CN105699167B - A kind of fexible film brittle failure method - Google Patents
A kind of fexible film brittle failure method Download PDFInfo
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- CN105699167B CN105699167B CN201610052811.5A CN201610052811A CN105699167B CN 105699167 B CN105699167 B CN 105699167B CN 201610052811 A CN201610052811 A CN 201610052811A CN 105699167 B CN105699167 B CN 105699167B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
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Abstract
The present invention relates to the field of scanning electron microscope sample preparation, in particular to a kind of fexible film brittle failure method, comprising the following steps: silicon wafer is processed into small elongated strip, obtains pre-groove silicon wafer；The pre-groove silicon wafer and fexible film are bonded；Both ends are fixed using clip, and then putting into coolant liquid is fully cooled it；It after freezing silicon wafer is taken out rapidly, while being bent to the slotted face of the freezing silicon wafer band, until freezing silicon wafer generation brittle failure, obtains the fexible film of brittle failure.While low temperature reduces fexible film toughness, this method limits mobile film, concentration transient stress by pre-groove silicon wafer is pasted and generates high strain rate, to be easier to obtain complete brittleness section, overcomes section obtained and be plastically deformed the various problems such as obvious and out-of-flatness.
Description
Technical field
The present invention relates to the field of scanning electron microscope sample preparation, in particular to a kind of fexible film brittle failure method.
Background technique
Usually need to observe the pattern in situ of fexible film section using scanning electron microscope under study for action.But fexible film
Material has thickness thin, the features such as material is soft, and intensity is higher, sample preparation it is difficult, if cut off or tear fracture if can
It is plastically deformed section, destroys the original pattern of section.Currently used method is that film is cut into small item then to impregnate
Enter in liquid nitrogen.This is because the temperature of liquid nitrogen is about -196 DEG C, organic matter can become fragile at low temperature, after sample cooling becomes fragile
Bar is clamped with two tweezers, then to bent intermediate, is broken sample, to obtain section sample.But this operation
Method has the following problems: being difficult to clamp with tweezers first is that sample is small, is also easy to lose because of avalanche after fracture；Second is that film is disconnected
Stress deformation, movement at face, stress are not concentrated, and interface out-of-flatness is caused, or generate apparent plastic deformation, or even break not
It opens；Third is that some samples still have part plasticity under liquid nitrogen temperature, complete brittle failure can not be presented.Fig. 6 is directly to SPEEK
The scanning electron microscope diagram for the sample that brittle failure obtains after proton exchange membrane progress liquid nitrogen frozen, as we can see from the figure using existing
The apparent fracture of section obtained with the presence of technology is irregular and plastic deformation.Fig. 9 is the lithium battery obtained using the prior art
The scanning electron microscope (SEM) photograph of polypropylene diaphragm, there are many microcellular structures for the material, from scanning electron microscope (SEM) photograph it can be seen that using existing
Method is readily formed closed pore.Figure 12 is the cross-section diagram of the polyethylene preservative film obtained using the prior art, can from figure
Complete plastic deformation has occurred rather than Brittle deformation to the section obtained using the prior art.
It is referred in the patent of invention application No. is 201410563142.9 a kind of for being carried out to scanning electron microscope example
The device of freeze fracture, Liquid nitrogen precooler is insufficient although this device solves existing scanning electron microscope example freeze fracture during
The problem of, but equipment is integrally huge, manufacture is complicated and complicated for operation, significantly limits the popularity of above-mentioned apparatus.?
Application No. is refer to a kind of prepare the low of scanning electron microscope sample section in the patent of invention of CN201410637248.9
Warm brittle failure device, device is huge, consumption liquid nitrogen is more, for fexible film sample especially small sample and is not suitable for.
Summary of the invention
This invention address that providing, a kind of operation is simpler, cost is cheaper, the scope of application is widely soft simultaneously
Property film brittle failure method.And this method uses the ordinary silicon chip easily obtained, conductive double sided adhesive tape and binder clip and scissors, liquid
Nitrogen, container, tweezers and the gloves for containing liquid nitrogen.
