CN114563325A - Device and method for testing water permeability by electrical Ca membrane method - Google Patents
Device and method for testing water permeability by electrical Ca membrane method Download PDFInfo
- Publication number
- CN114563325A CN114563325A CN202210256165.XA CN202210256165A CN114563325A CN 114563325 A CN114563325 A CN 114563325A CN 202210256165 A CN202210256165 A CN 202210256165A CN 114563325 A CN114563325 A CN 114563325A
- Authority
- CN
- China
- Prior art keywords
- film
- opening
- cover plate
- testing
- supporting table
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000012360 testing method Methods 0.000 title claims abstract description 138
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000012528 membrane Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 40
- 230000035699 permeability Effects 0.000 title claims abstract description 32
- 230000004888 barrier function Effects 0.000 claims abstract description 80
- 239000011575 calcium Substances 0.000 claims description 133
- 238000007789 sealing Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000004519 grease Substances 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 5
- 238000010998 test method Methods 0.000 claims description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 abstract description 3
- 238000011041 water permeability test Methods 0.000 abstract description 3
- 229920001971 elastomer Polymers 0.000 description 10
- 239000000523 sample Substances 0.000 description 7
- 229920002799 BoPET Polymers 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 229920002367 Polyisobutene Polymers 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000012935 Averaging Methods 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 238000000180 cavity ring-down spectroscopy Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 241000665848 Isca Species 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000003869 coulometry Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Images
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention discloses a device and a method for testing water permeability by an electrical Ca membrane method. The device for the electrical Ca membrane method water permeability test of the barrier membrane comprises: the clamp comprises a clamp body and a clamp body, wherein the clamp body comprises a containing cavity with a first opening, and an annular supporting table surface is formed on the inner wall of the containing cavity; the Ca film testing component is arranged in the accommodating cavity and is positioned on one side of the supporting table board, which is far away from the first opening, and comprises a Ca film testing card which comprises a Ca film line; the cover plate is provided with a second opening through which water and air can pass, and the cover plate can be arranged at the first opening of the accommodating chamber in an opening mode. The device for testing the water permeability of the barrier film by using the electrical Ca film method provided by the embodiment of the invention can be used for simply, conveniently and quickly fixing and disassembling the barrier film, the test card and cleaning the device, the area utilization rate of the barrier film is greatly improved, and the effective utilization rate of the barrier film is improved to be close to 1/2.
Description
Technical Field
The invention relates to a testing device, in particular to a device and a method for testing water permeability by an electrical Ca membrane method, and belongs to the technical field of packaging testing.
Background
The barrier properties of the barrier film are primarily characterized by the rate of water oxygen permeation through the barrier film, which is characterized by the water permeation rate (WVTR) and oxygen permeation rate (OTR), respectively. Of the two factors that mainly affect the lifetime of organic devices, water solubility is generally much stronger in polymers than oxygen, about 100-10000 times that of oxygen, so O2Has a negligible amount of penetration. The main current test categories of WVTR: MOCON (coulometry), optical/electrical Ca membrane methods, mass spectrometry, cavity ring-down spectroscopy (CRDS), radioisotope methods, and the like. Among them, the WVTR test method of the optical/electrical Ca film invented by Niasto, Paetzold et. is distinguished by the advantages of simple method, low total cost, high efficiency and intuition.
Ca is used as opaque metal, and the light transmittance and the electric conductivity of the opaque metal are obviously lower than those of CaO and Ca (OH) which are products after the opaque metal reacts with water and oxygen2The WVTR of the encapsulating film can be indirectly derived by measuring the change in permeability/conductivity of the sample of the encapsulated Ca film. Compared with an optical test method, the WVTR test method for the electrical Ca film has the advantages of capability of quantitatively measuring WVTR in real time, high space utilization rate, small error and simple statistical data. The WVTR test method of the electrical Ca film can also adjust the thickness of the Ca film of the test card structure and the area of the test window according to the test requirements, and avoid test data errors while adapting to different test environments.
However, in the prior art, the electrical Ca film WVTR testing method with a good testing effect fixes the barrier film on the testing mold semi-permanently mainly through adhesives such as epoxy resin, polyisobutylene, and the like. This design inherently results in excellent side sealing but has significant disadvantages.
