KR20120138468A - Method and apparatus for measuring transmission of water vapor and oxygen - Google Patents

Method and apparatus for measuring transmission of water vapor and oxygen Download PDF

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KR20120138468A
KR20120138468A KR1020110057958A KR20110057958A KR20120138468A KR 20120138468 A KR20120138468 A KR 20120138468A KR 1020110057958 A KR1020110057958 A KR 1020110057958A KR 20110057958 A KR20110057958 A KR 20110057958A KR 20120138468 A KR20120138468 A KR 20120138468A
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space
gas
polymer membrane
helium
nitrogen
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KR1020110057958A
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Korean (ko)
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유지범
조성민
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성균관대학교산학협력단
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Priority to KR1020110057958A priority Critical patent/KR20120138468A/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/44—Resins; Plastics; Rubber; Leather
    • 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
    • G01N2015/086—Investigating permeability, pore-volume, or surface area of porous materials of films, membranes or pellicules

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  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The present application relates to a method and apparatus for measuring moisture and oxygen permeability of a measurement object using helium gas.

Description

METHOD AND APPARATUS FOR MEASURING TRANSMISSION OF WATER VAPOR AND OXYGEN}

The present application relates to a method and apparatus for measuring moisture permeability and oxygen permeability of a measurement object using helium gas.

Organic devices used in fields such as organic light emitting devices, organic semiconductors, organic solar cells or thin film cells are very sensitive to moisture or oxygen present in the air and are easily decomposed. Therefore, it is common to prevent decomposition of the organic device by moisture and oxygen by applying a gas barrier material to the organic device. Accordingly, the water vapor transmission rate (WVTR) and oxygen transmission rate (OTR) of the material may be the most important factors for the selection of the gas barrier material.

On the other hand, as a method of measuring the moisture permeability and oxygen permeability of the material, there is a method of measuring the water permeability or oxygen permeability of the measurement target by using a radioactive tracer, but there is a problem of using a radioactive substance harmful to the human body. .

As another measuring method, there is a method of measuring moisture permeability or oxygen permeability of a measurement target using calcium (Calcium Test), but there is a problem that the measurement takes a long time and is expensive.

On the other hand, in the conventional water permeability measurement method, one surface of the object to be measured is placed in air containing moisture, and dry nitrogen gas is introduced to the other side of the object to be measured to contact the dried nitrogen with moisture that has passed through the object. After measuring the amount of moisture contained in the nitrogen, the amount of moisture passing through the thin film at a predetermined time was measured. However, this measurement method causes an error due to moisture permeating to the periphery of the measurement object, and when the permeability of the measurement object is small, there is a problem that the measurement takes a long time.

Accordingly, the present application is to measure the water permeability and oxygen permeability of the measurement object using helium gas, which is small in size and does not exist in the air, in order to improve the accuracy of the method of measuring the moisture permeability and oxygen permeability and to shorten the measurement time, and To provide a device.

However, the problems to be solved by the present invention are not limited to the problems described above, and other problems not described can be clearly understood by those skilled in the art from the following description.

A first aspect of the present application, in the first space and the second space divided by the measurement object, helium gas is introduced into the first space; Passing nitrogen gas through the second space; A helium gas that penetrates the measurement object from the first space and flows into the second space is mixed with nitrogen gas passing through the second space to form a nitrogen-helium mixed gas; Measure the molarity (C He ) of helium gas in the nitrogen-helium mixed gas flowing out of the second space; Measuring the water permeability (WVTR) of the helium gas by converting the molar concentration (C He ) of the helium gas into the amount of water that has passed through the measurement object by the following formula (1): Provide the method:

Formula (1)

WVTR = (18? C He ? V 2 ) / (A? T);

In the formula, C He represents the molar concentration of helium gas in the nitrogen-helium mixed gas, V 2 is the volume of the second space, A is the area of the object to be measured, and t is the measured time.