The present invention devises a kind of new fexible film brittle failure method to solve above-mentioned technical problem, this method include with
Lower step: A. processes silicon wafer, makes its one side with groove, obtains pre-groove silicon wafer；B. by the pre-groove silicon
Piece and flexible membrane bond, and compound silicon wafer are obtained, wherein not having reeded face to be connected in the flexible membrane and the pre-groove silicon wafer；
C. it is fully cooled the compound silicon wafer using coolant liquid, obtains freezing silicon wafer；D. freezing silicon wafer is separated with the freezing liquid；
E. the freezing silicon wafer two sides are fixed, while to the slotted face applied force of freezing silicon wafer band；F. to freeze silicon wafer hair
Raw brittle failure, obtains the flexible membrane of brittle failure.
As a kind of preferred embodiment: the silicon wafer Yu the fexible film of step B in the fexible film brittle failure method
It is connected by conductive double sided adhesive tape, the compound silicon wafer is sandwich structure, and wherein basecoat is silicon wafer, and intermediate one layer is conduction
Double-sided adhesive, topmost one layer is fexible film.Silicon wafer described in this method selects common single throwing silicon wafer of 0.3mm-1mm, single to throw
Silicon wafer is easy to get, and commercial thickness is generally all in 1mm hereinafter, there is easily removal etc. after the easy brittle failure of easy cutting, obtained section many
Advantage, so selecting in the present invention.The conductive double sided adhesive tape is the common carbonaceous conductive double-sided adhesive of electron microscopyc sample preparation, at low temperature
There are also very strong bonding forces, sandwich structure will not be made to disintegrate at low temperature, and do not have to removal after section is made.
As a kind of preferred embodiment:, can be by above sandwich knot if film toughness under liquid nitrogen temperature is also fine
Structure enhancing be five-layer structure, by pre-groove silicon wafer, carbonaceous conductive double-sided adhesive, macromolecule fexible film, carbonaceous conductive double-sided adhesive, silicon wafer according to
Secondary paste becomes comprehensive silicon piece, and wherein for silicon wafer in outermost layer, macromolecule fexible film occupy center, and carbonaceous conductive double-sided adhesive is centre
Layer.
As a kind of preferred embodiment: carrying out pre-embossed processing in the width direction to silicon wafer using icking tool and steel ruler in step A, carve
Slot is straight line, and occupy the center of rectangular silicon wafer.
As a kind of preferred embodiment: the silicon wafer used in the fexible film brittle failure method is strip, the silicon wafer
The ratio between length and width are greater than 2:1.Only when the length-width ratio of silicon wafer be greater than certain numerical value when just facilitate silicon wafer is clamped and is broken it is disconnected,
The too short silicon wafer structure inconvenience concentrated stress of length-width ratio.
As a kind of preferred embodiment: the size of the flexible membrane and the conductive double sided adhesive tape used in the method is little
In twice of the die size.If the width of fexible film is significantly greater than silicon wafer width, when silicon wafer brittle failure, may make soft
Property film on only silicon wafer be overlapped part occur brittle fracture, and the part wider than silicon wafer then without be broken or occur plasticity
Fracture.But if the size that the size of fexible film is less than silicon wafer is then possible.
Improvement as this method: coolant liquid used in step C is liquid nitrogen.The boiling point of liquid nitrogen under normal pressure is -196
DEG C, inertia is non-combustible, is easy to obtain, is the typical media of freezing.
As a kind of preferred embodiment: clamping silicon wafer sandwich structure in step C using clip.Clip preferentially selects herein
Use binder clip.Binder clip can clamp compound silicon wafer, while its handle is also convenient for pulling out from freezing liquid, can also make when breaking disconnected
For force part.It should be noted that the size of binder clip should be selected according to silicon wafer size, two sides binder clip should be close to silicon
It piece cutting and is arranged symmetrically.It is that a long rope is convenient on the handle of one end binder clip to pull out from liquid nitrogen.
As a kind of preferred embodiment: the time that compound silicon wafer immerses liquid nitrogen in step C is greater than 60 seconds to guarantee to be fully cooled.
Time enough will not be plastically deformed with ensuring that fexible film is completely brittle.
As a kind of preferred embodiment: using the fixed compound silicon wafer of clip in step C.The wherein preferred binder clip of clip.
As a kind of preferred embodiment: silicon wafer and freezing liquid will be freezed by clamping the long tail clip handle using tweezers in step D
Separation, can also directly extract in long tail clip handle end tether.
As a kind of preferred embodiment: fixing the two of the freezing silicon wafer respectively using the both hands with moisture retentive glove in step E
The clip handle at end is simultaneously bent.
Mechanism of the invention mainly has at 3 points.First, silicon wafer and conductive double sided adhesive tape limit thin in total stress
The movement of film, so that the tensile stress and strain inside film can only be along silicon wafer in-planes.Second, silicon wafer is exactly originally brittleness
Material, and because there is a cutting is broken first when stress at cutting, with the brittle failure of silicon wafer, the tensile stress undertaken originally by silicon wafer,
Moment is transferred on fexible film, and the tensile stress uprushed is considered as the Transient optical signal that film receives, it is assumed that the Transient optical signal is
Rectangular pulse is gained knowledge by structural dynamic it is recognised that the function and effect of Transient optical signal can achieve the 2 of identical numerical value dead load
Times.Third, because there is the presence of pre-groove, so that the moment stress of silicon wafer brittle failure all focuses among film at former silicon wafer cutting
Position.
In short, the tensile stress uprushed can regard impact load as, function and effect are much larger than dead load, even magnitude
Variation；Because being transient state pulling force, strain rate is improved, under high strain-rate, material is easier to that brittle break occurs；In silicon
The pre-embossed scratch of on piece greatly enhances fexible film and sends out along " indentation " direction so that the pulling force uprushed has apparent directionality
A possibility that raw brittle fracture.These factors all accelerate the fracture of fexible film, and generate very big instantaneous strain rate, and big
Strain rate can make material generate brittle deformation.Although so operation of the invention is simple, but good effect can be obtained.
Make fexible film that brittle failure occur using this method, has the advantage that firstly, silicon wafer is relatively flat, and can do
Ratio film it is big, facilitate manual operation, overcome and prepare that sample in electron microscopyc sample preparation is small to be difficult to the problem of clamping with tweezers；And it commonly uses
Method because fracture when section unbalance stress and cause section not smooth enough, but in this method silicon wafer because have in advance
Groove, fracture is relatively straight and the time of fracture is very of short duration, in the moment of silicon wafer fracture, neighbouring film by bonding it is mobile by
Limit, pre-groove region are broken to keep section smooth by the transient stress and high strain rate concentrated, overcome obtained
Section out-of-flatness the problem of can also overcome some samples under liquid nitrogen temperature or have certain toughness, it is different surely crisp
Disconnected problem.
Detailed description of the invention
Fig. 1 is provided in an embodiment of the present invention by pre-embossed silicon wafer schematic diagram.
Fig. 2 is the sandwich structure schematic diagram of compound silicon wafer provided in an embodiment of the present invention.
Fig. 3 is the schematic diagram of the compound silicon wafer of the fixed sandwich structure of binder clip.
Fig. 4 is the stress diagram of compound silicon wafer provided in an embodiment of the present invention.
Fig. 5 is the compound silicon wafer schematic diagram after generation brittle failure provided in an embodiment of the present invention.
Fig. 6 is that the section SEM of the flexible SPEEK film obtained using commonsense method is schemed.
Fig. 7 is the SEM figure of the section of the flexible SPEEK film obtained using the specific embodiment of the invention.
Fig. 8 is that the SEM of the section of the lithium battery diaphragm obtained using present invention specific implementation is schemed.
Fig. 9 is that the SEM of the section of the lithium battery diaphragm obtained using commonsense method is schemed.
Figure 10 is that the SEM of the section of the polyethylene preservative film obtained using present invention specific implementation is schemed.
Figure 11 is that the SEM of the polyethylene preservative film section obtained using commonsense method is schemed.
Figure 12 is that the SEM of the section of the small sulfonation SPEEK film obtained using present invention specific implementation is schemed.
Specific embodiment
The following detailed description of specific embodiments of the present invention.
Implement 1
For preparing the macromolecule fexible film brittle failure face for scanning electron microscope, fexible film is SPEEK matter
Proton exchange.
Firstly, silicon wafer long 1.5cm, wide 5mm, length-width ratio are far longer than as shown in Figure 1, preparing the silicon wafer of a strip
2:1 meets restrictive condition, and then the side glass cutter among silicon wafer strip is pre-embossed, obtains an one side with fluted
Silicon wafer.
It is ready for fexible film, macromolecule fexible film is cut into the long 1cm of strip silicon wafer slightly smaller dimension, it is wide
3mm。
Third step, as shown in Fig. 2, macromolecule fexible film, carbonaceous conductive double-sided adhesive, silicon wafer are successively pasted into sandwich knot
Structure becomes compound silicon wafer, wherein silicon wafer be lowest level, and with it is reeded down, carbonaceous conductive double-sided adhesive be middle layer, high score
Sub- fexible film is most upper one layer, and then both ends as shown in Figure 3 are fixed with binder clip, can be at the handle of one of binder clip
It is a rope.
Compound silicon wafer is put into liquid nitrogen and is submerged by the 4th step, is placed about two minutes, is fully cooled, is freezed to it
Silicon wafer.
5th step, lifting rope take out sample, and both hands wear gloves and hold the binder clips of two sides to the face for having pre-groove
Force, to its brittle failure.Fig. 4 is seen in specific direction.
Fig. 7 is shown in the profile scanning electron microscope using flexible membrane brittle failure method flexible membrane obtained provided by the invention
Generation brittle failure macromolecule fexible film section, it is seen that section exposes the particulate inclusions of itself without obvious plastic deformation.
Fig. 6 is seen using commonsense method, there are problems that plastic deformation and out-of-flatness.
Implement 2
By prepare for scanning electron microscope macromolecule fexible film brittle failure face for, fexible film be lithium battery every
Film, material are polypropylene, and there are many microcellular structures, commonsense method is readily formed closed pore.
Firstly, as shown in Figure 1, preparing the silicon wafer of a strip, silicon wafer long 1.5cm, wide 5mm, then in silicon wafer strip
Intermediate side glass cutter is pre-embossed, obtains an one side with reeded silicon wafer.
It is ready for fexible film, macromolecule fexible film is cut into the long 1cm of the similar size of strip silicon wafer, it is wide
3mm。
Third step, as shown in Fig. 2, macromolecule fexible film, carbonaceous conductive double-sided adhesive, silicon wafer are successively pasted into sandwich knot
Structure becomes compound silicon wafer, wherein silicon wafer be lowest level, and with it is reeded down, carbonaceous conductive double-sided adhesive be middle layer, high score
Sub- fexible film is most upper one layer, and then both ends are fixed with binder clip, can be a rope at the handle of one of binder clip
Son.
Compound silicon wafer is put into liquid nitrogen and is submerged by the 4th step, is placed about two minutes, is fully cooled, is freezed to it
Silicon wafer.
5th step, lifting rope take out sample, and both hands wear gloves and hold the binder clips of two sides to the face for having pre-groove
Force, to its brittle failure.Fig. 4 is seen in specific direction.
Fig. 8 is the profile scanning electron microscope using flexible membrane brittle failure method flexible membrane obtained provided by the invention.From
As can be seen that the intact preservation of porous structure of flexible membrane section, has with the flexible membrane section for using the prior art to obtain in figure
It is dramatically different.
Implement 3
For preparing the macromolecule fexible film brittle failure face for scanning electron microscope, fexible film is polyethylene guarantor
Fresh film, material are polypropylene, than more flexible under low temperature.
Firstly, as shown in Figure 1, preparing the silicon wafer of a strip, silicon wafer long 1.5cm, wide 5mm, then in silicon wafer strip
Intermediate side glass cutter is pre-embossed, obtains an one side with reeded silicon wafer.
It is ready for fexible film, macromolecule fexible film is cut into the size similar with strip silicon wafer, long 1cm is wide
3mm。
Third step, because polyethylene preservative film toughness under liquid nitrogen temperature is also fine, by above sandwich structure
Enhancing, pre-groove silicon wafer, carbonaceous conductive double-sided adhesive, macromolecule fexible film, carbonaceous conductive double-sided adhesive, silicon wafer, which are successively pasted, becomes multiple
Silicon wafer is closed, wherein for silicon wafer in outermost layer, macromolecule fexible film occupy center, and carbonaceous conductive double-sided adhesive is middle layer.Then both ends
It is fixed with binder clip, can be a rope at the handle of one of binder clip.
Compound silicon wafer is put into liquid nitrogen and is submerged by the 4th step, is placed about two minutes, is fully cooled, is freezed to it
Silicon wafer.
5th step, lifting rope take out sample, and both hands wear gloves and hold the binder clips of two sides to the face for having pre-groove
Force, to its brittle failure.Specific direction refers to Fig. 4.
Figure 10 is the profile scanning electron microscope using flexible membrane brittle failure method flexible membrane obtained provided by the invention.It can
To see that flexible membrane section almost complete absence of being plastically deformed, has very big difference with Figure 11.
Implement 4
For preparing the macromolecule fexible film brittle failure face for scanning electron microscope, fexible film is sulfonation
SPEEK proton exchange membrane, size is very small, and long only have 5mm, wide only 3mm, commonsense method at all can not brittle failure, because of tweezers
It can't clip and also do not apply power.
Firstly, as shown in Figure 1, preparing the silicon wafer of a strip, silicon wafer long 1cm, wide 5mm, then in silicon wafer strip
Between side glass cutter it is pre-embossed, obtain an one side with reeded silicon wafer.
Third step, as shown in Fig. 2, macromolecule fexible film, carbonaceous conductive double-sided adhesive, silicon wafer are successively pasted into sandwich knot
Structure becomes compound silicon wafer, wherein silicon wafer be lowest level, and with it is reeded down, carbonaceous conductive double-sided adhesive be middle layer, high score
Sub- fexible film is most upper one layer, and then both ends are fixed with binder clip, can be a rope at the handle of one of binder clip
Son.
Compound silicon wafer is put into liquid nitrogen and is submerged by the 4th step, is placed about two minutes, is fully cooled, is freezed to it
Silicon wafer.
5th step, lifting rope take out sample, and both hands wear gloves and hold the binder clips of two sides to the face for having pre-groove
Force, to its brittle failure.Fig. 4 is seen in specific direction.
Then the macromolecule fexible film section of generation brittle failure as shown in figure 12 can be obtained.It can be seen that although should
The very small unsuitable manpower of flexible membrane directly operates, but uses the still available preferable brittleness of method provided by the invention
The plane of disruption.
In summary it from the point of view of embodiment, compared with the brittle failure face directly obtained using liquid nitrogen frozen, is obtained using this method
The section of the fexible film arrived is more neat, is not plastically deformed, and is especially advantageous for the primary section shape of observation fexible film
State.
Three problems mentioned before fexible film brittle failure section overcomes are obtained using method provided by the invention, the
One: if sample is very small, it is only necessary to the area of silicon wafer be increased and conveniently manually operated, overcome and prepare in electron microscopyc sample preparation
Sample is small to be difficult to the problem of clamping with tweezers, and sample both ends are fixed the also taking-up of very convenient sample with binder clip and broken disconnected.The
Two: and section unbalance stress when commonly method is because of fracture, it may be uneven, but silicon wafer is preparatory because of having in this method
Groove, fracture when is broken suddenly, and neighbouring film stress is big and concentrates, and relatively easily causes smooth section, overcomes system
The problem of section out-of-flatness obtained.Third: although fexible film it is general at low temperature all compared with than under normal temperature condition more under it is crisp,
There are also certain toughness under liquid nitrogen temperature for many samples, and use fexible film brittle failure method provided by the invention, when stress
Limit the limitation that the movement of fexible film has received conductive double sided adhesive tape and silicon wafer, silicon chip stress concentrates moment fracture along cutting
Power is set to concentrate on the film near cutting, film is concentrated herein and biggish action of pulling stress is broken rapidly, can be obtained more preferable
Brittle fracture effect.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, such as is prepared and transmitted using this method
Electron microscope or the sample of atomic force microscope all shall be regarded as belonging to protection scope of the present invention.
Claims (9)
1. a kind of fexible film brittle failure method, it is characterised in that: method includes the following steps:
A. silicon wafer is processed, makes its one side with groove, obtains pre-groove silicon wafer；
B. the pre-groove silicon wafer and fexible film are bonded, obtains compound silicon wafer, wherein the fexible film and the pre-groove
Do not have reeded face to be connected in silicon wafer, the pre-groove silicon wafer is connected with the fexible film by conductive double sided adhesive tape, described multiple
Conjunction silicon wafer is sandwich structure, and wherein basecoat is pre-groove silicon wafer, and intermediate one layer is conductive two-sided
Glue, topmost one layer is fexible film；
C. it is fully cooled the compound silicon wafer using coolant liquid, obtains freezing silicon wafer；
D. freezing silicon wafer is separated with the coolant liquid；
E. the freezing silicon wafer two sides are fixed, while to the slotted face applied force of freezing silicon wafer band；
F. to freeze silicon wafer generation brittle failure, obtain the fexible film of brittle failure.
2. fexible film brittle failure method according to claim 1, it is characterised in that: use icking tool and steel ruler pair in step A
Silicon wafer is processed.
3. fexible film brittle failure method according to claim 1, it is characterised in that: used in the fexible film brittle failure method
The silicon wafer arrived is strip, and the ratio between the length of the silicon wafer and width are greater than 2:1.
4. fexible film brittle failure method according to claim 3, it is characterised in that: used in the fexible film brittle failure method
The size of the fexible film and the conductive double sided adhesive tape that arrive is not more than twice of the die size.
5. fexible film brittle failure method according to claim 1, it is characterised in that: in step C, compound silicon wafer immerses liquid nitrogen
Time be greater than 60 seconds.
6. fexible film brittle failure method according to claim 1, it is characterised in that: using described in clip fixation in step C
Compound silicon wafer.
7. fexible film brittle failure method according to claim 6, it is characterised in that: clamped in step D using tweezers described
Clip handle will freeze silicon wafer and separate with coolant liquid, or in clip handle end tether, directly extract.
8. fexible film brittle failure method according to claim 7, it is characterised in that: using with moisture retentive glove in step E
Both hands are fixed the clip handle at the both ends of the freezing silicon wafer respectively and are bent.
9. fexible film brittle failure method according to claim 1, it is characterised in that: coolant liquid used in step C is liquid
Nitrogen.
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| WO2018000350A1 (en) * | 2016-06-30 | 2018-01-04 | 周肇梅 | Method for fracturing fixable film |
| CN106814095B (en) * | 2017-02-12 | 2019-05-24 | 马新军 | Freezing sample preparation device for scanning electron microscope |
| CN106848109A (en) * | 2017-02-14 | 2017-06-13 | 武汉华星光电技术有限公司 | The cutting method of display pannel |
| CN108480922B (en) * | 2018-03-13 | 2020-05-19 | 广东长盈精密技术有限公司 | Flexible substrate and processing method and system thereof |
| CN109580635B (en) * | 2018-12-03 | 2021-05-18 | 高佳太阳能股份有限公司 | Method for rapidly determining reason for uneven thickness of diamond-cut silicon wafer |
| CN109752400B (en) * | 2018-12-26 | 2022-06-07 | 上海神力科技有限公司 | Method for processing characterization sample of membrane electrode interface structure of fuel cell |
| CN113533402A (en) * | 2021-07-14 | 2021-10-22 | 北京市理化分析测试中心 | Film coating brittle fracture method |
| CN118111788A (en) * | 2024-04-28 | 2024-05-31 | 武汉理工大学三亚科教创新园 | Freezing brittle fracture method of high-toughness porous material |
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| CN102128751A (en) * | 2010-12-17 | 2011-07-20 | 上海工程技术大学 | Method for researching fracture performance of metal film |
| CN103013024B (en) * | 2012-12-10 | 2014-07-09 | 厦门大学 | Styrene segmented copolymer membrane and preparation method thereof |
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| CN104316730B (en) * | 2014-11-05 | 2017-01-18 | 中国科学院生态环境研究中心 | Low-temperature brittle failure device for manufacturing scanning electron microscope sample section |
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