be detected, and the gas supplying gas generating device is used for generating gas supplying gas, and the gas supplying gas is mainly used for providing a high-pressure environment for the supply side chamber 210. The vacuum generating device 600 is used for adjusting the pressure and providing the vacuum degree. The detection device 700 is used to detect the content of the gas to be detected in the permeate side chamber 140, which may be a mass spectrometer.

In this embodiment, the gas generating apparatus 500 to be tested further has a second gas supply branch 520 interfacing with the buffer chamber 130, and the vacuum generating apparatus 600 further has a second vacuum branch 620 interfacing with the buffer chamber 130. In the testing process, the buffer chamber 130 is generally in a state of lower vacuum, so when a certain lower vacuum is required to be established for the buffer chamber 130, an operator can first establish the buffer chamber 130 at a higher vacuum by using the second vacuum branch 620, and then make the second air supply branch 520 briefly act on the buffer chamber 130, so that the buffer chamber 130 can be in a lower vacuum by repeatedly and alternately making the second air supply branch 520 and the second vacuum branch 620 act on the buffer chamber 130. It should be noted that, the gas in the buffer chamber 130 is the pressure-supplying gas provided by the second gas supply branch 520. Thereby avoiding affecting the accuracy of the test result of the test sample 900.

In this embodiment, a switch valve is disposed on the branch to facilitate the connection and disconnection between the chamber and the corresponding member. For example, the first switching valve 810 is disposed on the detection gas branch 410, the second switching valve 820 is disposed on the first gas supply branch 510, the third switching valve 830 is disposed on the second gas supply branch 520, the fourth switching valve 840 is disposed on the first vacuum branch 610, and the fifth switching valve 850 is disposed on the second vacuum branch 620. Of course, the implementation personnel can also omit the setting of the switch valve, and the chamber is in a desired state by controlling the starting or stopping of the corresponding components.

More specifically, in this embodiment, to facilitate the arrangement of the pipeline, one end of the second vacuum branch 620 is connected between two ends of the first vacuum branch 610, and the other end of the second vacuum branch 620 is connected between two ends of the second air supply branch 520, so as to simplify the arrangement manner of the pipeline.

The supply body 200 may have a large chamber shape, but the stability of the sample 900 on the sample supporting surface 110a is poor, so in this embodiment, the supply body 200 defines a second opening communicating with the supply side chamber 210, the supply body 200 has at least a testing position with respect to the support body 100, the supply body 200 and the support body 100 in the testing position are abutted, and the second opening and the first opening are abutted with each other, so that the supply body 200 and the support body 100 clamp the sample 900 on the sample supporting surface 110 a. The supply body 200 is disposed so as to be movable with respect to the support body 100 and hold the sample 900 therebetween, and thus the load bearing condition of the sample 900 can be effectively improved.

Meanwhile, to realize sample exchange of the sample 900, in this embodiment, the supply body 200 further has at least a sample exchange position, and the supply body 200 and the support body 100 at the sample exchange position are separated from each other, so that the sample bearing surface 110a is exposed for removing the sample 900 or placing the sample 900.

In more detail, referring to fig. 4, in the embodiment, the gas barrier testing system includes a testing seat 300, the testing seat 300 includes a seat body 300a and a movable cover 300b, wherein the seat body 300a and the movable cover 300b together define an external chamber 310. The supporting body 100 is disposed on the base 300a, and the supplying body 200 is movably disposed on the movable cover 300b and is movable together with the movable cover 300 b. The external chamber 310 in the test socket 300 is mainly used for interfacing with the third vacuum branch 630 with the sixth switch valve 860 in the vacuum generating device 600, so that the external chamber 310 has a certain vacuum degree. The purpose of this arrangement is that: since the supply body 200 and the support body 100 sandwich and fix the sample 900 together, a gap is necessarily formed between the supply body 200 and the support body 100, and when the support body 100 adopts the first sub-support body 101a and the second sub-support body 101b, a gap is necessarily formed between the first sub-support body 101a and the second sub-support body 101b, and due to the existence of these gaps, a part of water vapor may intrude into the transmission side chamber 140 from the side portion of the sample 900 or the second flexible film 120, thereby affecting the final test result. The interface between the supply body 200 and the support body 100 is accommodated in the vacuum environment formed by the external chamber 310, so that this situation can be effectively avoided.

