CN111044431A - Test device and test method for water vapor transmission rate of thin film - Google Patents
Test device and test method for water vapor transmission rate of thin film Download PDFInfo
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Abstract
本发明公开一种薄膜水汽透过率的测试装置及测试方法，其中的方法包括：S1、将被测样品放置在测试光路中，光源发出的光经准直光学系统准直成准直光后入射到第一分光棱镜上，通过第一分光棱镜将准直光分成测量光和参考光；S2、测量光和参考光通过遮光板的开合控制分别进入图像采集相机，得到样品图像和参考图像；其中，测量光穿过被测样品进入到图像采集相机，参考光不穿过被测样品进入图像采集相机；S3、根据样品图像和参考图像计算被测样品的透过率变化系数；S4、根据该透过率变化系数计算水汽透过率。本发明通过利用钙单质与水汽反应过程中透过率的变换情况计算得到薄膜的水汽透过性能，有效提高薄膜水汽透过率的测试精度，测试精度可达10‑6g/m2/day。
The invention discloses a testing device and testing method for water vapor transmittance of thin films, wherein the method includes: S1. Place a sample to be tested in a testing optical path, and the light emitted by a light source is collimated by a collimating optical system into collimated light. Incident on the first dichroic prism, the collimated light is divided into measurement light and reference light by the first dichroic prism; S2, the measurement light and reference light respectively enter the image acquisition camera through the opening and closing control of the shading plate to obtain the sample image and the reference image ; wherein, the measurement light enters the image acquisition camera through the tested sample, and the reference light does not pass through the tested sample and enters the image acquisition camera; S3, calculate the transmittance variation coefficient of the tested sample according to the sample image and the reference image; S4, The water vapor transmission rate was calculated based on the transmission rate variation coefficient. The invention calculates the water vapor permeability of the film by utilizing the change of the permeability in the reaction process of the calcium element and the water vapor, thereby effectively improving the test accuracy of the water vapor permeability of the film, and the test accuracy can reach 10-6 g/m 2 /day. .
Description
Technical Field
The invention relates to the technical field of photoelectric measurement, in particular to a device and a method for testing the water vapor transmittance of a film.
Background
In recent years, the thin film packaging technology is further developed and widely applied in the fields of organic electroluminescent devices, thin film solar cells and the like, and particularly, the invention of a flexible display device enables the thin film packaging to become an indispensable link in the device preparation process. In order to ensure the service life of the flexible display device, the packaging material is required to have extremely high water oxygen barrier property, and the water vapor transmission rate of the packaging material can reach 10-6g/m2/day。
At present, the water vapor transmission rate of the film is usually measured by a pressure difference method, namely the film is placed in a test cavity, the test cavity is divided into two parts by the film, high-humidity gas is introduced into one part of the cavity, a high-sensitivity water vapor measuring sensor is placed in the other part of the cavity, the water vapor content of the film is measured by the water vapor measuring sensor in unit time, and then the water vapor transmission rate of the film is calculated.
The method has simple testing principle, convenient implementation, and capability of measuring food packaging and medicine packaging materials, but the testing precision of the method can only reach 10-4g/m2However, today cannot meet the requirement of testing the packaging performance of electronic devices, so it is urgently needed to develop a testing device and a testing method for the water vapor transmittance of a high-precision film.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and solve the problem that the test precision of a pressure difference method cannot meet the test requirement of the packaging performance of an electronic device, and provides a test device and a test method for the water vapor transmittance of a film.
The invention provides a testing device for the water vapor transmittance of a film, which comprises a light source, a collimating optical system, a first beam splitter prism, a second beam splitter prism and an image acquisition camera; the light emitted by the light source is collimated into collimated light by the collimating optical system and then is incident on the first light splitting prism, and the collimated light is split into measuring light and reference light by the first light splitting prism; the measuring light penetrates through the measured sample and then is converged to the image acquisition camera through the second beam splitter prism, and the reference light does not penetrate through the measured sample and then is converged to the image acquisition camera through the second beam splitter prism.
Preferably, the testing device further comprises a first reflecting prism, a second reflecting prism, a first electric shading plate and a second electric shading plate; the measuring light sequentially passes through the first electric shading plate and the measured sample, then enters the image acquisition camera through the transmission of the second beam splitter prism, the reference light passes through the second electric shading plate after being reflected by the first reflecting prism, then is reflected to the second beam splitter prism through the second reflecting prism, and then enters the image acquisition camera through the reflection of the second beam splitter prism.
Preferably, the testing device further comprises a sample frame arranged between the first electric shading plate and the second beam splitter prism, and the tested sample is fixed on the sample frame.
Preferably, the light source is a uniform area light source.
Preferably, the light source is an incandescent lamp or an LED lamp.
