CN113466101A - Permeability detection equipment and detection method - Google Patents
Permeability detection equipment and detection method Download PDFInfo
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- CN113466101A CN113466101A CN202110706803.9A CN202110706803A CN113466101A CN 113466101 A CN113466101 A CN 113466101A CN 202110706803 A CN202110706803 A CN 202110706803A CN 113466101 A CN113466101 A CN 113466101A
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- 238000001514 detection method Methods 0.000 title claims abstract description 227
- 230000035699 permeability Effects 0.000 title claims abstract description 90
- 238000009825 accumulation Methods 0.000 claims abstract description 105
- 239000007789 gas Substances 0.000 claims description 162
- 230000008595 infiltration Effects 0.000 claims description 62
- 238000001764 infiltration Methods 0.000 claims description 62
- 238000009434 installation Methods 0.000 claims description 33
- 238000005303 weighing Methods 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 18
- 230000008569 process Effects 0.000 claims description 15
- 238000005259 measurement Methods 0.000 claims description 8
- 238000004891 communication Methods 0.000 claims description 5
- 238000001228 spectrum Methods 0.000 claims description 5
- 238000012935 Averaging Methods 0.000 claims description 2
- 238000011160 research Methods 0.000 abstract description 5
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 115
- 239000012466 permeate Substances 0.000 description 92
- 239000010408 film Substances 0.000 description 40
- 230000000875 corresponding effect Effects 0.000 description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 230000004888 barrier function Effects 0.000 description 7
- 238000009792 diffusion process Methods 0.000 description 6
- 230000003204 osmotic effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000003380 quartz crystal microbalance Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229920006280 packaging film Polymers 0.000 description 2
- 239000012785 packaging film Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
- G01N15/0826—Investigating permeability by forcing a fluid through a sample and measuring fluid flow rate, i.e. permeation rate or pressure change
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/0806—Details, e.g. sample holders, mounting samples for testing
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- Immunology (AREA)
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Abstract
The invention relates to a permeability detection device and a permeability detection method. The permeability detection apparatus includes: an air inlet cavity; the sample collecting device comprises a plurality of groups of permeation cavities, a plurality of groups of permeation cavities and a sample collecting cavity, wherein the permeation cavities are connected with an air inlet cavity; the detection cavity is connected with the multiple groups of permeation cavities, an accumulation valve is arranged between the permeation cavities and the detection cavity, and when the accumulation valve is opened, the detection cavity is communicated with the corresponding permeation cavity; and the mass spectrometer is communicated with the detection cavity. The device can detect the permeability of the high-barrier-rate film, can deepen the understanding of the permeability of the film, and is favorable for the follow-up research on the high-barrier-rate film.
Description
Technical Field
The invention relates to the technical field of film permeability detection, in particular to permeability detection equipment and a permeability detection method.
Background
For example, when the OLED device is packaged by using the packaging film, the packaging film is required to have a high gas barrier rate so as to prevent gases such as water vapor from permeating into the OLED device and affecting the service performance of the OLED device. Therefore, it is very important to detect and study the permeability of the film. However, in the related art, when the permeability of some films with high barrier rate is detected, the detection precision of some existing detection devices is limited due to the fact that the magnitude of the permeability is too tiny, and the permeability of the films is difficult to measure.
Disclosure of Invention
Based on the above, the invention provides a permeability detection device, which has high detection sensitivity and can detect the permeability of some high-barrier-rate films with low permeability, so that the understanding of the permeability of the films is further deepened, the subsequent research on the high-barrier-rate films is facilitated, the detection of the permeability of gases passing through various films can be realized, and the detection of the permeability of various gases passing through the films can also be realized.
A permeability detection apparatus comprising:
an air inlet cavity;
the permeation cavities are all connected with the air inlet cavity, an air inlet valve is arranged between each permeation cavity and the corresponding air inlet cavity, when the air inlet valve is opened, the air inlet cavities are communicated with the corresponding permeation cavities, and a first sample installation area for installing a first sample is arranged in each permeation cavity;
the detection cavity is connected with a plurality of groups of permeation cavities, an accumulation valve is arranged between the permeation cavities and the detection cavity, and when the accumulation valve is opened, the detection cavity is communicated with the corresponding permeation cavity;
a mass spectrometer in communication with the detection cavity.
In one embodiment, the infiltration cavity comprises an infiltration cavity air inlet section and an infiltration cavity accumulation section, the infiltration cavity air inlet section is connected with the air inlet cavity, the infiltration cavity accumulation section is connected with the detection cavity, the first sample installation area is formed between the infiltration cavity air inlet section and the infiltration cavity accumulation section, and a standard flow guide device is installed at one first sample installation area.
In one embodiment, the infiltration cavity comprises an infiltration cavity air inlet section and an infiltration cavity accumulation section, the infiltration cavity air inlet section is connected with the air inlet cavity, the infiltration cavity accumulation section is connected with the detection cavity, the first sample installation area is formed between the infiltration cavity air inlet section and the infiltration cavity accumulation section, in at least one infiltration cavity, a weighing component is arranged in the infiltration cavity air inlet section, the weighing component is provided with a second sample installation area, and the second sample installation area is used for placing a second sample.
In one embodiment, an infrared assembly is arranged in a region corresponding to at least one permeation cavity, and comprises a light source, an incident channel, an emergent channel and a spectrometer;
the permeation cavity comprises a permeation cavity air inlet section and a permeation cavity accumulation section, the permeation cavity air inlet section is connected with the air inlet cavity, the permeation cavity accumulation section is connected with the detection cavity, and the first sample installation area is formed between the permeation cavity air inlet section and the permeation cavity accumulation section;
the incident channel and the emergent channel are communicated with the infiltration cavity accumulation section, incident light rays emitted by the light source enter the infiltration cavity accumulation section through the incident channel and reach the first sample installation area, and emergent light rays reflected by the first sample enter the spectrometer through the emergent channel.
In one embodiment, the permeation cavity comprises a permeation cavity air inlet section and a permeation cavity accumulation section, the permeation cavity air inlet section is connected with the air inlet cavity, the permeation cavity accumulation section is connected with the detection cavity, and the first sample installation area is formed between the permeation cavity air inlet section and the permeation cavity accumulation section;
at least one infiltration cavity corresponds the region and is equipped with infrared subassembly, infrared subassembly includes light source, incident passageway, exit channel and spectrum appearance, the incident passageway exit channel all with infiltration cavity accumulation section intercommunication, the incident light that the light source sent passes through the incident passageway gets into infiltration cavity accumulation section and reachs first sample installing zone, the process emergent light after the first sample reflection passes through exit channel gets into the spectrum appearance, it has the weighing component to stretch into in the infiltration cavity section of admitting air, be equipped with second sample installing zone on the weighing component, second sample installing zone is used for placing the second sample.