The first disadvantage is that post-test cleaning is difficult, and removal is almost impossible if a cross-linked cured adhesive such as epoxy is used to secure the barrier film and test card to the test mold; the test mould becomes disposable article promptly, has greatly improved the test cost. Even if viscous rubber such as polyisobutylene is used as an adhesive, the viscous rubber is difficult to completely clean from a mould and wastes time and labor even if strong solvents such as chloroform, chlorobenzene and the like are introduced; meanwhile, the solvents have high toxicity and are unfavorable for environmental protection; the secondary disadvantage is that the area utilization rate of the barrier film of the method is very low, even if epoxy resin, polyisobutylene and the like with better barrier property in organic matters are used as adhesives, the length of the side edge seal needs to be greatly prolonged to avoid the side edge permeation problem, namely the area required by the test of the barrier film is far larger than the actual test area and even reaches below 1/10.
Disclosure of Invention
The invention mainly aims to provide a device and a method for testing water permeability by an electrical Ca membrane method, so as to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the device for testing the water permeability of the barrier film by using the electrical Ca film method provided by the embodiment of the invention comprises the following components:
the clamp comprises a clamp body and a clamp body, wherein the clamp body comprises a containing cavity with a first opening, and an annular supporting table surface is formed on the inner wall of the containing cavity;
the Ca film testing component is arranged in the accommodating cavity and is positioned on one side of the supporting table board, which is far away from the first opening, and comprises a Ca film testing card which comprises a Ca film line;
the cover plate is provided with a second opening through which water and air can pass, and the cover plate can be arranged at the first opening of the accommodating chamber in an opening mode;
when the cover plate is fixedly arranged at the first opening of the accommodating cavity, the first part of the resistance membrane to be measured is fixedly pressed between the cover plate and the supporting table top and is tightly attached to the supporting table top, the second part of the resistance membrane to be measured completely covers the first opening area of the accommodating cavity, and the second opening corresponds to the second part of the resistance membrane to be measured.
The embodiment of the invention also provides a method for testing the water permeability of the barrier film, which comprises the following steps:
providing the device, sealing and fixing the barrier film between the cover plate and the support table surface of the clamp main body, and placing the clamp main body packaged with the barrier film in a test environment;
applying an electrical signal to a Ca film testing component in the clamp body, collecting the resistance value of the Ca film line within a fixed time interval, and obtaining the water permeation rate WVTR of the barrier film according to formula 1);
wherein n is the reaction equivalent of water in the reaction process, deltaCaIs the density of Ca, ACaIs the area of the Ca membrane, AWMw is the molecular weight of water, M, for the effective area of the barrier filmCaIs the molecular weight of calcium, R is the measured resistance value of Ca film, RCaInitial resistance of Ca film at the time of starting test, h: the Ca film thickness at the start of the test, t is the test time.
Compared with the prior art, the invention has the advantages that:
1) the device for testing the water permeability of the barrier film by the electrical Ca film method provided by the embodiment of the invention can simply, conveniently and quickly fix and dismantle the barrier film, the test card and the cleaning device;
2) the device for testing the water permeability of the barrier film by using the electrical Ca film method provided by the embodiment of the invention greatly improves the area utilization rate of the barrier film, and the effective utilization rate of the barrier film is improved to be close to 1/2;
3) the embodiment of the invention also provides a method for testing the water permeability of the barrier film, which has simple test flow, high efficiency and environmental protection;
4) the embodiment of the invention also provides a method for testing the water permeability of the barrier film, which removes the influence of uncertain resistivity on the test result.
Drawings
Fig. 1 is a schematic structural diagram of an apparatus for electrical Ca membrane method water permeability test of a barrier membrane according to an exemplary embodiment of the present invention;
fig. 2 is an exploded view of the structure of an apparatus for electrical Ca membrane method water permeability testing of a barrier membrane provided in an exemplary embodiment of the present invention;
fig. 3 is a schematic structural diagram of a Ca membrane test card in an apparatus for electrical Ca membrane method water permeability test of a barrier membrane according to an exemplary embodiment of the present invention;
FIG. 4 is a resistance (R) -time (t) plot of the apparatus for electrical Ca-film water permeability testing of barrier films in an exemplary embodiment of the invention for testing the water permeability of a 125 μm PET film at 40 deg.C in a 100 RH% testing environment;
fig. 5 is a WVTR-time (t) graph of water permeability of a 125 μm PET film tested in a 100 RH% test environment at 40 c with an apparatus for electrical Ca film water permeability testing of barrier films in an exemplary embodiment of the invention.