Preferably, the optical system is a transmissive optical system, a reflective optical system, or a combined transflective optical system.
The invention provides a method for testing the water vapor transmittance of a film, which comprises the following steps:
s1, placing the tested sample in a test light path, collimating light emitted by a light source into collimated light through a collimating optical system, then irradiating the collimated light onto a first light splitting prism, and splitting the collimated light into measuring light and reference light through the first light splitting prism;
s2, the measuring light and the reference light respectively enter the image acquisition camera through the opening and closing control of the light shielding plate to obtain a sample image and a reference image; the measuring light penetrates through a measured sample and then is converged to the image acquisition camera through the second beam splitter prism, and the reference light does not penetrate through the measured sample and then is converged to the image acquisition camera through the second beam splitter prism;
s3, calculating the transmittance change coefficient P of the tested sample according to the sample image and the reference image, wherein the calculation formula is as follows:
wherein T (T) is the transmittance of the sample measured at time T, T (0) is the transmittance of the sample measured at the initial time, T (∞) is the transmittance when the sample is completely transmitted, and the transmittance T is the gray-scale value of the sample image/the gray-scale value of the reference image;
s4, calculating the water vapor transmittance of the detected sample according to the transmittance change coefficient P of the detected sample, wherein the calculation formula is as follows:
wherein WVTR is water oxygen transmission, c is water oxygen transmission coefficient,
is the molar coefficient of water, mCaIs the molar coefficient of calcium, ρCaIs calcium density, ACaIs the area of the calcium film, dCaIs the thickness of the calcium film, AEThe package area is denoted as t, and the package time is denoted as t.
Preferably, step S1 is preceded by the following steps:
s0, preparing the calcium simple substance film as a sample to be detected by using a vacuum thermal deposition method.
Preferably, in the test light path, the measurement light sequentially passes through the first electric shading layer and the sample to be tested and then enters the image acquisition camera through the transmission of the second beam splitter prism; the reference light passes through the second electric shading plate after being reflected by the first reflecting prism, is reflected to the second beam splitter prism through the second reflecting prism, and enters the image acquisition camera through the reflection of the second beam splitter prism.
Preferably, step S2 specifically includes the following steps:
s201, opening a first electric shading plate and closing a second electric shading plate at the same time, so that measuring light enters an image acquisition camera in a testing device to form a sample image after passing through a tested sample;
s202, opening the second electric shading plate and closing the first electric shading plate at the same time, so that the reference light enters the image acquisition camera to form a reference image.
The invention can obtain the following technical effects:
the water vapor permeability of the film is calculated by utilizing the change condition of the permeability in the reaction process of the calcium simple substance and the water vapor, the test precision of the water vapor permeability of the film is effectively improved, and the test precision can reach 10-6g/m2/day。
Drawings
FIG. 1 is a schematic structural diagram of a device for testing the water vapor transmission rate of a film according to an embodiment of the present invention;
fig. 2 is a schematic flow chart of a method for testing the water vapor transmission rate of a film according to an embodiment of the invention.
Wherein the reference numerals include: the device comprises a light source 1, a collimating optical system 2, a first beam splitter prism 3, a reflecting prism 4, a first electric shading plate 5, an electric shading plate 6, a sample holder 7, a sample to be measured 8, a beam splitter prism 9, a reflecting prism 10 and an image acquisition camera 11.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not to be construed as limiting the invention.
The device for testing the water vapor transmittance of the film is used for obtaining two images, wherein one image is a sample image, the other image is a reference image, the sample image is obtained by irradiating a measured sample by measuring light and then entering an image acquisition camera for acquisition, the reference image is obtained by introducing reference light which does not irradiate the measured sample into the image acquisition camera for acquisition, the reference light and the measuring light are both emitted by the same light source, the reference light and the measuring light are collimated by a collimating optical system into collimating light and then are divided into the reference light and the measuring light by a beam splitter prism, and the reference light and the measuring light are finally converged to the image acquisition camera by the other beam splitter prism for acquisition to obtain the reference image and the sample image, thereby laying the foundation for the subsequent calculation of the water vapor transmittance of the measured sample.
The detected sample is a calcium simple substance film, and the transmittance of the calcium simple substance film is increased due to the fact that the calcium simple substance film reacts with water oxygen in the air to generate calcium hydroxide, so that the water vapor transmittance of the calcium simple substance film can be calculated by calculating the change condition of the transmittance of the calcium simple substance film by selecting the calcium simple substance film as the detected sample.
The following describes a specific embodiment of the device for testing the water vapor transmission rate of a film according to the present invention with reference to specific embodiments.
