CN108445037A - A kind of test method of stress in thin films - Google Patents
A kind of test method of stress in thin films Download PDFInfo
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- CN108445037A CN108445037A CN201810062607.0A CN201810062607A CN108445037A CN 108445037 A CN108445037 A CN 108445037A CN 201810062607 A CN201810062607 A CN 201810062607A CN 108445037 A CN108445037 A CN 108445037A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/16—Investigating or analyzing materials by the use of thermal means by investigating thermal coefficient of expansion
Abstract
The present invention provides a kind of test method of stress in thin films, including step:One film sample to be measured is provided;Film sample to be measured is heated up to preset temperature with constant heating rate, the maximum contraction rate of film sample to be measured in temperature-rise period is obtained, to characterize the internal stress of film sample to be measured.Through the above scheme, the present invention is by testing and obtaining maximum contraction rate of the film sample to be measured during with constant speed heating, to characterize the internal stress of film to be measured, the internal stress for the characterization film to be measured that can be quantified, and film to be measured under the heating rate stablized, such as thin polymer film, generate phase transformation, it can stablize and measure its deformation situation, measuring accuracy is high, and the testing time of present invention test internal stress is determined by heating rate and range, it is not influenced by sample itself state, it can not only quantify and measure stress in thin films to be measured, and it can substantially shorten the testing time.
Description
Technical field
The invention belongs to membrane materials and field of new energy technologies, more particularly to a kind of test method of stress in thin films.
Background technology
New energy industry, the internal stress of the polymer porous membrane used in lithium ion battery are to influence lithium ion battery
One of an important factor for safety.If the internal stress of the porous membrane of the isolation film as lithium ion battery is too big, can cause
Film significant shrinkage in the short time when in use, causes positive and negative anodes short circuit even thermal runaway, ultimately causes lithium ion battery and catch fire
Or explosion.But the test of internal stress is characterized, all not quantitative analysis test method all the time.
Currently, common internal stress qualitative characterization is that film level is clipped in two pieces of transparent panels up and down, at 150 DEG C
Until film breaks, required baking time characterizes the internal stress of film for baking, and the time is shorter to illustrate that internal stress is bigger.The survey
Method for testing is easy by thin film shape, size, the material of upper lower clamp plate, the weight of upper lower clamp plate, baking oven heating rate, dries
The influence of many factors such as case volume, and judge that the time point of film breaks is also not easy to accurately control, it is easy erroneous judgement.And
And this method testing time is longer, can not estimate the time needed for each sample, sample can only be waited for be broken.
Therefore, a kind of test method of stress in thin films how is provided, to solve in the prior art to stress in thin films table
The above problem in the presence of sign is necessary.
Invention content
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of stress in thin films test side,
For solving, the prior art can not carry out test of quantitative analysis in stress in thin films characterization and measuring accuracy is low, test speed
The problems such as slow.
In order to achieve the above objects and other related objects, the present invention provides a kind of test method of stress in thin films, including
Step:
1) film sample to be measured is provided;And
2) film sample to be measured is heated up to preset temperature with constant heating rate, obtains and is waited for described in temperature-rise period
The maximum contraction rate for surveying film sample, to characterize the internal stress of the film sample to be measured.
As a preferred embodiment of the present invention, in step 2), a closure container is provided, and by the film sample to be measured
It is placed in the closure container, by heating up to the closure container, so that the film sample to be measured is with constant
Heating rate is warming up to the preset temperature.
As a preferred embodiment of the present invention, a clamping device is provided, the gripping apparatus grips are good described to be measured
The opposite both ends of film sample are placed in the closure container, wherein obtain the film sample to be measured along clamped both ends
Maximum contraction rate on line direction is to characterize the internal stress of the film sample to be measured.
As a preferred embodiment of the present invention, the chucking power of film sample to be measured described in the gripping apparatus grips between
Between 0.005N~2N.
Further include step in step 2) as a preferred embodiment of the present invention:It is passed through protection into the closure container
Gas, to prevent the film sample to be measured from being aoxidized.