Here, in the present embodiment, the supporting body 100 is bolted to the base body 300a through the connecting body 180 described above, and the movable cover 300b is slidably disposed on the movable cover 300b with respect to the movable cover 300 b. The movable cover 300b can move relative to the base 300a, so that the whole test base 300 can be switched between a combined state and an opened state. When the test seat 300 is in the coupled state, the movable cover 300b and the seat body 300a are coupled to each other, so that the external chamber 310 is in the closed state, and at this time, the supply body 200 can be switched between the testing position and the sample changing position. When the test seat 300 is in the opened state, the movable cover 300b and the seat body 300a are separated from each other. Since the supply body 200 moves together with the movable cover 300b, the supply body 200 is at the sample exchange position. Of course, other configurations of the test seat 300 may be employed by an practitioner, as the application is not particularly limited.

Having described the structure of the test system, the test method applied to the gas barrier test system according to the present embodiment will be further described below, and specifically includes:

s10, performing a test step on the sample 900:

s20, performing a sample changing step on the tested sample 900:

Step S10 can be implemented by an operator using the test method as described in embodiment 1, so that step S10 will not be described in detail, and step 20 will be further described below.

Referring to fig. 5, step S20 specifically includes:

s21, closing the first and sixth switching valves 810 and 860, and switching the supply body 200 to the sample exchange position so that the external chamber 310 and the supply-side chamber 210 communicate with each other;

s22, the test seat 300 is in an open state and the sample 900 is replaced, and in the process of replacing the sample 900, the second switch valve 820 is opened and the pressure-supplying gas generator continuously generates pressure-supplying gas, so that the pressure-supplying gas passes through the supply side chamber 210 to cover the sample bearing surface 110a;

s23, the test seat 300 is in a combined state, the second switch valve 820 is closed, and the sixth switch valve 860 is opened, so that the external chamber 310 and the supply side chamber 210 are in a negative pressure state;

s24, reducing the residual gas to be measured in the permeation side chamber 140.

In step S22, the purpose of continuously generating the supplied gas by the test generating device during the replacement of the sample 900 is to: a gas curtain is formed to block the intrusion of the external impurity gas into the support 100. It is desirable to use nitrogen as the gas supply and the first flexible membrane 110 is made of polyimide polymer. This is because: the present embodiment is applied to the water vapor barrier property test, and the first flexible film 110 has a high water vapor barrier capability in a nitrogen environment, so that the invasion of external water vapor into the permeation-side chamber 140 can be better prevented when the sample 900 is replaced.

In step S23, the effect of the gas flowing from the atmosphere into the external chamber 310 and the supply side chamber 210 is reduced when the test seat 300 is in the open state.

In step S24, after the end of one test, if too much water vapor is contained in the transmission side chamber 140 and the water vapor content is still in the rising state, the test result is greatly affected. The amount of water vapor should generally be divided to the detection limit, and the effect of water vapor is reduced to within the fluctuation range of the detection error, which generally takes 2 to 5 days. The residual amount of water vapor in the next test can be predicted according to the rule that the curve formed by the residual amount of water vapor and time is close to an exponential curve, and then the predicted residual amount of water vapor is subtracted when the water vapor content is calculated after the next test, so that the water vapor content transmitted by the sample 900 only can be obtained.

While the basic concepts have been described above, it will be apparent to those skilled in the art that the foregoing detailed disclosure is by way of example only and is not intended to be limiting. Although not explicitly described herein, various modifications, improvements, and adaptations of the present application may occur to one skilled in the art. Such modifications, improvements, and modifications are intended to be suggested within this application, and are therefore within the spirit and scope of the exemplary embodiments of this application.