Above-mentioned permeability check out test set is provided with multiunit infiltration cavity, and all is connected through the valve of admitting air between every group infiltration cavity and the chamber of admitting air, and every group infiltration cavity all is connected through the accumulation valve between the chamber with detecting, detects chamber and mass spectrograph intercommunication. When detecting, open the air inlet valve, close the accumulation valve, alright make the gas in the inlet chamber body get into in the infiltration cavity and carry out the infiltration accumulation, after the infiltration accumulation reaches a certain amount, open the accumulation valve, alright make the gas that accumulates in the infiltration cavity get into in the detection cavity, and then get into the mass spectrograph, record the pressure in the detection cavity and obtain the permeability through the mass spectrograph. Because the gas enters the detection cavity after being accumulated in the permeation cavity for a period of time, less gas can be gradually accumulated and enriched, so that the mass spectrometer is easier to detect the gas, and the detection of the permeation rate of the film with high barrier rate is realized. In addition, because a plurality of groups of permeation cavities are arranged, each group of permeation cavities can work independently, if different first samples are arranged in the first sample installation area in each group of permeation cavities, the detection of the permeation rate of gas passing through various films can be realized on the same equipment; if the same first sample is installed in the first sample installation area in each group of permeation cavities, but different gases are successively introduced into the gas inlet cavity, the detection of the permeability of various gases through the same first sample can be realized on the same equipment, so that the detection is more convenient and faster. In addition, if the same first sample is installed in the first sample installation area in each group of permeation cavities, the same gas is always introduced into the air inlet cavity, and by arranging the multiple groups of permeation cavities and the multiple first samples, detection errors can be reduced, and the accuracy of detection results is improved.
The invention also provides a permeability detection method, which can be used for detecting the permeability of the high-barrier-rate films with lower permeability, so that the understanding of the permeability of the films is further deepened, the subsequent research on the high-barrier-rate films is facilitated, the detection of the permeability of the gas passing through various films can be realized, and the detection of the permeability of the gas passing through the films can also be realized.
The permeability detection method comprises the following steps:
s10, arranging a plurality of groups of permeation cavities;
s20 selecting at least one set of the infiltration cavities and installing a first sample into the selected infiltration cavity;
s30, introducing gas into the permeation cavity selected in the S20 for permeation accumulation;
s40, releasing the gas accumulated in the permeation cavity into the detection cavity, and detecting through a mass spectrometer.
In one embodiment, in S20, at least two sets of the permeation cavities are selected, and the first sample installed in each set of the permeation cavities is the same;
in S40, releasing the gas accumulated in each group of permeation cavities into the detection cavities in sequence, and evacuating the gas exhausted from the previous group in the detection cavities between two adjacent groups of detections; and averaging the results of each group detected by the mass spectrometer.
In one embodiment, in S20, at least two groups of the permeation cavities are selected, and the first sample installed in each group of the permeation cavities is different;
in S30, the gas introduced into each group of permeation cavities is the same;
and S40, sequentially releasing the gas accumulated in each group of permeation cavities into the detection cavity, and evacuating the gas exhausted from the previous group in the detection cavity between two adjacent groups of detections.
In one embodiment, in S20, at least two sets of the permeation cavities are selected, and the first sample installed in each set of the permeation cavities is the same;
in S30, introducing different gases into each group of permeation cavities for permeation accumulation;
and S40, sequentially releasing the gas accumulated in each group of permeation cavities into the detection cavity, and evacuating the gas exhausted from the previous group in the detection cavity between two adjacent groups of detections.
In one embodiment, a standard flow guide device is arranged in one of the infiltration cavities, and data measured by the mass spectrometer are calibrated through the standard flow guide device.
In one embodiment, the method for calibrating the mass spectrometer by the standard flow guide device comprises the following steps:
s01, installing the standard conductance device as the first sample in the selected infiltration cavity;
s02, measuring the pressure of the introduced gas, calculating the gas flow, and calculating the permeability according to the obtained gas flow;
s03, introducing gas into the permeation cavity selected in the S01 for permeation accumulation;
s04, releasing the gas accumulated in the permeation cavity into the detection cavity, and detecting through the mass spectrometer;
s05 correlating the mass spectrometer measurements with the calculated permeabilities in S02;
s06, adjusting the pressure of the introduced gas, repeating S02 to S05 until the preset measuring range data of the mass spectrometer are covered, and establishing the corresponding relation between the data measured by the mass spectrometer and the permeability calculated by the standard conductance device;
s07 finds the corresponding standard data in the correspondence established in S06 using the data measured by the mass spectrometer described in S40.
The permeability detection method is provided with a plurality of groups of permeation cavities, when detection is carried out, after the permeation cavities are selected and the first sample is installed, gas enters the permeation cavities to carry out permeation accumulation, after the gas in the permeation cavities permeates and accumulates to a certain amount, the gas accumulated in the corresponding permeation cavities is released and enters the detection cavities, and the pressure in the detection cavities is measured through the mass spectrometer and the permeability is obtained. Because the gas enters the detection cavity after being accumulated in the permeation cavity for a period of time, less gas can be gradually accumulated and enriched, so that the mass spectrometer is easier to detect the gas, and the detection of the permeation rate of the film with high barrier rate is realized. In addition, because be provided with multiunit infiltration cavity, every group infiltration cavity can the autonomous working, and the first sample of installation is different in multiunit infiltration cavity, perhaps the gas that lets in is different, can realize the permeability under the multiple condition on same equipment and detect, can make and detect convenient and fast more.
Drawings
FIG. 1 is a front view of a permeability detection apparatus in one embodiment of the present invention;
FIG. 2 is a schematic view of the overall structure of the permeability detection apparatus of FIG. 1;
FIG. 3 is a schematic structural diagram of the permeability detection apparatus of FIG. 2 after various permeation cavities are hidden;
FIG. 4 is a schematic structural diagram of each permeation chamber of the permeation rate detection apparatus of FIG. 2;
FIG. 5 is a schematic diagram of one of the permeation chambers of the permeability detection apparatus of FIG. 4;
fig. 6 is a schematic diagram of the internal structure of one of the permeation chambers of the permeability detection apparatus of fig. 5.
Reference numerals:
the device comprises an air inlet cavity 100, an air inlet main pipe 110, an air inlet branch pipe 120, a vacuumizing upper interface 130 and a film vacuum gauge 140;
a first permeate cavity 200, a first permeate cavity gas inlet section 210, a first permeate cavity accumulating section 220;
a second permeate chamber 300;
a third permeate chamber 400, a third permeate chamber gas inlet section 410, a third permeate chamber accumulation section 420, and a standard conductance device 430;
the fourth infiltration cavity 500, the fourth infiltration cavity gas inlet section 510, the fourth infiltration cavity accumulating section 520, the placing table 530, the weighing assembly 540, the probe 541, the groove 542, the observation window 550, the infrared light incident channel 561, the laser incident channel 562, the exit channel 563, the first reflection box 570, the first light inlet window 571, the second light inlet window 572, the second reflection box 580, and the light outlet window 581;
the device comprises a detection cavity 600, a detection main pipe 610, a detection branch pipe 620 and a vacuumizing lower interface 630;
an intake valve 810, an intake valve interface 811, an accumulation valve 820, and an accumulation valve interface 821.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
Furthermore, the terms "first", "second" and "first" 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" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like as used herein are for illustrative purposes only and do not denote a unique embodiment.