Detailed Description
In view of the deficiencies in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide technical solutions of the present invention. The technical solution, its implementation and principles, etc. will be further explained as follows.
The device for testing the water permeability of the electrical Ca membrane method of the barrier membrane, provided by the embodiment of the invention, is mainly characterized in that the WVTR testing die of the electrical Ca membrane of the barrier membrane is fixed in a mode of combining the rubber ring and the vacuum grease, and the barrier membrane is fixed in a mode of combining the rubber ring and the vacuum grease, so that the barrier membrane, a Ca membrane testing card and the device can be conveniently and quickly fixed and detached and cleaned; meanwhile, the area utilization rate of the barrier film is greatly improved, so that the effective utilization rate of the barrier film is improved to be close to 1/2; the lower limit of the WVTR test of the barrier film of the device under the test environment of 100 RH% at 40 ℃ reaches 10-2g·m-2·day-1The magnitude order can be simultaneously applied to the barrier film WVTR test under the environment of 0-100 ℃/0-100RH percent.
The device for testing the water permeability of the barrier film by the electric Ca film method provided by the embodiment of the invention comprises the following components:
the clamp comprises a clamp body and a clamp body, wherein the clamp body comprises a containing cavity with a first opening, and an annular supporting table surface is formed on the inner wall of the containing cavity;
the Ca film testing component is arranged in the accommodating cavity and is positioned on one side of the supporting table board, which is far away from the first opening, and comprises a Ca film testing card which comprises a Ca film line;
the cover plate is provided with a second opening through which water and air can pass, and the cover plate can be arranged at the first opening of the accommodating chamber in an opening mode;
when the cover plate is fixedly arranged at the first opening of the accommodating cavity, the first part of the resistance membrane to be measured is fixedly pressed between the cover plate and the supporting table top and is tightly attached to the supporting table top, the second part of the resistance membrane to be measured completely covers the first opening area of the accommodating cavity, and the second opening corresponds to the second part of the resistance membrane to be measured.
In a specific embodiment, the cover plate further has a pressing portion corresponding to the supporting table, the pressing portion is disposed around the second opening,
when the cover plate is fixedly arranged at the first opening of the accommodating cavity, the pressing part is attached to the supporting table top, or the gap between the pressing part and the supporting table top is smaller than the thickness of the first part of the diaphragm to be measured.
In one embodiment, the apparatus further comprises: an annular elastic pressing component arranged between the cover plate and the supporting table top,
when the cover plate is fixedly arranged at the first opening of the accommodating cavity, the elastic pressing part can be respectively contacted with the cover plate and the supporting table top, and the elastic pressing part is in an elastic compression state.
In a specific embodiment, the elastic pressing member is disposed on the cover plate and surrounds the second opening.
In a specific embodiment, the device includes two or more elastic pressing members, and the two or more elastic pressing members are arranged at intervals along a radial direction of the second opening.
In a specific embodiment, the cover plate is further provided with a receiving groove, and the elastic pressing member is disposed in the receiving groove.
In a specific embodiment, a step structure is further formed at the first opening, and a surface of the step structure forms the support mesa.
In a specific embodiment, the support table is a smooth and continuous plane.
In a specific embodiment, Ca membrane test assembly still includes the circuit board, Ca membrane test card and circuit board setting are on a fixed frame and electric connection, fixed frame detachably sets up accept in the cavity.
In a specific embodiment, the Ca film test card includes a substrate, and an electrode and a Ca film formed on the substrate, the Ca film including a plurality of Ca film lines electrically connected to the electrode.
In a specific embodiment, the clamp body comprises a first clamp and a second clamp, and the first clamp and the second clamp are detachably connected and enclose to form the accommodating chamber.
In one embodiment, the cover plate is sealingly engaged with the clamp body.
In a specific embodiment, the first clamp and the second clamp are sealingly joined.