According to one embodiment of the present application, the first space may be in a vacuum state before helium gas is introduced, but is not limited thereto.

According to one embodiment of the present application, the second space may be in a vacuum state before passing nitrogen gas, but is not limited thereto.

According to one embodiment of the present application, the molarity (C He ) of helium gas in the nitrogen-helium mixed gas may be measured by a mass spectroscope, but is not limited thereto.

According to one embodiment of the present application, the measurement object may include, but is not limited to, an organic film, an inorganic film, a single organic / inorganic composite film, a multilayer organic / inorganic composite film, or a combination thereof. For example, the organic membrane may include a polymer membrane, and the polymer membrane may include, for example, an olefin polymer membrane, an ester polymer membrane, an ether polymer membrane, an acrylonitrile polymer membrane, a thioether polymer membrane, An aromatic vinyl polymer film, a nitrogen-containing polymer film, a fluorine-containing polymer film, an acrylic polymer film, or a combination thereof may be included, but is not limited thereto. For example, the inorganic film may include an aluminum oxide film, an aluminum nitride film, a silicon oxide film, a silicon nitride film, or a combination thereof, but is not limited thereto.

According to a second aspect of the present invention, in a first space and a second space divided by a measurement object, helium gas is introduced into the first space; Passing nitrogen gas through the second space; A helium gas that penetrates the measurement object from the first space and flows into the second space is mixed with nitrogen gas passing through the second space to form a nitrogen-helium mixed gas; Measure the molarity (C He ) of helium gas in the nitrogen-helium mixed gas flowing out of the second space; Measuring the oxygen permeability (OTR) of the measurement target by converting the molarity (C He ) of the helium gas into an amount of oxygen that has passed through the measurement target by the following formula (2): Provide the method:

Equation (2)

OTR = (32? C He ? V 2 ) / (A? T);

In the formula, C He Is the molar concentration of helium gas in the nitrogen-helium mixed gas, V 2 is the volume of the second space, A is the area of the object to be measured, and t is the time measured.

According to one embodiment of the present application, the first space may be in a vacuum state before helium gas is introduced, but is not limited thereto.

According to one embodiment of the present application, the second space may be in a vacuum state before passing nitrogen gas, but is not limited thereto.

According to one embodiment of the present application, the molarity (C He ) of helium gas in the nitrogen-helium mixed gas may be measured by a mass spectroscope, but is not limited thereto.

According to one embodiment of the present application, the measurement object may include, but is not limited to, an organic film, an inorganic film, a single organic / inorganic composite film, a multilayer organic / inorganic composite film, or a combination thereof. For example, the organic membrane may include a polymer membrane, and the polymer membrane may include, for example, an olefin polymer membrane, an ester polymer membrane, an ether polymer membrane, an acrylonitrile polymer membrane, a thioether polymer membrane, An aromatic vinyl polymer film, a nitrogen-containing polymer film, a fluorine-containing polymer film, an acrylic polymer film, or a combination thereof may be included, but is not limited thereto. For example, the inorganic film may include an aluminum oxide film, an aluminum nitride film, a silicon oxide film, a silicon nitride film, or a combination thereof, but is not limited thereto.

According to a third aspect of the present invention, there is provided an apparatus comprising: a first chamber including means capable of introducing helium gas from the outside; A second chamber comprising means for introducing nitrogen gas from the outside; Holding means for holding a measurement object provided at a portion where the first yarn and the second yarn communicate; An exhaust port through which the helium gas introduced into the first chamber passes through the measurement object and flows into the second chamber to be mixed with the nitrogen gas of the second chamber to flow out of the nitrogen-helium gas; And a detector provided in the exhaust port and capable of measuring the concentration of helium contained in the nitrogen-helium mixed gas.

