CN105547956B - A kind of device and method of vacuum meter measurement film gas permeability - Google Patents
A kind of device and method of vacuum meter measurement film gas permeability Download PDFInfo
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- CN105547956B CN105547956B CN201510915889.0A CN201510915889A CN105547956B CN 105547956 B CN105547956 B CN 105547956B CN 201510915889 A CN201510915889 A CN 201510915889A CN 105547956 B CN105547956 B CN 105547956B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
- G01N15/0826—Investigating permeability by forcing a fluid through a sample and measuring fluid flow rate, i.e. permeation rate or pressure change
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Abstract
The invention discloses a kind of device and method of vacuum meter measurement film gas permeability, sensitivity existing for the problem of solving the problems, such as cost existing for existing mass spectrograph permeability test macro and pressure sensor method measuring system is low.The inventive system comprises gas sources and high-vacuum pump, the gas source is communicated with gas compartment through pipeline and pressure reducing valve, the gas compartment is communicated with the infiltration room for placing tested film, the infiltration room is equipped with infiltration chamber heater, the infiltration room is communicated with measuring chamber, the measuring chamber is equipped with measurement chamber heater, and the measuring chamber is connected with vacuum gauge, and the vacuum gauge is connected with vacuum meter；The high-vacuum pump is connected to through vacuum valve A with measuring chamber, and the high-vacuum pump is also connected to through vacuum valve B with gas compartment, and the high-vacuum pump is communicated with roughing pump through low vacuum valve.
Description
Technical field
The invention belongs to the gas permeability field of measuring technique of the encapsulating material of the objects such as electromechanical device, food, drug,
The device and method for specifically disclosing a kind of vacuum meter measurement film gas permeability.
Background technique
The packaging or encapsulating material for the gas permeability that electronic device, food, drug and other items need to have low, to prevent
During use and storage, pernicious gas enters in device (such as organic electroluminescence device), leads to performance or the longevity of device
Life decline；Or prevent pernicious gas from entering in food and pharmaceutical packing, cause food and drug rotten；Or prevent food or medicine
The material vapor evolution packaging of product is outer, leads to the quality decline or failure of food and drug.
Design and manufacture out encapsulation or the packing timber of the electronic device for meeting use and storage requirement, food and drug
Material must just have the equipment and measurement method measured to the gas permeability of these encapsulation or packaging material.
There are many kinds of the methods for measuring the gas permeability of material, common are pressure sensor method measurement dress in the market
It sets, but the pressure sensor that this device uses works under atmospheric pressure, it is insensitive to the variation of small pressure, so that surveying
It is very low to measure sensitivity, can only generally measure 10-1g/m2The permeability of day.Method also is surveyed using mass-spectrometer measurement technology
The gas permeability for measuring material, is shown in 4944180 A of United States Patent (USP) US, Chinese patent ZL 200810045129.9 and ZL
201310026422.1.This kind of device has the advantages that measurement sensitivity is very high, can measure 10-4—10-6g/m2The infiltration of day
Rate, but mass spectrometric expensive, and mass spectrometric sensitivity is unstable, needs that sensitivity school is arranged in measuring system
Standard apparatus, this just further increases cost, is unfavorable for the industrialization of measuring device.
Summary of the invention
The present invention is in order to solve the problems, such as cost and pressure sensor existing for existing mass spectrograph permeability test macro
The low problem of sensitivity existing for method measuring system, and device and the side of a kind of vacuum meter measurement film gas permeability are provided
Method overcomes mass spectrograph permeability measurement systems disadvantage at high cost, while measurement sensitivity is measured higher than pressure sensor method
System has the characteristics that practical.
In order to solve the above technical problems, the technical scheme adopted by the invention is that:
A kind of device of vacuum meter measurement film gas permeability, which is characterized in that described including gas source and high-vacuum pump
Gas source is communicated with gas compartment through pipeline and pressure reducing valve, and the gas compartment is communicated with the infiltration room for placing tested film, described
Infiltration room is equipped with infiltration chamber heater, and the infiltration room is communicated with measuring chamber, and the measuring chamber is equipped with measurement chamber heater,
The measuring chamber is connected with vacuum gauge, and the vacuum gauge is connected with vacuum meter；The high-vacuum pump connects through vacuum valve A and measuring chamber
Logical, the high-vacuum pump is also connected to through vacuum valve B with gas compartment, and the high-vacuum pump is communicated with roughing pump through low vacuum valve.
The gas compartment is equipped with pressure gauge.
The high-pressure vacuum pump is connected to through vacuum valve A and pumping speed restriction conduit with measuring chamber.
The molecular flow conductance of the pumping speed restriction conduit is less than the specified pumping speed of high-vacuum pump, and pumping speed restriction conduit
Molecular flow conductance is less than the molecular flow conductance of vacuum valve A.
The vacuum valve A and vacuum valve B is high vacuum valve.
The vacuum gauge is ionization gauge, and the vacuum is calculated as ion gauge.
Vacuum sealing between the edge of the tested film and the inner wall for permeating room.
The high-vacuum pump is turbomolecular pump, oil diffusion pump or cryo pump.
The roughing pump is rotary vane mechanical pump.
A kind of method of vacuum meter measurement film gas permeability, comprising the following steps:
Step 1: tested diaphragm seal is indoor in infiltration；
Step 2: opening vacuum valve A, vacuum valve B and low vacuum valve, starting roughing pump takes out low vacuum to system；
Step 3: when pressure gauge reading is 0 atmospheric pressure, high-vacuum pump is opened, to system pumping high vacuum；
Step 4: opening vacuum meter, measurement of vacuum；
Step 5: gauge is read less than 10-2When Pa magnitude, infiltration chamber heater and measurement chamber heater are opened, to infiltration
Saturating room and measuring chamber carry out bakeout degassing；
Step 6: it closes and measures chamber heater, adjusting infiltration type heater to specific temperature (such as 70 DEG C, 80 DEG C, 85
DEG C, 90 DEG C, 60 DEG C etc.)；
Step 7: when measurement room temperature is down to room temperature, vacuum meter reading is reduced to 10-4—10-5When Pa magnitude, record measurement
The background pressure value P of room0；If measurement room temperature is down to room temperature, vacuum meter reading does not reach 10-4—10-5When Pa magnitude, table
There is leak holes for bright system, should shut down leak detection and reparation.
Step 8: closing vacuum valve B, open pressure reducing valve, gas source is filled into gas compartment, so that the pressure P of gas compartment1
Pressure reducing valve is closed when reaching 1 atmospheric pressure, and time t=0 at this time.
Step 9: record measurement chamber pressure P2The numerical value of t at any time；
Step 10: working as P2Increase to after a certain saturation value is basically unchanged, records P2Value；
Step 11: setting P2-P0=P3, P3To be tested measurement chamber pressure value added caused by the gas infiltration of film, according to
Used ionization gauge is to the relative sensitivity characteristic of tested gas, to P3Value is modified, and obtains true P3Value, according to such as
Lower formula calculates permeability at a temperature of T；
Wherein, μ is the molal weight of gas, and C is molecular flow conductance of the pumping speed restriction conduit to tested gas, and R gas is general
Suitable constant, T are temperature (absolute temperature scale), and A is the infiltrating area of tested film.
Compared with prior art, the invention has the following advantages:
The caused gas pressure intensity of gas infiltration using ion gauge measurement film of the invention changes.Due to ionization
Vacuum meter is very cheap, furthermore the sensitivity of ion gauge is very stable, does not need often to calibrate, measuring system can be saved sensitive
Calibrating installation is spent, therefore the cost of measuring system can substantially reduce.In terms of measurement sensitivity, since ion gauge can be with
It measures down to 10-5—10-7The pressure of Pa is significantly higher than the sensitivity of pressure sensor (about to the measurement sensitivity of pressure change
1Pa), after the background pressure for considering measuring chamber is to the adverse effect of measurement pressure change sensitivity, ionization gauge measuring system
The lower limit of permeability survey can be expanded to 10-2—10-3g/m2Day magnitude is better than pressure sensor method permeability measurement systems.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention；
Marked in the figure: 1, gas source, 2, pressure reducing valve, 3, gas compartment, 4, pressure gauge, 5, infiltration room, 6, osmotic membrane, 7, infiltration
Chamber heater, 8, measuring chamber, 9, measurement chamber heater, 10, vacuum gauge, 11, vacuum meter, 12, pumping speed restriction conduit, 13, flange
A, 14, flange B, 15, vacuum valve A, 16, vacuum valve B, 17, roughing pump, 18, low vacuum valve, 19, high-vacuum pump.
Specific embodiment
The present invention will be further described with reference to the examples below, and described embodiment is only present invention a part
Embodiment is not whole embodiment.Based on the embodiments of the present invention, those skilled in the art are not making
Other embodiments used obtained, belong to protection scope of the present invention under the premise of creative work.
In conjunction with attached drawing, the device of vacuum meter measurement film gas permeability of the invention, including gas source 1 and high-vacuum pump
19, the gas source 1 is communicated with gas compartment 3 through pipeline and pressure reducing valve 2, and gas compartment 3 is equipped with pressure gauge 4, and the gas compartment 3 is connected to
There is the infiltration room 5 for placing tested film 6, the infiltration room 5 is equipped with infiltration chamber heater 7, and the infiltration room 5 is communicated with
Measuring chamber 8, the measuring chamber 8 are equipped with measurement chamber heater 9, and the measuring chamber 8 is connected with vacuum gauge 10, the vacuum gauge 10
It is connected with vacuum meter 11；The high-vacuum pump 19 is connected to through vacuum valve A15 with measuring chamber 8, and the high-vacuum pump 19 is also through vacuum
Valve B16 is connected to gas compartment 3, and the high-vacuum pump 19 is communicated with roughing pump 17 through low vacuum valve 18.
The high-pressure vacuum pump 19 is connected to through vacuum valve A15 and pumping speed restriction conduit 12 with measuring chamber 8.Wherein, pumping speed limits
The both ends of fast pipeline 12 are connected to through flange A13 and flange B14 with measuring chamber 8 and vacuum valve A respectively.
The molecular flow conductance of the pumping speed restriction conduit 12 is less than the specified pumping speed of high-vacuum pump 19, and pumping speed limitation pipe
The 12 molecular flow conductances in road are less than the molecular flow conductance of vacuum valve A15；So that effective pumping speed of the high-vacuum pump to measuring chamber 8
It is totally dependent on the molecular flow conductance value of pumping speed speed limit pipeline.
As a kind of preferred mode of the present invention, the vacuum valve A15 and vacuum valve B16 are high vacuum valve；The vacuum
Rule 10 are ionization gauge, and the vacuum meter 11 is ion gauge.
Vacuum sealing between the edge of the tested film and the inner wall for permeating room.
The high-vacuum pump is turbomolecular pump, oil diffusion pump or cryo pump.
The roughing pump is rotary vane mechanical pump.
Using the oxygen filled with purity higher than 99% as gas source；Tested film is PET plastic film, is measurement oxygen pair
Permeability when PET plastic film is at T=80 DEG C.Valve used of the invention is in closed state, Ge Gerong before testing
Atmosphere is full of in device and pipeline, each equipment is not powered on.Certain present invention can also measure other gas sources for other materials
Permeability of the film under specific temperature (such as T=70 DEG C, 75 DEG C).
Oxygen permeability of the test PET plastic film at T=80 DEG C below, it is further to step of the invention to be situated between
It continues.
Wherein, before test, all valves of system are in close state, and atmosphere is full of in each container and pipeline,
Each equipment is not powered on.
A kind of method of vacuum meter measurement film gas permeability, comprising the following steps:
Step 1: tested film 6 is sealed in infiltration room 5；
Step 2: opening vacuum valve A15, vacuum valve B16 and low vacuum valve 18, starting roughing pump 17 takes out system low true
It is empty；
Step 3: when the reading of pressure gauge 4 is 0 atmospheric pressure, high-vacuum pump 19 is opened, to system pumping high vacuum；
Step 4: opening vacuum meter 11, measurement of vacuum；
Step 5: gauge 11 is read less than 10-2When Pa magnitude, infiltration chamber heater 7 and measurement chamber heater 9 are opened,
Make to permeate 100 DEG C of 5 temperature of room arrival, 8 temperature of measuring chamber reaches 200 DEG C, carries out bakeout degassing；And keep the temperature 2 of heater
A hour or more achievees the purpose that bakeout degassing；
Step 6: closing measurement chamber heater 9, adjust the temperature of infiltration type heater 7 to 80 DEG C；
Step 7: when 8 temperature of measuring chamber is down to room temperature, the reading of vacuum meter 11 is reduced to 10-4—10-5When Pa magnitude, record
The background pressure value P of measuring chamber 80；If 8 temperature of measuring chamber is down to room temperature, vacuum meter reading does not reach 10-4—10-5Pa amount
When grade, showing system, there is leak holes, should shut down leak detection and reparation.
Step 8: closing vacuum valve B16, open pressure reducing valve 2, oxygen is filled into gas compartment 3, so that the pressure of gas compartment 3
Strong P1Pressure reducing valve is closed when reaching 1 atmospheric pressure, and time t=0 at this time.
Step 9: record 8 pressure P of measuring chamber2The numerical value of t at any time；
Step 10: working as P2Increase to after a certain saturation value is basically unchanged, records P2Value；
Step 11: setting P2-P0=P3, P3To be tested measurement chamber pressure value added caused by the gas infiltration of film, according to
Used ion gauge is to the relative sensitivity characteristic (see related " vacuum technique " textbook) of tested gas, to P3Be worth into
Row amendment, obtains true P3Value, calculates permeability at a temperature of T according to the following formula；
Wherein, μ is the molal weight of gas, and C is pumping speed restriction conduit to the molecular flow conductance of tested gas, and R is gas
Universal constant, T are temperature (absolute temperature scale), and A is the infiltrating area of tested film.
Wherein, if the pumping speed S of 19 pumping hole of high-vacuum pump1, the effective pumping speed to measuring chamber 8 is S2, then vacuum system is from measurement
The gas flow taken away in room are as follows:
Q1=P2·S2
If pumping speed restriction conduit 12 is C to the molecular flow conductance of tested gas, and C < < S1, then
Obtain Q1=P2·C
According to the equation of gas state, the gas flow that the unit time flows through certain pipeline section is
In above formula: the pressure at P-pipeline section
V-unit time flows through the gas volume of the pipeline section
M-unit time flows through the gaseous mass of the pipeline section
μ-gas molal weight
R-gas universal constant
T-temperature (absolute temperature scale).
Claims (1)
1. a kind of method of vacuum meter measurement film gas permeability, the device that wherein this method uses includes gas source and high vacuum
Pump, the gas source are communicated with gas compartment through pipeline and pressure reducing valve, and the gas compartment is communicated with the infiltration for placing tested film
Room, the infiltration room are equipped with infiltration chamber heater, and the infiltration room is communicated with measuring chamber, and the measuring chamber is equipped with measuring chamber
Heater, the measuring chamber are connected with vacuum gauge, and the vacuum gauge is connected with vacuum meter；The high-vacuum pump through vacuum valve A and
Pumping speed restriction conduit is connected to measuring chamber；The molecular flow conductance of the pumping speed restriction conduit is less than the specified pumping speed of high-vacuum pump,
And the molecular flow conductance of pumping speed restriction conduit is less than the molecular flow conductance of vacuum valve A；The high-vacuum pump also through vacuum valve B and
Gas compartment connection, the high-vacuum pump are communicated with roughing pump through low vacuum valve；The vacuum gauge is ionization gauge, the vacuum meter
For ion gauge；The gas compartment is equipped with pressure gauge；The vacuum valve A and vacuum valve B is high vacuum valve；It is described be tested it is thin
Vacuum sealing between the edge of film and the inner wall for permeating room, which comprises the following steps:
Step 1: tested diaphragm seal is indoor in infiltration；
Step 2: opening high vacuum valve A, high vacuum valve B and low vacuum valve, starting roughing pump takes out low vacuum to system；
Step 3: when pressure gauge reading is 0 atmospheric pressure, high-vacuum pump is opened, to system pumping high vacuum；
Step 4: opening ion gauge, measurement of vacuum；
Step 5: gauge is read less than 10-2When Pa magnitude, infiltration chamber heater and measurement chamber heater are opened, to infiltration room
Bakeout degassing is carried out with measuring chamber；
Step 6: closing measurement chamber heater, adjust infiltration chamber heater to specific temperature；
Step 7: when measurement room temperature is down to room temperature, ion gauge reading is reduced to 10-4-10-5When Pa magnitude, measuring chamber is recorded
Background pressure value P0；
Step 8: closing high vacuum valve B, open pressure reducing valve, gas source is filled into gas compartment, so that the pressure P of gas compartment1Reach
Pressure reducing valve is closed when 1 atmospheric pressure, and time t=0 at this time；
Step 9: record measurement chamber pressure P2T and the numerical value that changes at any time；
Step 10: working as P2Increase to after a certain saturation value is basically unchanged, records P2Value；
Step 11: setting P2-P0=P3, P3To be tested measurement chamber pressure value added caused by the gas infiltration of film, according to as follows
Formula calculates permeability at a temperature of T；
Wherein, μ is the molal weight of gas, and C is molecular flow conductance of the pumping speed restriction conduit to tested gas, and R is that gas is pervasive
Constant, T are temperature, and A is the infiltrating area of tested film.
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| CN201510915889.0A CN105547956B (en) | 2015-12-10 | 2015-12-10 | A kind of device and method of vacuum meter measurement film gas permeability |
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| CN201510915889.0A CN105547956B (en) | 2015-12-10 | 2015-12-10 | A kind of device and method of vacuum meter measurement film gas permeability |
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| CN105547956B true CN105547956B (en) | 2019-05-24 |
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