The embodiment of the invention also provides a method for testing the water permeability of the barrier film, which comprises the following steps:
providing the device, sealing and fixing the barrier film between the cover plate and the support table surface of the clamp main body, and placing the clamp main body packaged with the barrier film in a test environment;
applying an electrical signal to a Ca film testing component in the clamp body, collecting the resistance value of the Ca film line within a fixed time interval, and obtaining the water permeation rate WVTR of the barrier film according to formula 1);
wherein n is the reaction equivalent of water in the reaction process, and if the final product of 1mol Ca and water isCa(OH)2When 2mol of water is consumed in the reaction process, n is-2, deltaCaIs the density of Ca, generally deltaCa＝1.55g/cm3，ACaIs the area of the Ca membrane, AWMw is the molecular weight of water, M, for the effective area of the barrier filmCaIs the molecular weight of calcium, R is the measured resistance value of Ca film, RCaInitial resistance of Ca film at the time of starting test, h: the Ca film thickness at the start of the test, t is the test time.
The effective area of the barrier film is an area covering the second portion of the first opening region of the housing chamber.
In a specific embodiment, the testing method further comprises: the method comprises the steps of firstly arranging vacuum grease on the supporting table top, then sealing and attaching the first part of the barrier film on the supporting table top, enabling the second part of the barrier film to completely cover the first opening area of the accommodating chamber, and enabling the second opening to correspond to the second part of the barrier film to be tested.
As will be described in further detail with reference to the accompanying drawings and specific embodiments, the circuit board, the Ca film test, the rubber ring, and the vacuum grease used in the embodiments of the present invention are known to those skilled in the art, and are commercially available, and the specific size, shape, etc. are not limited thereto unless otherwise specified.
Referring to fig. 1-3, an apparatus for electrical Ca film water permeability testing of a barrier film includes a fixture main body 100, a cover plate 200 and a Ca film testing assembly, wherein the fixture main body 100 includes a receiving chamber having a first opening, the Ca film testing assembly is disposed in the receiving chamber, the cover plate 200 is detachably connected to the fixture main body 100 and openably disposed at the first opening of the receiving chamber, so as to enclose the Ca film testing assembly in the receiving chamber, wherein the cover plate 200 has a second opening 201 through which water and gas can pass, and the Ca film testing assembly is used for testing water permeability of the barrier film.
In this embodiment, an annular supporting mesa 121 is formed on the inner wall of the receiving chamber, when the cover plate 200 is fixedly disposed at the first opening of the receiving chamber, a first portion of the resistance measuring diaphragm is fixedly pressed between the cover plate 200 and the supporting mesa 121 and tightly attached to the supporting mesa 121 without a gap, a second portion of the resistance measuring diaphragm completely covers the first opening area of the receiving chamber, and the second opening 201 corresponds to the second portion of the resistance measuring diaphragm, wherein the Ca film testing component is located on a side of the resistance measuring diaphragm away from or far away from the resistance measuring diaphragm, and the first portion of the resistance measuring diaphragm is disposed around the second portion.
In this embodiment, the supporting mesa 121 may be integrally formed with the inner wall of the receiving chamber, and it is understood that the supporting mesa 121 is formed by protruding a portion of the inner wall of the receiving chamber in a radial direction of the receiving chamber.
In other embodiments, a step structure is further formed at the first opening of the accommodating chamber, and a surface of the step structure forms the support platform.
Of course, in other embodiments, the support table 121 may be formed on a support ring fixedly disposed on the inner wall of the receiving chamber.
In this embodiment, in order to make the barrier film to be measured better closely fit with the supporting mesa 121, the supporting mesa 121 is set to be a smooth and flat plane.
In this embodiment, a pressing portion corresponding to the supporting mesa is further disposed on a side surface of the cover plate 200 facing the accommodating chamber, the pressing portion surrounds the second opening 201 and corresponds to the supporting mesa 121, when the cover plate 200 is fixedly disposed at the first opening of the accommodating chamber, the pressing portion is attached to the supporting mesa 121, or a gap between the pressing portion and the supporting mesa 121 is smaller than a thickness of the first portion of the resistance film to be measured, so as to fix the resistance film to be measured.
In this embodiment, the pressing portion may be an annular protrusion formed by partially protruding in the thickness or axial direction of the cover plate 200.