As a preferred embodiment of the present invention, the protective gas includes that nitrogen, argon gas, helium and hydrogen are constituted
At least one of group;And the protective gas is passed through with the constant speed that is passed through, the speed that is passed through is between 10ml/min
Between~100ml/min.
As a preferred embodiment of the present invention, in step 2), the heating rate of the film sample to be measured is between 1
DEG C/min~60 DEG C/min between.
As a preferred embodiment of the present invention, in step 2), the preset temperature is between 0 DEG C~600 DEG C.
As a preferred embodiment of the present invention, in step 2), tests and obtain film sample to be measured described in temperature-rise period
The inflection curves of product, to obtain the maximum contraction rate of the film sample to be measured.
As a preferred embodiment of the present invention, in step 1), the surface shape of the film sample to be measured includes rectangular
Shape in step 2), obtains maximum contraction rate of the film sample to be measured on the rectangular length direction.
As a preferred embodiment of the present invention, the film sample to be measured is selected from thin polymer film, the polymer
The material of film includes polyolefin, polyamide, polyimides, polyester, fluorine class polyolefin, polyethylene, polypropylene, aramid fiber, nonwoven
At least one of the group that cloth, Kynoar, polytetrafluoroethylene (PTFE) and polyethylene terephthalate are constituted.
As described above, the test method of the stress in thin films of the present invention, has the advantages that:
The present invention provides a kind of test method of stress in thin films, by testing and obtaining film sample to be measured with constant
Speed heating during maximum contraction rate, it is to be measured so as to quantitative characterization to characterize the internal stress of film to be measured
The internal stress of film, characteristic manner of the invention, film (such as thin polymer film) to be measured generates phase under stable heating rate
Transformation measures its deformation situation so as to stablize, and measuring accuracy is high, and the testing time of present invention test internal stress is by heating up
What speed and range were determined, it is not influenced by sample itself state, can not only quantify and measure film to be measured, especially resistance to height
The internal stress of warm film, and can substantially shorten the testing time.
Description of the drawings
Fig. 1 is shown as the flow chart of the stress in thin films test method of the present invention.
Fig. 2 is shown as stress in thin films of the present invention and tests the song that the length of film sample to be measured in an example changes over time
Line chart.
Component label instructions
S1~S2 steps 1)~step 2)
Specific implementation mode
Illustrate that embodiments of the present invention, those skilled in the art can be by this specification below by way of specific specific example
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also be based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
It please refers to Fig.1 to Fig. 2.It should be noted that the diagram provided in the present embodiment only illustrates this in a schematic way
The basic conception of invention, though package count when only display is with related component in the present invention rather than according to actual implementation in diagram
Mesh, shape and size are drawn, when actual implementation form, quantity and the ratio of each component can be a kind of random change, and its
Assembly layout form may also be increasingly complex.
As shown in Figure 1, the present invention provides a kind of test method of stress in thin films, include the following steps:
First, as shown in the S1 in Fig. 1, step 1) is carried out, a film sample to be measured is provided;
As an example, in step 1), the surface shape of the film sample to be measured includes rectangle, and in step 2), is surveyed
Try maximum contraction rate of the film sample to be measured on the rectangular length direction.
Specifically, preparing the sample for testing stress in thin films to be measured first, as an example, the film sample to be measured takes
From in the film to be measured for needing progress internal stress test, it is preferable that the film sample to be measured is prepared into strip, that is, is had
One length direction and size are less than the sample of the shape of the width direction of the length direction, and it is length to be preferably prepared to surface shape
Rectangular sample to be tested film, wherein the surface refers to the surface vertical with film thickness to be measured, the rectangular length
Ranging from 5~50mm, further preferably 8~24mm, this example selection be 20mm, the rectangular width range be 2~
10mm, preferably 3.5~4.5mm are selected as 4mm in this example, it should be noted that the sample of this shape takes convenient for test difference
To film internal stress, film is usually constructed with orientation, i.e., the Structural assignments of length direction and width direction are different, performance
It is variant, so rectangular film is made, convenient for the stress of the horizontal and vertical both direction of testing film respectively;In addition,
The test method of the present invention is to characterize internal stress by change in size, needs to minimize when testing the size in a direction another
The influence of the size of one dimension improves the accuracy of test so the sample of rectangular shape is made.
Then, as shown in the S2 in Fig. 1, step 2) is carried out, with the constant heating rate heating film sample to be measured
To preset temperature, the maximum contraction rate of film sample to be measured described in temperature-rise period is obtained, described in the maximum contraction rate characterization
The internal stress of film sample to be measured.
As an example, in step 2), a closure container is provided, and the film sample to be measured is placed in the closure container
In, by heating up to the closure container, so that the film sample to be measured is warming up to institute with constant heating rate
State preset temperature.
As an example, in step 2), a clamping device, the good film sample phase to be measured of the gripping apparatus grips are provided
To both ends after, be placed in the closure container, wherein obtain the film sample to be measured along the line side for being clamped both ends
Upward maximum contraction rate is to characterize the internal stress of the film sample to be measured.
As an example, the chucking power of film sample to be measured described in the gripping apparatus grips is between 0.005N~2N.
It heats up to the constant speed of film sample to be measured specifically, being realized in the step, as an example, by what is prepared
Film sample to be measured is placed in a closure container, can be held to the closure by the way that resistance wire in being closed container etc. is arranged
The cavity of device is heated, to realize heating up with constant heating rate to film sample to be measured, to be easy to ensure heating
The stability and controllability of process are such as felt it is of course also possible to be other heating modes well known within the skill of those ordinarily skilled
It should heat, irradiated heat, electric arc heated etc., wherein processing survey subsequently is carried out to film sample to be measured in the closure container
Examination, here, so-called closure container refer to other than gas is passed through the communication port of output, elsewhere all not with extraneous unicom
Channel.Wherein, sample is placed in the closure container, can first get well sample clamping to place into be closed in container, also
Can be closed container itself there is a hold assembly, putting sample into closure container is directly clamped with the hold assembly.
Preferably, it is selected as in this example and a clamping device is first provided, again by two after film sample to be measured is clamped
Person is put into jointly in the closure container, so as to facilitate control that the position of film sample to be measured is clamped, wherein when to be measured thin
When membrane sample is rectangle, the both ends clamping sample of rectangular length direction is preferably clamped, to the rectangular shape of side draw length
Become.In addition, the clamping device is the folder that can arbitrarily clamp film sample to be measured well known within the skill of those ordinarily skilled
Device is held, can be two fixtures, clamp the both ends of sample, then this fixture is fixed on to the inner wall etc. for being closed container,
This is not particularly limited.In addition, the chucking power is preferably between 0.005N~2N between 0.01N~0.05N, this
Example selection is 0.02N, so as to while keeping film not relaxed state, and not too large influences answering for film itself
Stress-strain, so as to obtain accurate ess-strain value.
As an example, in step 2), carry out during the test further including step:It is passed through into the closure container
Protective gas, to prevent the film sample to be measured from being aoxidized.
As an example, the protective gas includes at least one in the group that nitrogen, argon gas, helium and hydrogen are constituted
Kind, or the mixed gas that at least the two is constituted in above-mentioned gas;Preferably, the guarantor is passed through with the constant speed that is passed through
Protect gas, wherein the speed that is passed through is between 10ml/min~100ml/min.
Specifically, it is preferred that also needing to be passed through the protective gas in the closure container when testing, due to the test of the present invention
In method, in temperature elevation process, the material of film sample to be measured, such as polymer may be become by the size of oxidation influence itself
Change, so being passed through the inertia protection air-flow of constant speed, can prevent polymer from being aoxidized, further increase the precision of test,
In, the constant speed that is passed through for being passed through the protective gas is preferably between 40ml/min~60ml/min, this example selection
For 50ml/min.
As an example, in step 2), the heating rate of the film sample to be measured is between 1 DEG C/min~60 DEG C/min
Between, between preferably 3 DEG C/min~10 DEG C/min, 6 DEG C/min is selected as in this example.
As an example, the preset temperature is between 0 DEG C~600 DEG C.
As an example, in step 2), the inflection curves of film sample to be measured described in temperature-rise period are tested and obtain, with
To the maximum contraction rate of the film sample to be measured.
Specifically, film sample to be measured is placed after being closed in container, control heating so that film sample to be measured
Temperature is increased with constant heating rate, wherein temperature influences the phase transformation of film (film sample to be measured), and phase changed
Ess-strain occurs for film in journey, and stress refers to just the internal stress of film, and strain refers to just the length variation of film, stress and is answered
Change is mutual corresponding relationship, and during film shrunk, stress is bigger, and strain is also bigger, therefore, is based on film sample to be measured
Maximum contraction rate characterization film internal stress heated up with constant speed in temperature-rise period, polymerize under stable heating rate
Object film generates phase transformation, its deformation situation is measured so as to stabilization.
Specifically, in this example, by testing the deformation of film sample to be measured during heating, i.e., film sample to be measured
Length change with time, wherein the length of film sample to be measured changes over time figure for different thin-film material curves
Shape may be different, Fig. 2 provides a kind of example, tests out inflection curves to obtain the maximum contraction rate of sample, based on answering
The relationship of stress-strain, so as to symbolize the internal stress of film.
In addition, the preset temperature to be heated up when being tested is between 0~600 DEG C, preferably between 40~200 DEG C, example
Such as, the polyolefine isolating film used in lithium ion battery can usually be tested out at 200 DEG C or less, but novel resistance to
High temperature polymer isolation film, if the test temperature of aramid fiber isolation film can reach 400 DEG C even 500 DEG C, according to material selection, originally
The testing time of invention test internal stress is determined that temperature range/heating rate is to test by heating rate and range
Time is not influenced by sample itself state.Test error, which is mainly derived from sample size error caused by sample preparation precision, to be caused
's.
As an example, the film sample to be measured is selected from thin polymer film, the material of the thin polymer film includes poly-
Alkene, polyimides, polyester, fluorine class polyolefin, polyethylene, polypropylene, aramid fiber, non-woven fabrics, Kynoar, gathers polyamide
At least one of the group that tetrafluoroethene and polyethylene terephthalate are constituted.Stress in thin films based on the present invention
Test method can accurately and effectively test out the internal stress of the film of any one of the above material composition, applied widely.
The test method of the present invention is further described below in conjunction with specific comparative example and embodiment.
Comparative example 1
The film of this comparative example is polyethylene porous film, and the square sample of 5cm*5cm is made, saturating with weight about 200g
Bright glass plate is clipped in the middle, and is placed in 150 DEG C of baking ovens, the time required to observation film breaks calculate.Repeat experiment 3 times.
Comparative example 2
The film of this comparative example is aramid fiber coated porous film, the square sample of 5cm*5cm is made, with weight about 200g's
Transparency glass plate is clipped in the middle, and is placed in 150 DEG C of baking ovens, the time required to observation film breaks calculate.Repeat experiment 3 times.
Embodiment 1
The present embodiment polyethylene porous film, is made the Rectangular samples of 8mm long 4mm wide, is pressed from both sides at the both ends of length direction
Firmly, the power for loading 0.02N is placed in and is closed in container, and 180 DEG C are increased to from 40 DEG C with the speed of 5 DEG C/min, be closed in container with
The speed of 50mL/min is led into nitrogen.Test sample deformation rate and maximum contraction rate in temperature-rise period.Repeat experiment 3 times.
Embodiment 2
The present embodiment polyethylene porous film, is made the Rectangular samples of 16mm long 4.5mm wide, at the both ends of length direction
It clamps, loads the power of 0.01N, be placed in and be closed in container, be increased to 180 DEG C from 40 DEG C with the speed of 5 DEG C/min, be closed in container
Led into nitrogen with the speed of 50mL/min.Test sample deformation rate and maximum contraction rate in temperature-rise period.Repeat experiment 3 times.
Embodiment 3
The present embodiment polypropylene porous membrane, is made the Rectangular samples of 8mm long 4mm wide, is pressed from both sides at the both ends of length direction
Firmly, the power for loading 0.02N is placed in and is closed in container, and 200 DEG C are increased to from 50 DEG C with the speed of 5 DEG C/min, be closed in container with
The speed of 60mL/min is led into argon gas.Test sample deformation rate and maximum contraction rate in temperature-rise period.Repeat experiment 3 times.
Embodiment 4
The present embodiment aramid fiber coated porous film, is made the Rectangular samples of 8mm long 4mm wide, at the both ends of length direction
It clamps, loads the power of 0.01N, be placed in and be closed in container, be increased to 600 DEG C from 50 DEG C with the speed of 5 DEG C/min, be closed in container
Led into nitrogen with the speed of 50mL/min.Test sample deformation rate and maximum contraction rate in temperature-rise period.Repeat experiment 3 times.
Embodiment 5
The present embodiment aramid fiber coated porous film, is made the Rectangular samples of 8mm long 4mm wide, at the both ends of length direction
It clamps, loads the power of 0.01N, be placed in and be closed in container, be increased to 600 DEG C from 50 DEG C with the speed of 10 DEG C/min, be closed container
In led into nitrogen with the speed of 50mL/min.Test sample deformation rate and maximum contraction rate in temperature-rise period.Repeat experiment 3 times.
Wherein, the test evaluation result of comparative example 1-2 and embodiment 1-5 is as shown in table 1 below.
1 comparative example of table and embodiment evaluation test result
Project | Testing time/(min) | Test error (%) |
Comparative example 1 | 58 | 21 |
Comparative example 2 | >1440 | / |
Embodiment 1 | 28 | 0.1 |
Embodiment 2 | 28 | 0.1 |
Embodiment 3 | 30 | 0.2 |
Embodiment 4 | 110 | 0.1 |
Embodiment 5 | 55 | 0.2 |
The test result of embodiment 1-5 and comparative example 1-2 are evaluated:
1) mean test time/:The testing time of the average each sample of 3 experiments of record;
2) test error:The test error of 3 test results=(maximum value-minimum value)/average value * 100%;
It can be seen from Table 1 that:
Comparative example 1-2 has respectively carried out polyethylene film and aramid fiber coated film in 150 DEG C of baking rupture time survey
The test of stress, testing time of the average single sample of comparative example 1 are 58min, and 3 test errors are 21%, comparative example 2 by
It is very strong in aramid fiber coated film heat-resisting quantity, it is toasted in 150 DEG C of baking ovens, after observing 24H (1440min), film does not still have
Have fracture, can not this method measure quantitative result.
Embodiment 1-3 stress in thin films test methods using the present invention, have been respectively adopted two kinds of polyethylene and polypropylene
Porous membrane changes sample size, temperature range and power in preferred scope, and the protection gas and air inflow of use are equal
In preferred scope, the internal stress testing time is respectively 28min, 28min and 30min, and test error is no more than 1%.The present invention
The testing time of test internal stress is determined that temperature range/heating rate is the testing time by heating rate and range,
It is not influenced by sample itself state.Caused by test error is mainly derived from sample size error caused by sample preparation precision.It is real
It applies the internal stress that a 4-5 is aramid fiber coated film to test, wherein the heating rate of embodiment 4 is 5 DEG C/min, so when test
Between longer 110min, the heating rate of embodiment 5 is increased to 10 DEG C of min, and the corresponding testing time shortens to 55min.The two
Embodiment can not only quantify the internal stress for measuring high-temperature resistant membrane compared with comparative example 2, but also the testing time substantially shortens.
In conclusion the present invention provides a kind of test method of stress in thin films, including step:One film sample to be measured is provided
Product;And the film sample to be measured is heated up to preset temperature with constant heating rate, it obtains to be measured described in temperature-rise period
The maximum contraction rate of film sample, to characterize the internal stress of the film sample to be measured.Through the above scheme, the present invention provides one
The test method of kind of stress in thin films, by testing and obtaining film sample to be measured with constant speed heating during
Maximum contraction rate, it is of the invention so as to the internal stress of quantitative characterization film to be measured to characterize the internal stress of film to be measured
Characteristic manner, film (such as thin polymer film) to be measured generates phase transformation under stable heating rate, it is measured so as to stabilization
Deformation situation, measuring accuracy is high, and the testing time of present invention test internal stress is determined by heating rate and range, no
It is influenced by sample itself state, can not only quantify the internal stress for measuring film to be measured, especially high-temperature resistant membrane, Er Qieke
Substantially to shorten the testing time.So the present invention effectively overcomes various shortcoming in the prior art and has high industrial utilization
Value.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should by the present invention claim be covered.
Claims (11)
1. a kind of test method of stress in thin films, which is characterized in that include the following steps:
1) film sample to be measured is provided;And
2) film sample to be measured is heated up to preset temperature with constant heating rate, obtained to be measured thin described in temperature-rise period
The maximum contraction rate of membrane sample, to characterize the internal stress of the film sample to be measured.
2. the test method of stress in thin films according to claim 1, which is characterized in that in step 2), provide a closure
Container, and the film sample to be measured is placed in the closure container, by heating up to the closure container, so that
The film sample to be measured is warming up to the preset temperature with constant heating rate.
3. the test method of stress in thin films according to claim 2, which is characterized in that a clamping device is provided, by institute
It states the opposite both ends of the good film sample to be measured of gripping apparatus grips to be placed in the closure container, wherein described in acquisition
Film sample to be measured is along the maximum contraction rate being clamped on the line direction of both ends, to characterize the planted agent of the film sample to be measured
Power.
4. the test method of stress in thin films according to claim 3, which is characterized in that described in the gripping apparatus grips
The chucking power of film sample to be measured is between 0.005N~2N.
5. the test method of stress in thin films according to claim 2, which is characterized in that further include step in step 2):
It is passed through protective gas into the closure container, to prevent the film sample to be measured from being aoxidized.
6. the test method of stress in thin films according to claim 5, which is characterized in that the protective gas includes nitrogen
At least one of the group that gas, argon gas, helium and hydrogen are constituted;And the protection gas is passed through with the constant speed that is passed through
Body, the speed that is passed through is between 10ml/min~100ml/min.
7. the test method of stress in thin films according to claim 1, which is characterized in that described to be measured thin in step 2)
The heating rate of membrane sample is between 1 DEG C/min~60 DEG C/min.
8. the test method of stress in thin films according to claim 1, which is characterized in that in step 2), the default temperature
Degree is between 0 DEG C~600 DEG C.
9. the test method of stress in thin films according to claim 1, which is characterized in that in step 2), test and obtain
The inflection curves of film sample to be measured described in temperature-rise period, to obtain the maximum contraction rate of the film sample to be measured.
10. the test method of stress in thin films according to claim 1, which is characterized in that described to be measured thin in step 1)
The surface shape of membrane sample includes rectangle, in step 2), obtains the film sample to be measured along the rectangular length side
Upward maximum contraction rate.
11. the test method of the stress in thin films according to any one of claim 1~10, which is characterized in that described
Film sample to be measured is selected from thin polymer film, the material of the thin polymer film include polyolefin, polyamide, polyimides,
Polyester, fluorine class polyolefin, polyethylene, polypropylene, aramid fiber, non-woven fabrics, Kynoar, polytetrafluoroethylene (PTFE) and poly terephthalic acid
At least one of the group that glycol ester is constituted.
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CN109256516A (en) * | 2018-09-20 | 2019-01-22 | 上海恩捷新材料科技有限公司 | For the isolation film of electrochemical appliance, electrochemical appliance and preparation method thereof |
CN109357805A (en) * | 2018-11-26 | 2019-02-19 | 杨凌美畅新材料股份有限公司 | A kind of detection method of nickel aminosulfonic bath system internal stress |
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