Referring to fig. 1 and fig. 2, a permeability detection apparatus according to an embodiment of the present invention includes an air inlet chamber 100, a detection chamber 600, a mass spectrometer 710, and a plurality of sets of permeation chambers. The multiple groups of permeation cavities are arranged between the air inlet cavity 100 and the detection cavity 600, one end of each group of permeation cavities is connected with the air inlet cavity 100, the other end of each group of permeation cavities is connected with the detection cavity 600, first sample installation areas are arranged in each group of permeation cavities, and the first sample installation areas are used for installing first samples. An air inlet valve 810 is arranged between the infiltration cavity and the air inlet cavity 100, when the air inlet valve 810 is opened, the air inlet cavity 100 is communicated with the corresponding infiltration cavity, and the gas in the air inlet cavity 100 can enter the corresponding infiltration cavity; when the inlet valve 810 is closed, the inlet chamber 100 is no longer in communication with the corresponding permeate chamber and gas cannot flow between the two. An accumulation valve 820 is arranged between the permeation cavity and the detection cavity 600, when the accumulation valve 820 is opened, the permeation cavity is communicated with the corresponding permeation cavity, and gas accumulated in the corresponding permeation cavity can flow into the detection cavity 600; when the accumulation valve 820 is closed, the detection chamber 600 is no longer in communication with the corresponding permeation chamber and gas cannot flow between the two. The mass spectrometer 710 is in communication with the detection chamber 600 and can detect the gas in the detection chamber 600. When the air inlet valve 810 is opened and the accumulation valve 820 is closed, the gas in the air inlet cavity 100 enters the corresponding permeation cavity, the gas permeates the first sample at the first sample installation area, and the gas permeating the first sample cannot be discharged due to the closing of the accumulation valve 820, so that the gas is gradually accumulated and enriched in the permeation cavity. When the accumulation valve 820 is opened, the gas accumulated and enriched in the permeation cavity is discharged into the detection cavity 600, and then can be detected by the mass spectrometer 710, and the pressure in the detection cavity 600 is measured by the mass spectrometer 710 and the permeability is obtained.
In the invention, the gas enters the detection cavity 600 after being accumulated in the permeation cavity for a period of time, and when a film with higher barrier rate is detected, the gas amount permeating through the first sample is very small due to the lower permeability, and the original less gas can be gradually accumulated and enriched due to the accumulation for a period of time, so that the gas can be easily detected by the mass spectrometer 710, and the detection sensitivity of the gas is improved. In addition, because be provided with multiunit infiltration cavity, every group infiltration cavity can the autonomous working, and the first sample of installation is different in multiunit infiltration cavity, perhaps the gas that lets in is different, can realize the permeability under the multiple condition on same equipment and detect, can make and detect convenient and fast more. For example, if different first samples are installed in the first sample installation areas in each group of permeation cavities, the detection of the permeation rate of gas through various membranes can be realized on the same equipment. If the same first sample is installed in the first sample installation area in each group of permeation cavities, but different gases are sequentially introduced into the gas inlet cavity 100, the detection of the permeability of various gases through the same first sample can be realized on the same equipment, so that the detection is more convenient and faster. If the same first sample is installed in the first sample installation area in each group of permeation cavities, the same gas is always introduced into the gas inlet cavity 100, and by arranging a plurality of groups of permeation cavities and a plurality of first samples, detection errors can be reduced, and the accuracy of detection results is improved.
Referring to fig. 2 to 4, in particular, the air inlet cavity 100 includes an air inlet main pipe 110 and a plurality of air inlet branch pipes 120, the plurality of air inlet branch pipes 120 are all communicated with the air inlet main pipe 110, and the air inlet is located on the air inlet main pipe 110. An inlet valve 810 is connected to an end of each of the plurality of inlet manifolds 120, an inlet valve port 811 is disposed on the inlet valve 810, and the inlet valve port 811 at the end of each inlet manifold 120 is connected to a corresponding one of the permeate cavities. The main inlet pipe 110 is further provided with an upper vacuum port 130, and the upper vacuum port 130 can be connected to a vacuum pump, so as to vacuum the inlet chamber 100 and the channel communicated therewith. The main gas inlet pipe 110 is further provided with a film vacuum gauge 140 for measuring the pressure of the introduced gas.
Similarly, the detection chamber 600 includes a detection main pipe 610 and a plurality of detection branch pipes 620, each of the plurality of detection branch pipes 620 is communicated with the detection main pipe 610, and the detection main pipe 610 is communicated with the mass spectrometer 710. An accumulation valve 820 is connected to each of the plurality of detection branch pipes 620, an accumulation valve connector 821 is arranged on each accumulation valve 820, and the accumulation valve connector 821 on each detection branch pipe 620 is connected with a corresponding permeation cavity. The detection main pipe 610 is further provided with a vacuumizing lower interface 630, and the vacuumizing lower interface 630 can be connected with a vacuum pump, so that the detection cavity 600 and a channel communicated with the detection cavity are vacuumized. Preferably, the detection main pipe 610 is provided with a plurality of vacuuming lower interfaces 630, which can be connected with a vacuum pump at the same time to accelerate the vacuuming process.
Referring to fig. 2-4, in some embodiments, the permeation chamber includes a permeation chamber gas inlet section connected to the gas inlet chamber 100 and a permeation chamber accumulation section connected to the detection chamber 600, with a first sample mounting region formed between the permeation chamber gas inlet section and the permeation chamber accumulation section. An ionization gauge 720 is connected to each permeate chamber and can be used to measure the gas pressure within the permeate chamber. In the embodiment shown in the drawings, four permeation cavities are provided, namely a first permeation cavity 200, a second permeation cavity 300, a third permeation cavity 400 and a fourth permeation cavity 500, and four inlet branch pipes 120 and four detection branch pipes 620 are correspondingly provided. Of course, in other embodiments, the number of permeate cavities may be increased or decreased.
Specifically, the first osmotic chamber 200 includes a first osmotic chamber inlet section 210 and a first osmotic chamber accumulation section 220, the top end of the first osmotic chamber inlet section 210 is connected to an inlet valve port 811 at the end of one of the inlet branches 120, and the bottom end of the first osmotic chamber accumulation section 220 is connected to an accumulation valve port 821 on one of the detection branches 620. The first permeate chamber gas inlet section 210 is located above the first permeate chamber accumulating section 220 with a gap therebetween forming the first sample mounting area as previously described. A first sample can be placed in the gap and the first permeate chamber gas inlet section 210 can be fixedly connected to the first permeate chamber accumulating section 220, thereby clampingly securing the first sample therebetween. If the inlet valve port 811 corresponding to the first permeation cavity 200 is opened and the accumulation valve port 821 corresponding to the first permeation cavity 200 is closed, the gas in the inlet cavity 100 enters the inlet section 210 of the first permeation cavity and gradually flows downwards, and when the gas flows to the first sample, part of the gas permeates the first sample to reach the accumulation section 220 of the first permeation cavity and is accumulated in the accumulation section 220 of the first permeation cavity. After a certain amount of gas has been accumulated, the corresponding accumulation valve port 821 of the first permeate chamber 200 is opened, and the gas accumulated in the first permeate chamber accumulation section 220 will flow downward into the detection chamber 600. The first osmosis chamber 200 has the same structure as the second osmosis chamber 300, and the structure of the second osmosis chamber 300 is not described in detail.