The present application measures the helium permeability of the object to be measured using helium gas instead of directly injecting moisture or oxygen, and then converts the helium permeability into moisture permeability or oxygen permeability, thereby improving the accuracy of moisture permeability and oxygen permeability measurement. It is possible to provide a method and apparatus for measuring moisture and oxygen permeability, which shortens the measurement time and has a simple configuration. Specifically, there is no problem of generating an error due to moisture or oxygen permeating to the object to be measured by not using water vapor and oxygen to measure moisture and oxygen permeability, but instead using helium gas that is not present in the air. By using helium gas, even when the permeability of the measurement object is small, moisture and oxygen permeability can be measured in a relatively short time. In particular, the moisture permeability of the measurement object can be measured with a sensitivity of 10 -6 g / m 2 / day or less, and the oxygen permeability of the measurement object is 10 -6 cm 3 (STP) / m 2 / day / atm or less Can be measured.

1 is a schematic diagram of an apparatus for measuring moisture permeability and oxygen permeability in an embodiment of the present disclosure.

Hereinafter, embodiments and examples of the present invention will be described in detail with reference to the accompanying drawings, which will be readily apparent to those skilled in the art to which the present invention pertains.

It should be understood, however, that the present invention may be embodied in many different forms and is not limited to the embodiments and examples described herein. In the drawings, parts irrelevant to the description are omitted in order to clearly describe the present invention, and like reference numerals designate like parts throughout the specification.

Throughout this specification, when an element is referred to as "including " an element, it is understood that the element may include other elements as well, without departing from the other elements unless specifically stated otherwise.

As used herein, the terms "about", "substantially", and the like, are used at, or in close proximity to, numerical values when manufacturing and material tolerances inherent in the meanings indicated are provided to aid the understanding herein. In order to prevent the unfair use of unscrupulous infringers. In addition, throughout this specification, "step to" or "step of" does not mean "step for."

Hereinafter, an embodiment of a method for measuring moisture permeability and oxygen permeability of the present application will be described with reference to the drawings.

FIG. 1 schematically shows an apparatus for measuring moisture permeability and oxygen permeability of a measurement target 5 in one embodiment of the present application.

The apparatus for measuring moisture permeability and oxygen permeability includes a first chamber 1 having a flange 15 into which helium gas 20 is introduced, a measurement object 5, and a first chamber 1. And a second chamber 2 having a flange 15 located on the opposite side, and within the first chamber 1 there is a first space 3 into which the helium gas 20 is introduced. The second chamber may include a second space 4 through which the nitrogen gas 30 passes.

In order to introduce the helium gas 20, the helium gas introduction pipe 6 may be connected to the first chamber 1. The second chamber 2 discharges a nitrogen gas introduction conduit 7 for introducing the nitrogen gas 30 as a carrier gas, and a nitrogen-helium mixed gas 40 mixed in the second space 4. The exhaust conduit 8 can be connected. The exhaust conduit 8 may include a detector 9 capable of measuring the molarity (C He ) of helium gas in the nitrogen-helium mixed gas 40.

The said measurement object 5 can be hold | maintained by the holding means 10 provided in the side of the site | part which communicates the said 1st chamber 1 and the said 2nd chamber 2. The holding means 10 includes a sealing material 11 such as a 0-ring between the grooves 12 formed on the flange 15, and the measurement object 5 is inserted between the sealing materials 11. Can be. In addition, the flange 15, the bolt 13 is inserted and passed from one side of the flange, the nut 14 is fastened from the opposite side can be fixed.

Referring to FIG. 1, a method of measuring moisture permeability or oxygen permeability of the present application will be described in detail. The helium gas 20 is introduced into the first space 3, and the first space 3 is filled with helium gas. On the other hand, nitrogen gas 30 is introduced into the second space 4. Meanwhile, helium gas in the first space 3 penetrates the measurement object 5 and permeates into the second space 4 and is introduced into the second space 2, and nitrogen passes through the surface of the measurement object. It is mixed with the gas to form a nitrogen-helium mixed gas 40, which is introduced into the detector 9. The detector 9 measures the molar concentration of helium gas in the nitrogen-helium mixed gas 40 to measure the molar concentration of helium gas that has passed through the measurement object 5, and the molar concentration of helium gas thus measured. The water permeability or oxygen permeability of the measurement target 5 can be measured by converting the amount of water or oxygen transmitted through the measurement target.