Meanwhile, the present application uses specific words to describe embodiments of the present application. Reference to "one embodiment," "an embodiment," and/or "some embodiments" means that a particular feature, structure, or characteristic is associated with at least one embodiment of the present application. Thus, it should be emphasized and should be appreciated that two or more references to "an embodiment" or "one embodiment" or "an alternative embodiment" in various positions in this specification are not necessarily referring to the same embodiment. Furthermore, certain features, structures, or characteristics of one or more embodiments of the present application may be combined as suitable.

Likewise, it should be noted that in order to simplify the presentation disclosed herein and thereby aid in understanding one or more application embodiments, various features are sometimes grouped together in a single embodiment, figure, or description thereof for the purpose of streamlining the disclosure. This method of disclosure, however, is not intended to imply that more features than are presented in the claims are required for the subject application. Indeed, less than all of the features of a single embodiment disclosed above.

In some embodiments, numbers describing the components, number of attributes are used, it being understood that such numbers being used in the description of embodiments are modified in some examples by the modifier "about," approximately, "or" substantially. Unless otherwise indicated, "about," "approximately," or "substantially" indicate that the number allows for ±% variation. Accordingly, in some embodiments, numerical parameters set forth in the specification and claims are approximations that may vary depending upon the desired properties sought to be obtained by the individual embodiments. In some embodiments, the numerical parameters should take into account the specified significant digits and employ a method for preserving the general number of digits. Although the numerical ranges and parameters set forth herein are approximations that may be employed in some embodiments to confirm the breadth of the range, in particular embodiments, the setting of such numerical values is as precise as possible.

For each patent, patent application publication, and other material, such as articles, books, specifications, publications, documents, etc., cited in this application, the entire contents of which are hereby incorporated by reference into this application, except for the application history documents which are inconsistent or conflict with the contents of this application, and for documents which have limited the broadest scope of the claims of this application (currently or hereafter attached to this application). It is noted that the descriptions, definitions, and/or terms used in the subject matter of this application are subject to the use of descriptions, definitions, and/or terms in case of inconsistent or conflicting disclosure.

Claims (12)

1. A gas barrier testing system, comprising:

a support defining a first cavity having a first opening for interfacing with the supply side chamber with each other;

a first flexible film and a second flexible film, wherein the first flexible film is combined on the end face of the first opening to close the first opening, the surface of the first flexible film, which is opposite to the supporting body, forms a sample bearing surface for bearing a sample, and the second flexible film extends into the first cavity; the space between the first flexible membrane and the second flexible membrane of the first cavity forms a buffer cavity which is in a closed shape and has adjustable pressure, and the space of the first cavity on one side of the second flexible membrane, which is opposite to the buffer cavity, forms a permeation side cavity.

2. The gas barrier test system of claim 1, wherein the film thickness of the first flexible film is greater than the film thickness of the second flexible film, and/or the film thickness of the second flexible film is 40 to 400um.

3. The gas barrier testing system of claim 1 or 2, wherein the support comprises a first sub-support defining the first opening and having a first sub-cavity and a second sub-support having a second sub-cavity, the first and second sub-supports interfacing with each other such that the first and second sub-cavities communicate and at least partially form the first cavity, the second flexible membrane being sandwiched between the first and second sub-supports.

4. The gas barrier test system of claim 1, wherein the first flexible film has an air permeability of 0.1 to 10cm ³ /(m ³ 24 h.bar) the second flexible film having an air permeability of 0.1 to 10cm ³ /(m ³ 24 h.bar); and/or the number of the groups of groups,

the material of the first flexible film is selected from at least one of polyimide, polyamide, polycarbonate, polyether ether ketone, polyether sulfone, polyamide imide, polyethylene, polypropylene, polyethylene terephthalate, polyethylene naphthalate, polyvinyl chloride, polyvinylidene chloride, polyacrylonitrile, polystyrene, polyphenylene sulfide, polytetrafluoroethylene and polyhexamethylene adipamide, and the material of the second flexible film is selected from at least one of polyimide, polyamide, polycarbonate, polyether ether ketone, polyether sulfone, polyamide imide, polyethylene, polypropylene, polyethylene terephthalate, polyethylene naphthalate, polyvinyl chloride, polyvinylidene chloride, polyacrylonitrile, polystyrene, polyphenylene sulfide, polytetrafluoroethylene and polyhexamethylene adipamide.

5. The gas barrier test system according to claim 1, wherein the support body further includes a first support portion provided between the first flexible film and the second flexible film, the first support portion having a first support surface covered by the first flexible film, the first support portion having formed thereon a first passage extending from the first support surface and communicating with the buffer chamber; and/or

The support body further comprises a second support part arranged on one side of the second flexible film, which is opposite to the buffer chamber, the second support part is provided with a second support surface covered by the second flexible film, and a second channel which extends from the second support surface and is communicated with the transmission side chamber is formed on the second support part.

6. The gas barrier test system of claim 1, further comprising:

a supply body defining the supply-side chamber;

the gas generating device to be detected is at least provided with a detection gas branch which is in butt joint with the buffer chamber so as to provide the gas to be detected for the buffer chamber;

the pressure-supplying gas generating device is provided with at least a first gas supply branch which is in butt joint with the buffer chamber so as to supply pressure-supplying gas to the buffer chamber, thereby adjusting the pressure in the supply side chamber;

The vacuum generating device is provided with at least a first vacuum branch which is in butt joint with the permeation side cavity;

the detection device is used for detecting the content of the gas to be detected in the permeation side cavity.

7. The gas barrier testing system of claim 6, wherein the gas generating apparatus to be tested further has a second gas supply branch interfacing with the buffer chamber, and the vacuum generating apparatus further has a second vacuum branch interfacing with the buffer chamber.

8. The gas barrier testing system of claim 6, wherein said supply body defines a second opening in communication with said supply-side chamber, said supply body having at least a testing position and a sample exchange position relative to said support body, said supply body and said support body in said testing position being in abutment with each other, and said second opening and said first opening being in abutment with each other such that said supply body and said support body grip said sample on said sample-bearing surface, said supply body and said support body in said sample exchange position being separated to reveal said sample-bearing surface.

9. The gas barrier testing system of claim 8, wherein the gas barrier testing system comprises a test seat defining an external chamber having at least a closed state, the support body, the supply body being coupled to the test seat, and the support body defining the first opening and the supply body defining the second opening extending into the external chamber, the vacuum generating device further having at least a third vacuum branch interfacing with the external chamber.

10. A gas barrier property testing method using the gas barrier property testing system according to any one of claims 1 to 9, comprising the steps of:

disposing a sample on the sample-bearing surface;

adjusting the pressure of the buffer chamber to enable the buffer chamber to have a first vacuum degree, and adjusting the pressure of the transmission side chamber to enable the transmission side chamber to have a second vacuum degree, wherein the first vacuum degree is smaller than the second vacuum degree;

introducing gas to be detected into the supply side chamber so that the pressure in the supply side chamber is higher than the pressure in the buffer chamber;

And determining the content of the gas to be detected in the permeation side cavity.

11. The method of claim 10, wherein adjusting the pressure of the permeate-side chamber to provide the permeate-side chamber with a second vacuum level comprises:

the pressure of the permeation side chamber is adjusted through a dry pump so that the permeation side chamber has a third vacuum degree, the pressure of the permeation side chamber is adjusted through a cold pump so that the permeation side chamber is changed from the third vacuum degree to the second vacuum degree, and the third vacuum degree is smaller than the second vacuum degree.

12. The gas barrier testing method according to claim 10, wherein before the test is performed on the test specimen, the testing method further comprises the steps of:

adjusting the pressure of the permeate side chamber so that the permeate side chamber has the second vacuum;

introducing the gas to be detected with preset content into the permeation side cavity, and determining the corrected detection content of the gas to be detected in the permeation side cavity;

obtaining an error proportional relation between the preset content and the corrected detection content according to the preset content and the corrected detection content;

Wherein the determining the content of the gas to be detected in the permeation-side chamber includes:

determining the actual detection content of the gas to be detected in the permeation side cavity;

and determining the content of the gas to be detected in the permeation side cavity according to the actual detection content and the error proportion relation.