Referring to fig. 1, an apparatus for testing a water vapor transmittance of a film according to an embodiment of the present invention includes: the device comprises a light source 1, a collimating optical system 2, a first beam splitter prism 3, a first reflecting prism 4, a first electric shading plate 5, a second electric shading plate 6, a sample holder 7, a second beam splitter prism 9, a second reflecting prism 10 and an image acquisition camera 11; the collimating optical system 2 is arranged in front of the light source 1, the first beam splitter prism 3 is arranged in front of the collimating optical system 2, the first reflection prism 4 is arranged in the reflection direction of the first beam splitter prism 3, the second electric shading plate 6 and the second reflection prism 10 are respectively arranged in the reflection direction of the first reflection prism 4, the second electric shading plate 6 is arranged between the second reflection prism 10 and the first reflection prism 4, the first electric shading plate 5, the sample holder 7 and the second beam splitter prism 9 are respectively arranged in the transmission direction of the first beam splitter prism 3, the sample holder 7 is arranged between the first electric shading plate 5 and the second beam splitter prism 9, and the image collecting camera 11 is arranged in the emergent direction of the second beam splitter prism 9.
The light source 1 is used for emitting light and may be an incandescent lamp or an LED lamp, and when the light source 1 is an incandescent lamp, it may be a light source such as a tungsten halogen lamp, and the light source 1 is preferably a uniform surface light source, i.e. an integrating sphere light source, which may generate a uniform surface light source.
The collimating optical system 2 is used for collimating the light emitted by the light source 1 to form collimated light. The collimating optical system 2 may be a transmissive optical system, a reflective optical system, or a combined transflective optical system.
The first reflecting prism 4 is used for dividing collimated light into two paths, one path is reference light, and the other path is measuring light.
The first reflecting prism 4 is used to reflect the reference light to the second reflecting prism 10.
The second electric light shielding plate 6 plays a role of shielding the reference light, and when the second electric light shielding plate 6 is opened, the reference light is prevented from being reflected to the second reflecting prism 10, and when the second electric light shielding plate 6 is closed, the reference light is transmitted and reflected to the second reflecting prism 10.
The second reflecting prism 10 is used for reflecting the reference light to the second beam splitting prism 9.
The sample holder 7 is used for fixing the calcium simple substance film 8.
The first electric light shielding plate 5 plays a role in shielding the measuring light, when the first electric light shielding plate 5 is opened, the measuring light is prevented from irradiating the calcium simple substance film 8, and when the first electric light shielding plate 5 is closed, the reference light is made to irradiate the calcium simple substance film 8 and then is irradiated into the second beam splitter prism 9.
The second beam splitting prism 9 is used for converging the reference light and the measurement light to the image acquisition camera 11 for image acquisition.
The test light path of the test device is as follows: light emitted by the light source 1 is collimated into collimated light through the collimating optical system 2 and then enters the first beam splitter prism 3, the collimated light is divided into measuring light and reference light by the first beam splitter prism 3, the measuring light sequentially passes through the first electric shading plate 5 and the calcium simple substance film 8 and then enters the image acquisition camera 11 through transmission of the second beam splitter prism 9, the reference light is reflected by the first reflecting prism 4 and then passes through the second electric shading plate 6, and then is reflected to the second beam splitter prism 9 through the second reflecting prism 10 and then enters the image acquisition camera 11 through reflection of the second beam splitter prism.
It can be seen that the reference light does not irradiate the elemental calcium film 8, and the measurement light irradiates the elemental calcium film 8. When testing is carried out, firstly, the first electric shading plate 5 is opened, the second electric shading plate 6 is closed, the image acquisition camera 11 acquires one image, then the first electric shading plate 5 is closed, the second electric shading plate 6 is opened, the image acquisition camera 11 acquires another image, the image formed by the measuring light can have a tested sample area, and the image formed by the reference light can not have the tested sample area.
Through the comparative analysis of the two images, the transmittance change coefficient of the tested sample is calculated according to the change degree of the gray value of the tested sample area, and the calculation formula is as follows:
where T (T) is the transmittance of the sample measured at time T, T (0) is the transmittance of the sample measured at the initial time, T (∞) is the transmittance when the sample is completely transmitted, and the transmittance T is the gray-scale value of the sample image/the gray-scale value of the reference image.
And then calculating the water vapor transmittance of the calcium simple substance film 8 according to the transmittance change coefficient P of the calcium simple substance film 8, wherein the calculation formula is as follows:
wherein WVTR is water oxygen transmission, c is water oxygen transmission coefficient,
is the molar coefficient of water, mCaIs the molar coefficient of calcium, ρCaIs calcium density, ACaIs the area of the calcium film, dCaIs the thickness of the calcium film, AEThe package area is denoted as t, and the package time is denoted as t.
The device for testing the water vapor transmittance of the film provided by the embodiment of the invention can effectively improve the test precision of the water vapor transmittance of the calcium simple substance film 8 by calculating the water vapor transmittance of the calcium simple substance film 8 by utilizing the change condition of the transmittance in the reaction process of the calcium simple substance and the water vapor, and can achieve the aim of10-6g/m2/day。
The above details describe the testing apparatus for testing the water vapor transmittance of the film according to the embodiments of the present invention, and the present invention further provides a method for testing the film by using the testing apparatus for testing the water vapor transmittance of the film, corresponding to the testing apparatus.
Referring to fig. 2, a method for testing a water vapor transmittance of a film according to an embodiment of the present invention includes the following steps:
s1, placing the sample to be tested in a test light path, collimating the light emitted by the light source 1 into collimated light through the collimating optical system 2, then, emitting the collimated light onto the first light splitting prism 3, and splitting the collimated light into measuring light and reference light through the first light splitting prism 3.
Step S1 is preceded by the following steps:
s0, preparing the calcium simple substance film as a sample to be detected by using a vacuum thermal deposition method.
And preparing a layer of calcium simple substance film on the glass substrate by using a vacuum thermal deposition method to be used as the detected sample 8. The vacuum thermal deposition method for producing the calcium film is prior art and will not be described herein.
Preparing a packaging film on a glass substrate with a tested sample, wherein the packaging film completely covers the tested sample, the part of the packaging film except the part covering the tested sample can be tightly combined with the glass substrate, and the packaging film plays a role in packaging the tested sample.
The reason why the calcium simple substance film 8 is selected as the detected sample is that the calcium simple substance film 8 reacts with water oxygen in the air to generate calcium hydroxide, and the transmittance of the detected sample 8 is increased, so that the water vapor transmittance of the calcium simple substance film 8 can be calculated by calculating the change condition of the transmittance of the calcium simple substance film 8.
And S2, the measuring light and the reference light respectively enter the image acquisition camera through the opening and closing control of the light shielding plate to obtain a sample image and a reference image.
Step S2 specifically includes the following steps:
s201, opening the first electric light shielding plate 5 and closing the second electric light shielding plate 6, enabling the measuring light to pass through the calcium simple substance film 8 and then to be converged to the image collecting camera 11 through the second light splitting prism 9, and collecting the measuring light through the image collecting camera 11 to form a sample image.
Since the second motorized shade 6 is in the closed state, the reference light does not enter the image pickup camera 11.
S202, opening the second electric shading plate 6 and closing the first electric shading plate 5, so that the reference light does not pass through the calcium simple substance film 8 and then is converged to the image collecting camera 11 through the second light splitting prism 9, and is collected by the image collecting camera 11 to form a reference image.
Since the first electric shade 5 is in the closed state, the measurement light does not enter the image pickup camera 11.
S3, calculating the transmittance change coefficient P of the tested sample according to the sample image and the reference image, wherein the calculation formula is as follows:
where T (T) is the transmittance of the sample measured at time T, T (0) is the transmittance of the sample measured at the initial time, T (∞) is the transmittance when the sample is completely transmitted, and the transmittance T is the gray-scale value of the sample image/the gray-scale value of the reference image. Since the reference image does not have the detected sample region, but the sample image has the detected sample region, the transmittance change coefficient of the detected sample 8 can be calculated by analyzing the two images, and the transmittance change coefficient can reflect the change degree of the gray value of the detected sample region.
S4, calculating the water vapor transmittance of the detected sample according to the transmittance change coefficient P of the detected sample, wherein the calculation formula is as follows:
wherein WVTR is water oxygen transmission, c is water oxygen transmission coefficient,
is the molar coefficient of water, mCaIs the molar coefficient of calcium, ρCaIs calcium density, ACaIs the area of the calcium film, dCaIs the thickness of the calcium film, AEThe package area is denoted as t, and the package time is denoted as t.
Since the measured sample 8 reacts with the water oxygen in the air to generate calcium hydroxide, the transmittance of the measured sample 8 is increased, and therefore, the water vapor transmittance of the film can be calculated by calculating the change of the transmittance of the measured sample 8.
The change of the transmittance of the measured sample 8 is the transmittance ratio of the measured sample 8.
According to the method for testing the water vapor transmittance of the film, provided by the embodiment of the invention, the water vapor transmittance of the tested sample 8 is calculated by utilizing the change condition of the transmittance in the reaction process of the calcium simple substance and the water vapor, so that the test precision of the water vapor transmittance of the tested sample 8 can be effectively improved and can reach 10-6g/m2/day。
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
The above embodiments of the present invention should not be construed as limiting the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.
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| CN115979150B (en) * | 2023-03-01 | 2024-03-12 | 合肥东昇智能装备股份有限公司 | Method for detecting thickness of substrate through prism refraction |
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