Referring to fig. 2-4, in some embodiments, a standard conductance device 430 is mounted at the first sample mounting region of one of the permeation chambers. Specifically, in the embodiment shown in the drawings, the third permeate cavity 400 includes a third permeate cavity gas inlet section 410 and a third permeate cavity accumulating section 420, and the third permeate cavity 400 has a structure similar to that of the first permeate cavity 200, except that a standard conductance device 430 is disposed in a gap between the third permeate cavity gas inlet section 410 and the third permeate cavity accumulating section 420. The Standard conductance device 430(Standard conductor element) is a micro-nano porous plug structure made of stainless steel by sintering, the average pore diameter of the micro-nano porous plug structure is less than 1 micron, and the micro-nano porous plug structure can generate a molecular flow effect under a preset pressure condition and maintain constant conductance. When the mass spectrometer 710 is used for detection, the basic principle is to measure the weak gas signal penetrating through the membrane by the related vacuum metering device to indirectly obtain the corresponding permeability value. The permeability value corresponding to the data measured by the mass spectrometer 710 is generally susceptible to many factors, and may have a large error and may not result in an accurate permeability. In this embodiment, the standard conductance device 430 may be regarded as a standard barrier sample with high barrier property, and the mass spectrometer 710 is calibrated by using the standard conductance device 430, so that an error may be reduced, and accuracy of a detection result may be improved. The specific calibration process will be described in the following method embodiments.
In some embodiments, in at least one infiltration chamber, a weighing component 540 is arranged in the air inlet section of the infiltration chamber, and a second sample installation area is arranged on the weighing component 540 and used for placing a second sample. Specifically, referring to fig. 4 to 6, the fourth permeation cavity 500 is cylindrical and hollow to form a fourth permeation cavity air inlet section 510 and a fourth permeation cavity accumulation section 520, a placing table 530 is disposed between the fourth permeation cavity air inlet section 510 and the fourth permeation cavity accumulation section 520, the placing table 530 forms a first sample installation area, the first sample can be placed on the placing table 530, and the weighing component 540 is located in the fourth permeation cavity air inlet section 510. When the inlet valve 810 corresponding to the fourth osmosis chamber 500 is opened, the gas enters the inlet section of the osmosis chamber from the inlet chamber 100, and passes through the second sample placed on the weighing assembly 540, so that the weight of the second sample is increased.
As is well known to those skilled in the art, permeation processes include adsorption, dissolution, diffusion and desorption. Taking the direction of gas permeation through the membrane as the first direction (here, only the macroscopic direction is shown, and actually, the permeation direction of each gas molecule may have an angle with the first direction), when the gas reaches the membrane surface, the gas will be adsorbed on the surface and partially dissolved on the membrane surface. In the dissolved part, part of the solution can diffuse along the first direction to reach the other side of the film, and the solution continuously moves towards the first direction to gradually desorb the film, so that the whole permeation process is completed; meanwhile, the adsorption side is adsorbed by the film and dissolved in the gas, and part of the gas is continuously desorbed from the surface of the film along the reverse direction of the first direction. In this embodiment, the first direction is a downward direction at an angle shown in the drawing, when the gas flows downward, adsorption, diffusion and desorption occur at the adsorption side of the second sample, and the weighing component 540 weighs the weight increase of the second sample in real time, so as to draw a change curve of the weight increase with time. And correspondingly calculating the change curve according to Fick's law to obtain a corresponding diffusion coefficient. The diffusion coefficient is a very important infiltration parameter, which is helpful for further understanding the infiltration intermediate process. The calculation of the diffusion coefficient according to Fick's law is common knowledge in the art and will not be described herein.
In some embodiments, the second sample and the first sample may be the same film, and the apparatus may be used to perform weighing and permeability measurements simultaneously, and in use, the weighing and permeability measurements may be performed in the fourth permeate chamber gas inlet section 510 and the detection chamber 600, respectively. Therefore, the diffusion coefficient and the permeability can be simultaneously detected by using only one channel of one device, the number of devices required to be used can be reduced, the detection flow is simplified, and the detection time is shortened. Of course, the weighing test may be performed only in the fourth permeate chamber inlet section 510, or the permeability test may be performed only in the test chamber 600. In other embodiments, the second sample and the first sample may be two films, and one film may be weight tested and the other permeability tested using the apparatus.
In some embodiments, the gas introduced into the gas inlet cavity 100 is water vapor. The weighing component 540 is a quartz crystal microbalance, and the probe 541 of the quartz crystal microbalance is a quartz crystal. The quartz crystal microbalance is a high-sensitivity quality detection instrument based on the principle of quartz crystal piezoelectric effect, the test precision can reach ng level, and the quality change in the microscopic process can be tracked and monitored well on line. The probe 541 of the quartz crystal microbalance extends into the fourth permeation cavity gas inlet section 510, the probe 541 is suspended in the fourth permeation cavity gas inlet section 510, a second sample is placed on the probe 541, and the gas passes through the probe 541 in the process of entering the fourth permeation cavity accumulation section 520 from the fourth permeation cavity gas inlet section 510, so that the weight of the second sample placed on the probe 541 is increased.
In some embodiments, a recess 542 recessed downward is provided at the top surface of the probe 541, and a second sample can be placed in the recess 542. Can cut out the sample into with recess 542 shape assorted shape, it can to put into recess 542 with it again. In the embodiment shown in the drawings, the shape of the groove 542 is a regular hexagon, but is not limited thereto, and may be a triangle, a circle, an ellipse, or another polygon. The depth of the groove 542 is ensured to be larger than the thickness of the sample, so that the sample is not easy to fall off. Preferably, the sample may be stuck in the groove 542 so that the sample is not easily dropped.
In some embodiments, at least one infiltration chamber is provided with an infrared component in a region corresponding thereto. Specifically, referring to fig. 4 to 6, the fourth permeation cavity 500 is in a column shape, and the interior of the fourth permeation cavity is hollow to form a fourth permeation cavity air inlet section 510 and a fourth permeation cavity accumulation section 520, a placing table 530 is disposed between the fourth permeation cavity air inlet section 510 and the fourth permeation cavity accumulation section 520, the placing table 530 forms a first sample installation area, and a first sample can be placed on the placing table 530. The incident channel and the exit channel 563 are both communicated with the fourth permeable cavity accumulating section 520, incident light emitted by the light source enters the fourth permeable cavity accumulating section 520 through the incident channel and reaches the first sample mounting area, and exit light reflected by the first sample enters the spectrometer through the exit channel 563.
When the gas in the fourth permeate cavity gas inlet section 510 permeates into the fourth permeate cavity accumulating section 520 through the first sample, the incident light is reflected by the first sample and finally enters the spectrometer. In the process that gas permeates through the film sample, specific intermolecular chemical bond spectrum change in the first sample can be caused, the change curve can be output through the spectrometer, so that researchers can further research and analyze the permeation process, and the internal structure defect and the reaction process of the sample can be represented by means of the spectrometer, so that the internal structure defect and the permeation mechanism can be conveniently researched. In conclusion, the permeation process detection equipment in the application can further deepen the understanding of the permeation process of the film, and is favorable for the follow-up research on the high-barrier-rate film.