In this embodiment, an annular elastic pressing member 800 is further disposed on a side surface of the cover plate 200 facing the accommodating chamber, the elastic pressing member 800 is disposed around the second opening 201 and corresponds to the supporting table 121, when the cover plate 200 is fixedly disposed at the first opening of the accommodating chamber, the elastic pressing member 800 can contact with the supporting table, or a gap between the elastic pressing member 800 and the supporting table 121 is smaller than a thickness of the first portion of the resistance measuring diaphragm, and when the cover plate 200 and the elastic pressing member 800 are combined with the fixture body 100 and the resistance measuring diaphragm is fixed, the elastic pressing member 800 is in an elastic compression state.
In this embodiment, the elastic pressing member 800 may be a rubber ring or the like.
In this embodiment, the cover plate 200 is provided with two or more elastic pressing members 800, and the two or more elastic pressing members 800 are arranged at intervals along the radial direction of the second opening.
In this embodiment, a receiving groove is further disposed on a side surface of the cover plate 200 facing the receiving cavity, a part of the elastic pressing member 800 is disposed in the receiving groove, and the rest is exposed from the receiving groove, and the exposed part is used for pressing the barrier diaphragm to be measured.
In this embodiment, the fixture main body 100 includes a first fixture 110 and a second fixture 120, the first fixture 110 has a first chamber 101 therein, the second fixture 120 has a second chamber 102 therein, and the first fixture 110 and the second fixture 120 are detachably connected and enclose to form the receiving chamber, which is mainly composed of the first chamber 101 and the second chamber 102, and the first chamber 102, the second chamber 102 and a second opening on the cover plate 200 are all through to allow moisture in the environment to penetrate through the barrier film from the second opening of the cover plate and then reach the Ca film testing assembly in the receiving chamber.
In the present embodiment, the supporting table 121 is formed on the wall of the second chamber 102 inside the second fixture 120, and the first opening is also disposed on the second fixture 120, it can be understood that the cover plate 200 is directly connected to and matched with the second fixture 120.
In this embodiment, the first clamp 110 and the second clamp 120 may be connected by a threaded connection member such as a bolt, and the first clamp 110 and the second clamp 120 are in sealing fit, and in order to make the first clamp 110 and the second clamp 120 in better sealing fit, a rubber ring or the like for sealing may be further provided at a connection region between the first clamp 110 and the second clamp 120.
In this embodiment, the cover plate 200 may be fixedly connected to the second fixture 120 through a threaded connection member such as a bolt, and the cover plate 200 and the second fixture 120 also need to be connected in a sealing manner, so that moisture in the environment can only enter the receiving cavity through the second opening 210 on the cover plate, for example, a sealing member such as a rubber ring may be disposed between the cover plate 200 and the second fixture 120.
In this embodiment, the Ca film testing assembly is located on one side of the supporting table 121 away from the first opening or the cover plate in the accommodating chamber, the Ca film testing assembly includes a Ca film testing card 400 and a circuit board 500, the Ca film testing card 400 includes a Ca film wire 410 and an electrode, and the electrode of the Ca film testing card 400 is electrically connected to the circuit board 500 through a probe.
In this embodiment, a clamping groove is provided in the first chamber of the first clamp 110, the circuit board 500 is embedded in the clamping groove, the Ca membrane test card 400 is disposed on an annular fixing frame 600, a plurality of probe holes 601 for probes to pass through are provided on the fixing frame 600, and the probes of the circuit board 500 and the Ca membrane test card 400 are connected and disposed in the probe holes of the fixing frame 600.
In this embodiment, the Ca film test card 400 is fixed to the fixing frame 600 via a pressing plate 700, and the Ca film test card 400 is confined between the pressing plate 700 and the fixing frame 600, wherein the pressing plate 700 may be connected to the fixing frame 600 by a connector such as a bolt.
It should be noted that the fixing frame 600 and the pressing plate 700 are both annular members, or the fixing frame 600 and the pressing plate 700 both have openings exposing the Ca film test card 400, so that water vapor entering from the outside can contact the Ca film test card 400; it is understood that the second opening of the cover plate 200 is communicated with the first chamber 102, the second chamber 102, the pressure plate and the fixing frame.
In this embodiment, the Ca membrane test assembly is further connected to an HVG socket for connection to other test components such as a circuit board and an externally provided source meter.