Measuring the moisture permeability (WVTR) by converting the molar concentration of helium gas that has passed through the measurement object into the amount of water may be performed using the following equation (1):

Formula (1)

WVTR = (18? C He ? V 2 ) / (A? T);

In the formula, C He represents the molar concentration of helium gas in the nitrogen-helium mixed gas, V 2 is the volume of the second space, A is the area of the object to be measured, and t is the measured time.

Measuring the oxygen permeability (OTR) by converting the molar concentration of helium gas that has passed through the measurement object into the amount of water may be performed using the following equation (2):

Equation (2)

OTR = (32? C He ? V 2 ) / (A? T);

In the formula, C He Is the molar concentration of helium gas in the nitrogen-helium mixed gas, V 2 is the volume of the second space, A is the area of the object to be measured, and t is the time measured.

Meanwhile, the first space 3 may be in a vacuum state before the helium gas is introduced, and the second space 4 may be in a vacuum state before the nitrogen gas passes. Although not shown in FIG. 1, the first chamber 1 and the second chamber 2 may each be connected with a pump for vacuuming the first space 3 and the second space 4. have.

The molarity (C He ) of helium gas in the nitrogen-helium mixed gas 40 may be measured by the detector 9, and the detector 9 may include a mass spectroscope. However, the present invention is not limited thereto.

The measurement object 5 may include an organic film, an inorganic film, a single organic / inorganic composite film, a multilayer organic / inorganic composite film, or a combination thereof, but is not limited thereto. The organic membrane may include, for example, a polymer membrane, and the polymer membrane may include, for example, an olefin polymer membrane such as polyethylene, polypropylene, or polymethylpentene; Ester polymer membranes such as polyethylene terephthalate, polybutylene terephthalate, polycyclohexylenedimethylene terephthalate, polyarylate, and polycarbonate; Ether polymer membranes such as polyethylene oxide, polypropylene oxide, polyacetal, polyphenylene ether, polyether ether ketone, and polyetherimide; Sulfone polymer membranes such as polysulfone and polyether sulfone; Acrylonitrile-based polymer membranes such as polyacrylonitrile, AS resin, and ABS resin; Thioether polymer membranes such as polyphenylene sulfide; Aromatic vinyl polymer films such as polystyrene; Nitrogen-containing polymer membranes such as polyimide and aramid resins; Fluorine-containing polymer membranes such as polyethylene and polyvinylidene fluoride; Acrylic polymer films such as polymethyl methacrylate; Or combinations thereof: but is not limited thereto. The inorganic film may include, for example, an aluminum oxide film, an aluminum nitride film, a silicon nitride film, a silicon oxide film, or a combination thereof, but is not limited thereto.

Although described above with reference to a preferred embodiment of the present application, those skilled in the art that various modifications of the present invention without departing from the spirit and scope of the invention described in the claims below And can be changed.

1: first chamber 2: second chamber
3: first space 4: second space
5: measuring object 6: helium gas introduction pipe
7: nitrogen gas introduction pipeline 8: helium-nitrogen mixed gas exhaust pipeline
9: detector 10: holding means
11: seal 12: home
13: Bolt 14: Nut
15: flange 16: valve
17: valve 20: helium gas
30: nitrogen gas 40: nitrogen-helium mixed gas

Claims (17)

A first space and a second space divided by a measurement object, wherein helium gas is introduced into the first space;
Passing nitrogen gas through the second space;
A helium gas that penetrates the measurement object from the first space and flows into the second space is mixed with nitrogen gas passing through the second space to form a nitrogen-helium mixed gas;
Measure the molarity (C He ) of helium gas in the nitrogen-helium mixed gas flowing out of the second space;
Measuring the water permeability (WVTR) of the measurement target by converting the molar concentration (C He ) of the helium gas into the amount of water that has passed through the measurement target by the following equation (1):
Including, the method of measuring the moisture permeability:
Formula (1)
WVTR = (18? C He ? V 2 ) / (A? T);
In the formula, C He represents the molar concentration of helium gas in the nitrogen-helium mixed gas, V 2 is the volume of the second space, A is the area of the object to be measured, and t is the measured time.