In some embodiments, the infrared assembly further includes a first reflective box 570, the first reflective box 570 having a first lens group disposed therein. The light source includes an infrared light source and a laser light source, and the incident channel includes an infrared light incident channel 561 and a laser incident channel 562. The first reflection box 570 is provided with a first light inlet 571 and a second light inlet 572, the infrared light source is installed at the first light inlet 571, and the laser light source is installed at the second light inlet 572. The infrared light emitted from the infrared light source enters the first reflection box 570 from the first light inlet window 571, reaches the first lens set, is reflected by the first lens set, and then enters the fourth permeable cavity accumulating section 520 from the infrared light incidence channel 561. The laser emitted from the laser source enters the first reflection box 570 from the second light inlet window 572, reaches the first lens group, is reflected by the first lens group, and then enters the fourth permeable cavity accumulating section 520 from the laser incident channel 562. During infrared detection, a beam of visible light wave band laser with fixed wavelength and a beam of infrared light with tunable wavelength simultaneously enter the surface of a sample at the same point, a beam of sum-frequency optical signal with the frequency of the sum of the two beams of incident laser frequency is generated in the reflection direction, and the optical signal enters a spectrometer. Therefore, the infrared light is made to coincide with the position where the laser light reaches the first sample mounting area, that is, the infrared light coincides with the position where the laser light reaches the first sample. Through setting up first reflection case 570, can reduce the interference of light source to the testing process in external environment, improve the accuracy of detecting. Set up first lens group in first reflection case 570 and reflect light, can adjust the light direction, make it satisfy preset incident direction, can also focus simultaneously, improve light intensity. The first lens group may be a single mirror or a plurality of mirrors.
In some embodiments, the infrared module further includes a second reflection box 580, a second lens set is disposed in the second reflection box 580, a light exit window 581 is disposed on the second reflection box 580, and the spectrometer is mounted at the light exit window 581. The emergent light reflected by the first sample enters the second reflection box 580 through the emergent channel 563, and is reflected by the second lens group and enters the spectrometer. The second lens group may be a single mirror or a plurality of mirrors.
In some embodiments, an observation window 550 is disposed at the fourth permeate cavity accumulating section 520. The observation window 550 is transparent, so that an operator can observe whether the directions of the infrared light, the laser light and the emergent light meet the requirements or not from the inside of the observation window 550.
In some embodiments, the second sample and the first sample may be the same film, and infrared detection and permeability detection may be performed simultaneously using the apparatus, and in use, may be performed in the fourth permeate chamber accumulating section 520 and the detection chamber 600, respectively. Therefore, infrared detection and permeability detection can be realized simultaneously by using only one channel of one device, the number of devices required to be used can be reduced, the detection flow is simplified, and the detection time is shortened. Of course, infrared detection may be accomplished only in the fourth permeate chamber accumulating section 520, or permeability detection may be accomplished only in the detection chamber 600. In other embodiments, the second sample and the first sample may be two films, one of which may be tested for infrared and the other of which may be tested for permeability using the apparatus.
In some embodiments, infrared components are disposed in the area corresponding to at least one infiltration chamber, and a weighing component 540 extends into the infiltration chamber air inlet section of the infiltration chamber. Namely, the weighing detection and the infrared detection can be finished in the same permeation cavity. Specifically, referring to fig. 4 to 6, in the fourth permeation cavity 500, the weighing component 540 is placed in the fourth permeation cavity air inlet section 510, the incident channel and the exit channel 563 are both communicated with the fourth permeation cavity accumulation section 520, the incident light emitted by the light source enters the fourth permeation cavity accumulation section 520 through the incident channel and reaches the first sample installation area, and the exit light reflected by the first sample enters the spectrometer through the exit channel 563.
In some embodiments, the second sample and the first sample may be the same film, and the apparatus may be used for simultaneous weighing, infrared detection and permeability detection, and in use, the weighing, infrared detection and permeability detection may be performed in the fourth permeate chamber gas inlet section 510, the fourth permeate chamber accumulating section 520 and the detection chamber 600, respectively. Therefore, weighing detection, infrared detection and permeability detection can be realized simultaneously by using only one channel of one device, the number of devices required to be used can be reduced, the detection flow is simplified, and the detection time is shortened. Of course, the weighing detection may be done only in the fourth permeate chamber inlet section 510, or the infrared detection may be done only in the fourth permeate chamber accumulating section 520, or the permeability detection may be done only in the detection chamber 600. In other embodiments, the second sample and the first sample may be two films, and one film may be weighed and the other infrared and permeability measurements may be made using the apparatus.
In some embodiments, the permeability detection method comprises the steps of:
s10, arranging a plurality of groups of permeation cavities;
s20 selecting at least one set of permeate cavities and installing a first sample into the selected permeate cavity;
s30, introducing gas into the permeation cavity selected in S20 for permeation and accumulation;
s40 releases the gas accumulated in the permeate cavity into the detection cavity 600 for detection by the mass spectrometer 710.
Specifically, in some embodiments, before the detection starts, a vacuum needs to be drawn in each channel to prevent the residual gas in the channel from affecting the accuracy of the detection. The aforementioned upper vacuum pumping port 130 and each lower vacuum pumping port 630 may be connected to a vacuum pump to achieve vacuum pumping. Preferably, the channel may be baked by heating while vacuuming, for example, the heating temperature is set to 120 ℃ and the baking time is set to 5 hours. Through heating and baking, the separation of gases such as water vapor and the like attached to the inner wall of the channel can be accelerated, so that the vacuumizing process is accelerated, and the detection time is shortened.
Specifically, in some embodiments, at least two sets of permeation cavities are selected in step S20, with the first sample installed in each set of permeation cavities being the same. In step S40, the gas that permeates and accumulates in each group of permeation cavities is sequentially released into the detection cavity 600, and between two adjacent groups of detections, the gas that is discharged from the previous group in the detection cavity 600 is evacuated, so as to prevent the residual gas of the previous group from affecting the detection result of the next group; the mass spectrometer 710 averages the results of each set. In other words, in this embodiment, the films to be detected are the same, the introduced gas is also the same, and the detection results of the selected permeation cavities are averaged to reduce the error and improve the detection accuracy.
For example, in the embodiment shown in the figures, it is selected that the same first sample is installed in both the first permeation chamber 200 and the second permeation chamber 300. The gas entering the gas inlet chamber 100 is the same gas, such as water vapor. The accumulation valve 820 between the first permeate chamber 200 and the detection chamber 600 is closed first and the accumulation valve 820 between the second permeate chamber 300 and the detection chamber 600 is closed. The intake valve 810 between the first permeate chamber 200 and the intake chamber 100 is opened and the intake valve 810 between the second permeate chamber 300 and the intake chamber 100 is opened. The water vapor enters the first permeation cavity 200 and the second permeation cavity 300, and the water vapor permeates downwards through the two first samples arranged in the first permeation cavity 200 and the second permeation cavity 300. After a period of time, the accumulation valve 820 between the first permeate chamber 200 and the detection chamber 600 is opened and the accumulation valve 820 between the second permeate chamber 300 and the detection chamber 600 remains closed. Water vapor accumulated in the first permeate chamber accumulating section 220 of the first permeate chamber 200 enters the detection chamber 600 for detection. Then, the accumulation valve 820 between the first osmosis chamber 200 and the detection chamber 600 is closed, the detection chamber 600 is vacuumized, and the accumulation valve 820 between the second osmosis chamber 300 and the detection chamber 600 is opened, so that the water vapor accumulated after the second osmosis chamber 300 permeates enters the detection chamber 600 for detection. The detection of the first 200 and second 300 permeate chambers is performed alternately a plurality of times to obtain more stable sets of data. Finally, the results of the first and second permeate cavities 200 and 300 are averaged.
In some embodiments, at least two sets of permeate cavities are selected in step S20, with the first sample installed differently within each set of permeate cavities. In step S30, the gas introduced into each set of permeation cavities is the same. In step S40, the gas that permeates and accumulates in each permeation cavity is sequentially released into the detection cavity 600, and the gas that is discharged from the previous group in the detection cavity 600 is evacuated between the two adjacent groups. In other words, in this embodiment, the films to be detected are different, and the introduced gas is the same, so that the detection of the permeability of the gas permeating through different films can be realized.