In this embodiment, the method for testing the water permeability of the barrier film with the apparatus for electrical Ca film method water permeability testing of the barrier film shown in fig. 1 to 3 may include the steps of:
1) the Ca film test card as shown in fig. 3 was provided:
sequentially evaporating a Cu electrode and a Ca testing film on a smooth 24.5 x 24.5mm glass testing card substrate to obtain a Ca film WVTR glass substrate-Cu electrode testing card for later use, wherein the Ca film testing card is provided with 4 standard Ca testing film lines, the length of the Ca testing film line is 25mm, the line width is 0.9mm, the thicknesses of the Ca film and the Cu electrode can be regulated and controlled through evaporation conditions, and the adopted equipment and process of the evaporation process can be known by those skilled in the art;
2) after aligning the Ca film test card with the probe, placing the Ca film test card in a clamping groove in an accommodating cavity in the clamp main body;
3) coating vacuum grease on the surface of the supporting table-board 121, attaching a barrier film to the supporting table-board 121, fixing the cover plate 200 and the clamp main body 100, and tightly attaching the rubber ring on the cover plate 200 and the barrier film, so that the barrier film is fixed and pressed between the rubber ring and the supporting table-board, and sealing between the barrier film and the clamp main body is realized;
4) placing the packaged device in a constant-temperature and constant-humidity test environment, connecting a test source meter with a Ca film test assembly, continuously sending an electric signal to the Ca film test assembly through a current converter through a cable, monitoring resistance value changes of 4 Ca film wires on a Ca film test card along with time in real time within a fixed interval time, obtaining a water permeation speed WVTR of the barrier film according to formula 1), obtaining a WVTR-time curve graph from the resistance-time curve value, and further obtaining a steady-state WVTR value of the barrier film;
wherein n is the reaction equivalent of water in the reaction process, if the final product of 1mol Ca and water is Ca (OH)2When 2mol of water is consumed in the reaction process, n is-2, deltaCaIs the density of Ca, generally deltaCa＝1.55g/cm3，ACaIs the area of the Ca membrane, AWMw is the molecular weight of water, M, for the effective area of the barrier filmCaIs the molecular weight of calcium, R is the measured resistance value of Ca film, RCaInitial resistance of Ca film at the time of starting test, h: the Ca film thickness at the start of the test, t is the test time.
In the present embodiment, a testing apparatus of a Ca film test card having four Ca film lines was used to test the water permeability of a 125 μm PET film in a 100 RH% testing environment at 40 ℃, and the 125 μm PET film was fixedly packaged between a cover plate and a jig main body;
testing the resistance of the Ca film by a four-wire method, wherein the testing voltage is 20mv, and the resistance is tested once per minute to obtain R-t resistance change curve graphs of four Ca film wires, as shown in figure 4;
substituting the R value obtained by testing into the formula 1), counting the obtained WVTR value once every 15min and averaging to obtain four Ca film line WVTR-t curves, and finally averaging according to the value when the WVTR reaches a steady state value to obtain the actually measured WVTR value of the barrier film. As shown in FIG. 5, the PET film obtained by the test had an observed steady state WVTR of 2.2 g.m-2·day-1The result is similar to the result obtained by other standard test methods after test verification.
The device for testing the water permeability of the barrier film by the electrical Ca film method provided by the embodiment of the invention can simply, conveniently and quickly fix and dismantle the barrier film, the test card and clean the clamp; the device for testing the water permeability of the barrier film by using the electrical Ca film method provided by the embodiment of the invention greatly improves the area utilization rate of the barrier film, and the effective utilization rate of the barrier film is improved to be close to 1/2.
The embodiment of the invention also provides a method for testing the water permeability of the barrier film, which has simple test flow, high efficiency and environmental protection; in addition, the embodiment of the invention also provides a method for testing the water permeability of the barrier film, so that the influence of uncertain resistivity on the test result is eliminated.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. An apparatus for electrical Ca membrane process water permeability testing of barrier membranes, characterized by comprising:
the clamp comprises a clamp body and a clamp body, wherein the clamp body comprises a containing cavity with a first opening, and an annular supporting table surface is formed on the inner wall of the containing cavity;
the Ca film testing component is arranged in the accommodating cavity and is positioned on one side of the supporting table board, which is far away from the first opening, and comprises a Ca film testing card which comprises a Ca film line;
the cover plate is provided with a second opening through which water and air can pass, and the cover plate can be arranged at the first opening of the accommodating chamber in an opening mode;
when the cover plate is fixedly arranged at the first opening of the accommodating cavity, the first part of the resistance membrane to be measured is fixedly pressed between the cover plate and the supporting table top and is tightly attached to the supporting table top, the second part of the resistance membrane to be measured completely covers the first opening area of the accommodating cavity, and the second opening corresponds to the second part of the resistance membrane to be measured.