The method of claim 1,
And the first space is in a vacuum state before the helium gas is introduced.
The method of claim 1,
And the second space is in a vacuum state before the nitrogen gas passes.
The method of claim 1,
The molar concentration (C He ) of helium gas in the nitrogen-helium mixed gas is measured by a mass spectroscope, the method for measuring moisture permeability.
The method of claim 1,
The measurement object is an organic membrane, an inorganic membrane, a single organic / inorganic composite membrane, a multilayer organic / inorganic composite membrane, or a combination thereof, the method for measuring moisture permeability.
The method of claim 5, wherein
The organic membrane comprises a polymer membrane (polymer membrane), the method of measuring moisture permeability.
The method according to claim 6,
The polymer membrane may include an olefin polymer membrane, an ester polymer membrane, an ether polymer membrane, an acrylonitrile polymer membrane, a thioether polymer membrane, an aromatic vinyl polymer membrane, a nitrogen-containing polymer membrane, a fluorine-containing polymer membrane, an acrylic polymer membrane, or a combination thereof. Phosphorus, moisture permeability measurement method.
The method of claim 5, wherein
The inorganic film is an aluminum oxide film, an aluminum nitride film, a silicon oxide film, a silicon nitride film, or a combination thereof, the measuring method of moisture permeability.
A first space and a second space divided by a measurement object, wherein helium gas is introduced into the first space;
Passing nitrogen gas through the second space;
A helium gas that penetrates the measurement object from the first space and flows into the second space is mixed with nitrogen gas passing through the second space to form a nitrogen-helium mixed gas;
Measure the molarity (C He ) of helium gas in the nitrogen-helium mixed gas flowing out of the second space;
Measuring the oxygen permeability (OTR) of the measurement object by converting the molar concentration (C He ) of the helium gas to the amount of oxygen that has passed through the measurement object by the following formula (2):
Method of measuring the oxygen permeability, comprising:
Equation (2)
OTR = (32? C He ? V 2 ) / (A? T);
In the formula, C He Is the molar concentration of helium gas in the nitrogen-helium mixed gas, V 2 is the volume of the second space, A is the area of the object to be measured, and t is the time measured.
The method of claim 9,
And the first space is in a vacuum state before the helium gas is introduced.
The method of claim 9,
And the second space is in a vacuum state before the nitrogen gas passes.
The method of claim 9,
The molar concentration (C He ) of helium gas in the nitrogen-helium mixed gas is measured by a mass spectrometer.
The method of claim 9,
The measurement object is a method for measuring oxygen permeability, including an organic film, an inorganic film, a single organic / inorganic composite film, a multilayer organic / inorganic composite film, or a combination thereof.
The method of claim 13,
The organic membrane comprises a polymer membrane (polymer membrane), measuring method of oxygen permeability.
15. The method of claim 14,
The polymer membrane may include an olefin polymer membrane, an ester polymer membrane, an ether polymer membrane, an acrylonitrile polymer membrane, a thioether polymer membrane, an aromatic vinyl polymer membrane, a nitrogen-containing polymer membrane, a fluorine-containing polymer membrane, an acrylic polymer membrane, or a combination thereof. Phosphorus, moisture permeability measurement method.
The method of claim 13,
The inorganic film is an aluminum oxide film, an aluminum nitride film, a silicon oxide film, a silicon nitride film, or a combination thereof, the measuring method of moisture permeability.
A first chamber comprising means capable of introducing helium gas from the outside;
A second chamber comprising means for introducing nitrogen gas from the outside;
A holding means for holding a measurement object provided at a portion where the first yarn and the second yarn communicate;
An exhaust port through which the helium gas introduced into the first chamber passes through the measurement object and flows into the second chamber to be mixed with the nitrogen gas of the second chamber to flow out; And
A detector provided in the exhaust port and capable of measuring the concentration of helium contained in the nitrogen-helium mixed gas:
A water permeability or oxygen permeability measuring device comprising a.
KR1020110057958A 2011-06-15 2011-06-15 Method and apparatus for measuring transmission of water vapor and oxygen KR20120138468A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103439240A (en) * 2013-09-09 2013-12-11 南京林业大学 Wood material moisture-penetrability test device
DE102013018070A1 (en) 2012-11-30 2014-06-05 Mando Corporation Method for controlling stopping of motor-driven type power steering apparatus mounted in vehicle, involves delaying stopping of motor-driven power steering apparatus for predetermined time depending on confirmation result
KR101585986B1 (en) 2014-07-10 2016-01-18 한국표준과학연구원 Apparatus and method for measuring of water vapor transmission rate using heating equipment
KR20160061898A (en) * 2014-11-24 2016-06-01 꼼미사리아 아 레네르지 아토미끄 에뜨 옥스 에너지스 앨터네이티브즈 Method and device for measuring permeation by mass spectrometry
CN106525683A (en) * 2016-10-27 2017-03-22 华中科技大学 Thin film permeability measuring device and method
CN109357989A (en) * 2018-12-14 2019-02-19 温州际高检测仪器有限公司 A kind of novel micro air permeability test instrument
CN112881256A (en) * 2020-12-30 2021-06-01 浙江汇力胶囊有限公司 Oxygen permeability detection device of hollow capsule
KR102589777B1 (en) * 2023-08-17 2023-10-13 강정민 Hydrogen transmission measurement system and measurement method using it