For example, in the embodiment shown in the figures, it is selected that a different first sample is installed in each of the first permeation chamber 200 and the second permeation chamber 300. The gas entering the gas inlet chamber 100 is the same gas, such as water vapor. The accumulation valve 820 between the first permeate chamber 200 and the detection chamber 600 is closed first and the accumulation valve 820 between the second permeate chamber 300 and the detection chamber 600 is closed. The intake valve 810 between the first permeate chamber 200 and the intake chamber 100 is opened and the intake valve 810 between the second permeate chamber 300 and the intake chamber 100 is opened. The water vapor enters the first permeation cavity 200 and the second permeation cavity 300, and the water vapor permeates downwards through two different first samples arranged in the first permeation cavity 200 and the second permeation cavity 300. After a period of time, the accumulation valve 820 between the first permeate chamber 200 and the detection chamber 600 is opened and the accumulation valve 820 between the second permeate chamber 300 and the detection chamber 600 remains closed. Water vapor accumulated in the first permeate chamber accumulating section 220 of the first permeate chamber 200 enters the detection chamber 600 for detection. Then, the accumulation valve 820 between the first osmosis chamber 200 and the detection chamber 600 is closed, the detection chamber 600 is vacuumized, and the accumulation valve 820 between the second osmosis chamber 300 and the detection chamber 600 is opened, so that the water vapor accumulated after the second osmosis chamber 300 permeates enters the detection chamber 600 for detection. The detection of the first 200 and second 300 permeate chambers is performed alternately a plurality of times to obtain more stable sets of data. According to the valve opening and closing time, the data output by the mass spectrometer 710 is split into two groups of data corresponding to the first permeation cavity 200 and the second permeation cavity 300, that is, the detection result of the gas passing through the two first samples is obtained.
In some embodiments, at least two sets of permeation cavities are selected in step S20, the first sample installed within each set of permeation cavities being the same. In step S30, different gases are introduced into each set of permeation cavities for permeation accumulation. In step S40, the gas that permeates and accumulates in each permeation cavity is sequentially released into the detection cavity 600, and the gas that is discharged from the previous group in the detection cavity 600 is evacuated between the two adjacent groups. In other words, in this embodiment, the films to be detected are the same, and the gas introduced is different, so that the detection of the permeability of different gases permeating through the same film can be realized.
For example, in the embodiment shown in the figures, it is selected that the same first sample is installed in both the first permeation chamber 200 and the second permeation chamber 300. The accumulation valve 820 between the first permeate chamber 200 and the detection chamber 600 is closed first and the accumulation valve 820 between the second permeate chamber 300 and the detection chamber 600 is closed. The intake valve 810 between the first permeate chamber 200 and the intake chamber 100 is opened and the intake valve 810 between the second permeate chamber 300 and the intake chamber 100 is closed. The first gas is introduced into the gas inlet cavity 100, enters the first permeation cavity 200, and permeates downwards through a first sample arranged in the first permeation cavity 200. After a period of time, the accumulation valve 820 between the first permeation chamber 200 and the detection chamber 600 is opened. The first gas accumulated in the first permeate chamber accumulating section 220 of the first permeate chamber 200 enters the detection chamber 600 for detection. The accumulation valve 820 between the first permeate chamber 200 and the detection chamber 600 is then closed and the first gas feed to the inlet chamber 100 is stopped, the detection chamber 600 is evacuated and the inlet chamber 100 and the first permeate chamber 200 are evacuated. Then the air inlet valve 810 between the first permeation cavity 200 and the air inlet cavity 100 is closed, the air inlet valve 810 between the second permeation cavity 300 and the air inlet cavity 100 is opened, the second gas is introduced into the air inlet cavity 100, the second gas enters the second permeation cavity 300, and permeates downwards through the first sample position arranged in the second permeation cavity 300. After a period of time, the accumulation valve 820 between the second permeate chamber 300 and the detection chamber 600 is opened. The second gas permeated and accumulated in the second permeation cavity 300 enters the detection cavity 600 for detection. The detection of the first 200 and second 300 permeate chambers is performed alternately a plurality of times to obtain more stable sets of data. According to the valve opening and closing time, the data output by the mass spectrometer 710 is split into two groups of data corresponding to the first permeation cavity 200 and the second permeation cavity 300, that is, the detection result of the gas passing through the two first samples is obtained.
As described above, the data measured by the mass spectrometer 710 may be calibrated by the standard flow guide device 430 to reduce errors and improve the accuracy of the detection results.
Specifically, the method for calibrating the mass spectrometer 710 by the standard flow guide device 430 includes:
s01 installing the standard conductance device 430 as a first sample within the selected osmotic chamber. For example, it is fixed at the gap between the third permeate cavity inlet section 410 and the third permeate cavity accumulating section 420.
S02, measuring the pressure of the introduced gas, calculating the gas flow rate, and calculating the permeability according to the obtained gas flow rate. The product of the pressure difference across the conduit and the conduit conductance is the conduit flow, since the pressure in the detection chamber 600 is already very low. It is negligible and therefore the gas flow rate can be directly obtained by multiplying the gas pressure in the gas inlet cavity 100 measured by the thin film vacuum gauge 140 by the standard conductance of the standard conductance device 430. Calculating the permeability from the obtained gas flow is prior art and will not be described herein.
S03 gas is introduced into the selected permeation cavity in S01 for permeation accumulation. Specifically, the accumulation valve 820 corresponding to the third permeate chamber 400 is closed and the intake valve 810 corresponding to the third permeate chamber 400 is opened. The gas in the inlet plenum 100 enters the third permeate chamber inlet section 410, permeates through the standard flow directing device 430 towards the third permeate chamber accumulating section 420 and accumulates in the third permeate chamber accumulating section 420.
S04 releases the gas that has permeated and accumulated in the permeation chamber into the detection chamber 600, and the gas is detected by the mass spectrometer 710. Specifically, the accumulation valve 820 corresponding to the third permeation cavity 400 is opened, the gas accumulated in the accumulation section 420 of the third permeation cavity enters the detection cavity 600, and the value measured by the mass spectrometer 710 is the pressure in the detection cavity 600.
S05 correlates the results of the mass spectrometer 710 measurements with the calculated permeability in S02. Specifically, the measured value of the mass spectrometer 710 is correlated with the standard value calculated by the standard conductance device 430, for example, when the pressure measured by the mass spectrometer 710 is P, the calculated permeability is a.
S06 adjusts the pressure of the introduced gas, and repeats S02 to S05 until the preset range data of the mass spectrometer 710 are covered, establishing a correspondence between the data measured by the mass spectrometer 710 and the permeability calculated by the standard conductance device 430. Specifically, the steps S02 to S05 are repeated, all values within the preset range of the measured pressure of the mass spectrometer 710 are covered, and the finally established correspondence relationship is that each measured pressure value P of the mass spectrometer 710 has a corresponding calculated permeability a. The corresponding relationship between the two can be represented by a graph or a table so as to facilitate the search. The preset range may include all values in the measurement pressure range of the mass spectrometer 710, and of course, if the preset range is limited by the model of the standard conductance device 430, the whole range cannot be covered, and the preset range may also include some values in the measurement pressure range of the mass spectrometer 710, and the whole range coverage is realized by replacing different types of standard conductance devices 430.
S07 finds the corresponding standard data in the correspondence established in S06 using the data measured by the mass spectrometer 710 in S40. Specifically, when a first sample is set to measure the permeability, for example, when the first sample is set in the first permeation chamber 200 and the permeability of the gas permeating through the first sample is detected, the valve is opened and closed to perform permeation accumulation and detection in the manner described in the foregoing embodiment, and when the value measured by the mass spectrometer 710 is P1, the obtained correspondence is searched, and when the detected value is P1, the corresponding permeability is what the value is.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (11)
1. Permeability detection apparatus, characterized by comprising:
an air inlet cavity;
the permeation cavities are all connected with the air inlet cavity, an air inlet valve is arranged between each permeation cavity and the corresponding air inlet cavity, when the air inlet valve is opened, the air inlet cavities are communicated with the corresponding permeation cavities, and a first sample installation area for installing a first sample is arranged in each permeation cavity;
the detection cavity is connected with a plurality of groups of permeation cavities, an accumulation valve is arranged between the permeation cavities and the detection cavity, and when the accumulation valve is opened, the detection cavity is communicated with the corresponding permeation cavity;
a mass spectrometer in communication with the detection cavity.
2. The permeability detection apparatus according to claim 1, wherein the permeation cavity comprises a permeation cavity inlet section and a permeation cavity accumulation section, the permeation cavity inlet section is connected with the inlet cavity, the permeation cavity accumulation section is connected with the detection cavity, the first sample installation areas are formed between the permeation cavity inlet section and the permeation cavity accumulation section, and one of the first sample installation areas is provided with a standard flow guide device.
3. The permeability detection apparatus according to claim 1, wherein the permeation cavity comprises a permeation cavity inlet section and a permeation cavity accumulation section, the permeation cavity inlet section is connected to the inlet cavity, the permeation cavity accumulation section is connected to the detection cavity, the first sample installation area is formed between the permeation cavity inlet section and the permeation cavity accumulation section, a weighing component is arranged in the permeation cavity inlet section in at least one of the permeation cavities, a second sample installation area is arranged on the weighing component, and the second sample installation area is used for placing a second sample.
4. The permeability detection apparatus according to claim 1, wherein at least one region corresponding to the permeation chamber is provided with an infrared component, and the infrared component comprises a light source, an incident channel, an exit channel and a spectrometer;
the permeation cavity comprises a permeation cavity air inlet section and a permeation cavity accumulation section, the permeation cavity air inlet section is connected with the air inlet cavity, the permeation cavity accumulation section is connected with the detection cavity, and the first sample installation area is formed between the permeation cavity air inlet section and the permeation cavity accumulation section;
the incident channel and the emergent channel are communicated with the infiltration cavity accumulation section, incident light rays emitted by the light source enter the infiltration cavity accumulation section through the incident channel and reach the first sample installation area, and emergent light rays reflected by the first sample enter the spectrometer through the emergent channel.
5. The permeability detection apparatus according to claim 1, wherein the permeation cavity comprises a permeation cavity inlet section and a permeation cavity accumulation section, the permeation cavity inlet section is connected with the inlet cavity, the permeation cavity accumulation section is connected with the detection cavity, and the first sample installation region is formed between the permeation cavity inlet section and the permeation cavity accumulation section;
at least one infiltration cavity corresponds the region and is equipped with infrared subassembly, infrared subassembly includes light source, incident passageway, exit channel and spectrum appearance, the incident passageway exit channel all with infiltration cavity accumulation section intercommunication, the incident light that the light source sent passes through the incident passageway gets into infiltration cavity accumulation section and reachs first sample installing zone, the process emergent light after the first sample reflection passes through exit channel gets into the spectrum appearance, it has the weighing component to stretch into in the infiltration cavity section of admitting air, be equipped with second sample installing zone on the weighing component, second sample installing zone is used for placing the second sample.
6. The permeability detection method is characterized by comprising the following steps:
s10, arranging a plurality of groups of permeation cavities;
s20 selecting at least one set of the infiltration cavities and installing a first sample into the selected infiltration cavity;
s30, introducing gas into the permeation cavity selected in the S20 for permeation accumulation;
s40, releasing the gas accumulated in the permeation cavity into the detection cavity, and detecting through a mass spectrometer.
7. The permeability detection method according to claim 6,
at S20, selecting at least two groups of the permeation cavities, wherein the first samples installed in each group of the permeation cavities are the same;
in S40, releasing the gas accumulated in each group of permeation cavities into the detection cavities in sequence, and evacuating the gas exhausted from the previous group in the detection cavities between two adjacent groups of detections; and averaging the results of each group detected by the mass spectrometer.
8. The permeability detection method according to claim 6,
at least two groups of permeation cavities are selected in S20, wherein the first samples installed in the permeation cavities in each group are different;
in S30, the gas introduced into each group of permeation cavities is the same;
and S40, sequentially releasing the gas accumulated in each group of permeation cavities into the detection cavity, and evacuating the gas exhausted from the previous group in the detection cavity between two adjacent groups of detections.
9. The permeability detection method according to claim 6,
at S20, selecting at least two groups of the permeation cavities, wherein the first samples installed in each group of the permeation cavities are the same;
in S30, introducing different gases into each group of permeation cavities for permeation accumulation;
and S40, sequentially releasing the gas accumulated in each group of permeation cavities into the detection cavity, and evacuating the gas exhausted from the previous group in the detection cavity between two adjacent groups of detections.
10. The permeability detection method according to claim 6, wherein a standard conductance device is installed in one of the permeation cavities, and data measured by the mass spectrometer is calibrated through the standard conductance device.
11. The permeability detection method of claim 10, wherein the mass spectrometer is calibrated by the standard flow guide device by:
s01, installing the standard conductance device as the first sample in the selected infiltration cavity;
s02, measuring the pressure of the introduced gas, calculating the gas flow, and calculating the permeability according to the obtained gas flow;
s03, introducing gas into the permeation cavity selected in the S01 for permeation accumulation;
s04, releasing the gas accumulated in the permeation cavity into the detection cavity, and detecting through the mass spectrometer;
s05 correlating the mass spectrometer measurements with the calculated permeabilities in S02;
s06, adjusting the pressure of the introduced gas, repeating S02 to S05 until the preset measuring range data of the mass spectrometer are covered, and establishing the corresponding relation between the data measured by the mass spectrometer and the permeability calculated by the standard conductance device;
s07 finds the corresponding standard data in the correspondence established in S06 using the data measured by the mass spectrometer described in S40.
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Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3015775A (en) * | 1959-01-09 | 1962-01-02 | Coulter Electronics | Fluid metering system and apparatus |
| US20050167598A1 (en) * | 2004-02-04 | 2005-08-04 | Bujas Roko S. | Method and apparatus for measuring ultralow permeation |
| US20100268488A1 (en) * | 2009-02-24 | 2010-10-21 | Halliburton Energy Services, Inc. | Methods and Apparatus for Determining the Permeability and Diffusivity of a Porous Solid |
| CN101949813A (en) * | 2010-07-27 | 2011-01-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method and device for detecting water oxygen infiltration index in device packaging |
| US20120078541A1 (en) * | 2010-09-29 | 2012-03-29 | Conocophillips Company - Ip Services Group | High-pressure quartz crystal microbalance |
| US20120210770A1 (en) * | 2010-09-10 | 2012-08-23 | Aziz Mahfoud Familia | Systems and methods for permeability rate testing of barrier films using vapor accumulation |
| CN104020185A (en) * | 2014-06-18 | 2014-09-03 | 东南大学 | Method for measuring macromolecule ultrathin membrane phase inversion temperature |
| CN105547956A (en) * | 2015-12-10 | 2016-05-04 | 电子科技大学 | Device and method for measuring gas permeability of thin film by using vacuometer |
| CN106290117A (en) * | 2016-10-19 | 2017-01-04 | 中国科学院光电研究院 | A kind of apparatus and method causing gas infiltration for testing material radiation |
| CN106525683A (en) * | 2016-10-27 | 2017-03-22 | 华中科技大学 | Thin film permeability measuring device and method |
| CN107894376A (en) * | 2017-12-12 | 2018-04-10 | 中国计量大学 | Water vapor diffusion coefficient measuring device and its measuring method |
| CN108918381A (en) * | 2018-07-12 | 2018-11-30 | 南京林业大学 | A method of quickly, biological material moisture diffusion and penetrability are measured simultaneously |
| US20190301992A1 (en) * | 2018-03-29 | 2019-10-03 | U.S. Army Research Laboratory | Spectroscopic membrane permeation cell for simultaneous measurements of gas permeation rates and infrared reflection absorption spectroscopic analysis of membrane surfaces |
| US20210011053A1 (en) * | 2018-09-06 | 2021-01-14 | Bruker Nano, Inc. | Method And Apparatus Of Atomic Force Microscope Based Infrared Spectroscopy With Controlled Probing Depth |
| CN112444471A (en) * | 2020-11-13 | 2021-03-05 | 大连卡瑞博纳科技有限公司 | Full-automatic gas separation membrane permeability testing device and method |
| CN112964619A (en) * | 2021-02-05 | 2021-06-15 | 浙江大学 | Device and method for measuring interfacial water vapor permeability coefficient of multilayer porous material |
Family Cites Families (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4858461A (en) * | 1987-09-29 | 1989-08-22 | General Electric Company | Permeation cell gas detector |
| CN100507510C (en) * | 2004-09-30 | 2009-07-01 | 清华大学 | Testing method for water oxygen permeability and its testing equipment |
| JP2010249609A (en) * | 2009-04-14 | 2010-11-04 | Ulvac Japan Ltd | Instrument and method for measuring permeation amount of steam |
| CN102628785A (en) * | 2012-03-27 | 2012-08-08 | 济南兰光机电技术有限公司 | Gas permeability test device |
| CN102928326B (en) * | 2012-11-08 | 2015-03-25 | 济南兰光机电技术有限公司 | Device and method for testing permeability of organic gases to films |
| JP5703365B1 (en) * | 2013-12-25 | 2015-04-15 | 株式会社ピュアロンジャパン | Manufacturing method of micropore filter |
| CN104483227A (en) * | 2014-12-12 | 2015-04-01 | 西南石油大学 | Sulfur deposition device based on magnetic suspension balance |
| CN105466831B (en) * | 2015-11-20 | 2018-09-28 | 中国特种设备检测研究院 | A kind of measuring gas permebility device |
| CN108287128A (en) * | 2018-01-29 | 2018-07-17 | 中国科学院武汉岩土力学研究所 | A kind of ground drying and watering cycle permeability measurement systems and its method |
| CN209311289U (en) * | 2018-12-26 | 2019-08-27 | 济南思克测试技术有限公司 | A kind of UF membrane test device of positive/negative-pressure one |
| CN112098292B (en) * | 2019-06-18 | 2023-11-17 | 哈尔滨工业大学 | Device and method for measuring high-temperature gas permeability of micro-nano pore material based on two-dimensional seepage effect |
| CN111551476B (en) * | 2020-04-24 | 2022-12-09 | 广州西唐机电科技有限公司 | Gas permeability testing system and method based on differential pressure method |
-
2021
- 2021-06-24 CN CN202110706803.9A patent/CN113466101B/en active Active
- 2021-08-30 WO PCT/CN2021/115362 patent/WO2022267218A1/en unknown
Patent Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3015775A (en) * | 1959-01-09 | 1962-01-02 | Coulter Electronics | Fluid metering system and apparatus |
| US20050167598A1 (en) * | 2004-02-04 | 2005-08-04 | Bujas Roko S. | Method and apparatus for measuring ultralow permeation |
| US20100268488A1 (en) * | 2009-02-24 | 2010-10-21 | Halliburton Energy Services, Inc. | Methods and Apparatus for Determining the Permeability and Diffusivity of a Porous Solid |
| CN101949813A (en) * | 2010-07-27 | 2011-01-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method and device for detecting water oxygen infiltration index in device packaging |
| US20120210770A1 (en) * | 2010-09-10 | 2012-08-23 | Aziz Mahfoud Familia | Systems and methods for permeability rate testing of barrier films using vapor accumulation |
| US20120078541A1 (en) * | 2010-09-29 | 2012-03-29 | Conocophillips Company - Ip Services Group | High-pressure quartz crystal microbalance |
| CN104020185A (en) * | 2014-06-18 | 2014-09-03 | 东南大学 | Method for measuring macromolecule ultrathin membrane phase inversion temperature |
| CN105547956A (en) * | 2015-12-10 | 2016-05-04 | 电子科技大学 | Device and method for measuring gas permeability of thin film by using vacuometer |
| CN106290117A (en) * | 2016-10-19 | 2017-01-04 | 中国科学院光电研究院 | A kind of apparatus and method causing gas infiltration for testing material radiation |
| CN106525683A (en) * | 2016-10-27 | 2017-03-22 | 华中科技大学 | Thin film permeability measuring device and method |
| CN107894376A (en) * | 2017-12-12 | 2018-04-10 | 中国计量大学 | Water vapor diffusion coefficient measuring device and its measuring method |
| US20190301992A1 (en) * | 2018-03-29 | 2019-10-03 | U.S. Army Research Laboratory | Spectroscopic membrane permeation cell for simultaneous measurements of gas permeation rates and infrared reflection absorption spectroscopic analysis of membrane surfaces |
| CN108918381A (en) * | 2018-07-12 | 2018-11-30 | 南京林业大学 | A method of quickly, biological material moisture diffusion and penetrability are measured simultaneously |
| US20210011053A1 (en) * | 2018-09-06 | 2021-01-14 | Bruker Nano, Inc. | Method And Apparatus Of Atomic Force Microscope Based Infrared Spectroscopy With Controlled Probing Depth |
| CN112444471A (en) * | 2020-11-13 | 2021-03-05 | 大连卡瑞博纳科技有限公司 | Full-automatic gas separation membrane permeability testing device and method |
| CN112964619A (en) * | 2021-02-05 | 2021-06-15 | 浙江大学 | Device and method for measuring interfacial water vapor permeability coefficient of multilayer porous material |
Non-Patent Citations (4)
| Title |
|---|
| 任国华等: "质谱计校准技术发展现状", 《真空与低温》 * |
| 吴成耀等: "分压力质谱计校准技术研究进展", 《真空与低温》 * |
| 杨威等: "OLED封装材料气体渗透率测试的发展", 《功能材料》 * |
| 杨齐民;熊秉衡;: "现代光电检测综述" * |
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