2. The apparatus of claim 1, wherein: the cover plate is also provided with a pressing part corresponding to the supporting table surface, the pressing part is arranged around the second opening,
when the cover plate is fixedly arranged at the first opening of the accommodating cavity, the pressing part is attached to the supporting table top, or the gap between the pressing part and the supporting table top is smaller than the thickness of the first part of the diaphragm to be measured.
3. The apparatus of claim 1 or 2, further comprising: an annular elastic pressing component arranged between the cover plate and the supporting table top,
when the cover plate is fixedly arranged at the first opening of the accommodating cavity, the elastic pressing part can be respectively contacted with the cover plate and the supporting table top, and the elastic pressing part is in an elastic compression state.
4. The apparatus of claim 3, wherein: the elastic pressing part is arranged on the cover plate and surrounds the second opening.
5. The apparatus according to claim 4, comprising two or more elastic pressing members, wherein the two or more elastic pressing members are arranged at intervals along a radial direction of the second opening; preferably, the cover plate is further provided with an accommodating groove, and the elastic pressing part is arranged in the accommodating groove.
6. The apparatus of claim 4, wherein: a step structure is further formed at the first opening, and the surface of the step structure forms the supporting table-board;
preferably, the support table is a smooth and continuous plane.
7. The apparatus of claim 1, wherein: the Ca film testing assembly also comprises a circuit board, the Ca film testing card and the circuit board are arranged on a fixing frame and are electrically connected, and the fixing frame is detachably arranged in the accommodating cavity;
preferably, the Ca film test card includes a substrate, and an electrode and a Ca film formed on the substrate, the Ca film including a plurality of Ca film lines electrically connected to the electrode.
8. The apparatus of claim 1, wherein: the clamp body comprises a first clamp and a second clamp, and the first clamp and the second clamp are detachably connected and enclose to form the accommodating chamber;
preferably, the cover plate is combined with the clamp body in a sealing way; preferably, the first clamp and the second clamp are sealingly joined.
9. A method of testing the water permeability of a barrier film, comprising:
providing the device of any one of claims 1-8 and sealingly securing the barrier film between the cover plate and the support table of the fixture body and placing the fixture body encapsulating the barrier film in a test environment;
applying an electrical signal to a Ca film testing component in the clamp body, collecting the resistance value of the Ca film line within a fixed time interval, and obtaining the water permeation rate WVTR of the barrier film according to formula 1);
wherein n is the reaction equivalent of water in the reaction process, deltaCaIs the density of Ca, ACaCa film area, Aw barrier film effective area, Mw water molecular weight, MCaIs the molecular weight of calcium, R is the measured resistance value of Ca film, RCaInitial resistance of Ca film at the time of starting test, h: the Ca film thickness at the start of the test, t is the test time.