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102013018070A1 (en) 2012-11-30 2014-06-05 Mando Corporation Method for controlling stopping of motor-driven type power steering apparatus mounted in vehicle, involves delaying stopping of motor-driven power steering apparatus for predetermined time depending on confirmation result
CN103439240A (en) * 2013-09-09 2013-12-11 南京林业大学 Wood material moisture-penetrability test device
CN103439240B (en) * 2013-09-09 2015-08-12 南京林业大学 Wood material moisture-penetrabilitest test device
KR101585986B1 (en) 2014-07-10 2016-01-18 한국표준과학연구원 Apparatus and method for measuring of water vapor transmission rate using heating equipment
KR20160061898A (en) * 2014-11-24 2016-06-01 꼼미사리아 아 레네르지 아토미끄 에뜨 옥스 에너지스 앨터네이티브즈 Method and device for measuring permeation by mass spectrometry
CN106525683A (en) * 2016-10-27 2017-03-22 华中科技大学 Thin film permeability measuring device and method
CN106525683B (en) * 2016-10-27 2019-03-08 华中科技大学 A kind of film permeation rate measuring device and measurement method
CN109357989A (en) * 2018-12-14 2019-02-19 温州际高检测仪器有限公司 A kind of novel micro air permeability test instrument
CN109357989B (en) * 2018-12-14 2020-12-01 温州际高检测仪器有限公司 Novel micro-ventilation tester
CN112881256A (en) * 2020-12-30 2021-06-01 浙江汇力胶囊有限公司 Oxygen permeability detection device of hollow capsule
CN112881256B (en) * 2020-12-30 2024-05-10 浙江汇力胶囊有限公司 Oxygen permeability detection device for hollow capsules
KR102589777B1 (en) * 2023-08-17 2023-10-13 강정민 Hydrogen transmission measurement system and measurement method using it

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