10. The testing method of claim 9, further comprising: the method comprises the steps of firstly arranging vacuum grease on the supporting table top, then sealing and attaching the first part of the barrier film on the supporting table top, enabling the second part of the barrier film to completely cover the first opening area of the accommodating chamber, and enabling the second opening to correspond to the second part of the barrier film to be tested.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210256165.XA CN114563325A (en) | 2022-03-15 | 2022-03-15 | Device and method for testing water permeability by electrical Ca membrane method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210256165.XA CN114563325A (en) | 2022-03-15 | 2022-03-15 | Device and method for testing water permeability by electrical Ca membrane method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114563325A true CN114563325A (en) | 2022-05-31 |
Family
ID=81719400
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210256165.XA Pending CN114563325A (en) | 2022-03-15 | 2022-03-15 | Device and method for testing water permeability by electrical Ca membrane method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114563325A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105973548A (en) * | 2016-05-07 | 2016-09-28 | 上海大学 | Water vapor transmittance testing clamp based on active metal electrical method |
| CN106979916A (en) * | 2016-01-15 | 2017-07-25 | 张家港康得新光电材料有限公司 | The test device of water vapor rejection film |
| CN107449704A (en) * | 2017-05-22 | 2017-12-08 | 茆胜 | The method of testing of film water vapor transmittance |
| CN109696390A (en) * | 2019-01-28 | 2019-04-30 | 中山大学 | The device of electric-resistivity method testing film gas permeation rate and its production, test method |
| CN111781120A (en) * | 2020-06-24 | 2020-10-16 | 吉林大学 | Testing method for thin film package |
| CN111971168A (en) * | 2018-02-02 | 2020-11-20 | 凸版印刷株式会社 | Gas barrier film and method for producing same |
| CN112461732A (en) * | 2020-12-14 | 2021-03-09 | 赣州优膜科技有限公司 | Testing arrangement of super high barrier film's steam transmissivity |
-
2022
- 2022-03-15 CN CN202210256165.XA patent/CN114563325A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106979916A (en) * | 2016-01-15 | 2017-07-25 | 张家港康得新光电材料有限公司 | The test device of water vapor rejection film |
| CN105973548A (en) * | 2016-05-07 | 2016-09-28 | 上海大学 | Water vapor transmittance testing clamp based on active metal electrical method |
| CN107449704A (en) * | 2017-05-22 | 2017-12-08 | 茆胜 | The method of testing of film water vapor transmittance |
| CN111971168A (en) * | 2018-02-02 | 2020-11-20 | 凸版印刷株式会社 | Gas barrier film and method for producing same |
| CN109696390A (en) * | 2019-01-28 | 2019-04-30 | 中山大学 | The device of electric-resistivity method testing film gas permeation rate and its production, test method |
| CN111781120A (en) * | 2020-06-24 | 2020-10-16 | 吉林大学 | Testing method for thin film package |
| CN112461732A (en) * | 2020-12-14 | 2021-03-09 | 赣州优膜科技有限公司 | Testing arrangement of super high barrier film's steam transmissivity |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP1841002B1 (en) | Battery leakage detection system | |
| US20110214504A1 (en) | Disposable pressure sensor systems and packages therefor | |
| US8664963B2 (en) | Test device for measuring permeability of a barrier material | |
| CN102062671A (en) | Method for detecting leakage of lithium ion battery | |
| KR20130059173A (en) | Complexed structure having separation membrane used for sensing gas, gas-sensing apparatus comprising the same, method and apparatus for measuring gas concentration | |
| CN106896271A (en) | A kind of apparatus and method for the test of battery diaphragm electrical conductivity | |
| CN201876343U (en) | Lithium ion battery leakage detecting device | |
| KR20080062969A (en) | Fixation device for insulation resistance measurement of battery | |
| CN114563325A (en) | Device and method for testing water permeability by electrical Ca membrane method | |
| JP2007248313A (en) | Constant-potential electrolysis type gas sensor | |
| CN110133061B (en) | High-temperature sample table suitable for testing dielectric property of material | |
| JP6873508B2 (en) | Electrochemical gas sensor system with improved accuracy and speed | |
| US8773152B2 (en) | Device for detecting physical state variables of a medium | |
| WO2003062779A1 (en) | Pressure sensor, flowmeter electronic component, and method for manufacturing the same | |
| JP6622593B2 (en) | Sensor inspection method and sensor manufacturing method | |
| RU186174U1 (en) | Device for rapid assessment of gas permeability of proton-conducting membrane of a fuel cell | |
| KR101057881B1 (en) | Jig Device for Insulation Testing of Cell Module Assemblies | |
| US8110081B2 (en) | Oxygen sensor improvement method | |
| GB2299863A (en) | Electrochemical measuring sensor | |
| CN212410498U (en) | Hydrogen sensor | |
| TWI633291B (en) | High-pressure sealed box device and method for measuring water vapor permeability of soft board | |
| JPH06273248A (en) | Pressure sensor and manufacture thereof | |
| CN206618804U (en) | A kind of device tested for battery diaphragm electrical conductivity | |
| JP2864878B2 (en) | Galvanic cell type oxygen sensor | |
| JP2003121284A (en) | Semiconductor pressure detection device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |