KR20170002068A - A manufacturing method of polymer test sample for x-ray 3d imaging analysis - Google Patents
A manufacturing method of polymer test sample for x-ray 3d imaging analysis Download PDFInfo
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- KR20170002068A KR20170002068A KR1020150091978A KR20150091978A KR20170002068A KR 20170002068 A KR20170002068 A KR 20170002068A KR 1020150091978 A KR1020150091978 A KR 1020150091978A KR 20150091978 A KR20150091978 A KR 20150091978A KR 20170002068 A KR20170002068 A KR 20170002068A
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- polymer
- ray
- sample
- test sample
- filler
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
- G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
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- 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; rubber; leather
- G01N33/442—Resins, plastics
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/40—Imaging
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/623—Specific applications or type of materials plastics
Abstract
Description
The present invention relates to a method for producing a polymer sample for X-ray 3D image analysis.
When various polymers are prepared, it is common to incorporate an internal filler such as silica in order to improve the physical properties of the polymer itself.
A transmission electron microscope (TEM) has been widely used as a technique for analyzing the filler in the polymer. In order to observe the structure of a particle by a transmission electron microscope, it is generally necessary to prepare a very thin sample slice (thin slice) to such a degree that the electron beam can penetrate. The thickness of the slice is usually about 100 nm to 300 nm though it depends on the performance of the transmission electron microscope , The filler distributed in the polymer can be confirmed only in the local region.
In this regard, in Japanese Patent Application Laid-Open No. 2005-326211, a thin piece placed on a support is heated under a reduced pressure or under an atmosphere of nitrogen gas or inert gas to volatilize the polymer material portion in the thin section. Although a method for preparing a sample for an electron microscope has been disclosed, there is still a drawback in that the distribution of the filler distributed in the polymer can be confirmed over a wider area and the quantitative analysis can not be performed.
It is an object of the present invention to provide a polymer sample preparation method for observing the distribution state of a filler in a polymer by using an X-ray 3D image apparatus.
It is another object of the present invention to provide a method for analyzing the distribution of a filler in a polymer including the method for producing a polymer sample.
The present invention relates to: 1) a step of cutting a part of a sample of a polymer material with a cryo-microtome to form a polymer scaffold;
2) a step of cutting a part of the sample of the polymer material with a freezing section to make a polymer piece; And
3) placing the polymeric particles on top of the polymer scaffold
And a method for producing a polymer sample for X-ray 3D image analysis.
The present invention also provides a method for analyzing the distribution of a filler in a polymer, which comprises a method of producing a polymer sample for X-ray 3D image analysis.
According to the polymer sample preparation method of the present invention, a sample having a size of 20 탆 3 or more can be prepared in accordance with conditions, a sample can be produced in a short time, and it is simple and economical. The glass transition temperature (Tg) There is an advantage that it can be adjusted.
1 is a schematic view of a method for producing a polymer sample of the present invention.
2 is a front view of the polymer sample prepared in Example 1 by an optical microscope.
3 is a side view of the polymer sample prepared in Example 1 by optical microscope.
FIG. 4 is a photograph of the filler (silica) in the polymer sample prepared in Example 1, analyzed by an X-ray 3D image apparatus. FIG.
Fig. 5 is a photograph of the polymer (silica) in the polymer sample prepared in Example 2, analyzed by an X-ray 3D image apparatus. Fig.
The present invention relates to: 1) a step of cutting a part of a polymer with a cryo-microtome to form a polymer scaffold;
2) cutting a part of the polymer with a freezing section to make a polymer piece; And
3) placing the polymeric particles on top of the polymer scaffold
To a method for producing a polymer sample for X-ray 3D image analysis.
The polymer is not limited as long as it contains a filler.
The X-ray 3D image analysis polymer sample is for monitoring the distribution state of the filler in the polymer, preferably the distribution of the filler aggregate in the polymer, but is not limited thereto.
In the present invention, in order to obtain good resolution using an X-ray 3D imaging apparatus, it is preferable that the size of the sample is not less than 20 탆 3 , preferably not less than 30 탆 3 .
However, the method using a conventional focused ion beam devices (FIB) is a long time to produce a sample of the polymer material too long, 10 ㎛ 3 There was a disadvantage that only the following samples could be produced.
Therefore, in the present invention, a sample of a polymer material is made hard at a low temperature by using a freezing section, and then a desired size of 30 탆 3 The sample slice could be prepared. However, if a frozen section is used to produce a sample slice of a size, the slice of the sample is thin and it is difficult to control the thickness.
Therefore, in the present invention, a sample having a large size of about 100 탆 x 100 탆 x 60 탆 was first prepared, and a piece having a size of about 30 탆 30 탆 30 탆 was formed thereon.
That is, the size of the polymer scaffold should be large enough to support the polymer scaffold, and the size of the polymer scaffold is preferably larger than that of the polymer scaffold.
The distribution of the filler in the polymer can be clearly observed with the X-ray 3D image device in a stable state by using the polymer sample manufactured by the polymer sample preparation method as described above.
The following advantages are obtained by preparing a sample according to the polymer sample preparation method provided by the present invention.
Conventional focused ion beam devices (FIB) roneun and possible pieces produced in less than 10 ㎛ 1 primary particle (primary particle) to be observed, but the required production time is 24 hours or more inconvenience, pieces of more than 20 ㎛ 3 Size There is a disadvantage in that accuracy can not be made.
However, when a polymer sample is prepared according to the present invention, it is possible to manufacture a sample size from 30 μm 3 or more to one hour or less, so that the filler aggregate distribution state of several hundreds of nano size can be easily .
In addition, it is possible to control the glass transition temperature (Tg) suitable for the polymer sample, and thus it is possible to produce various kinds of polymer samples having different glass transition temperatures.
The present invention relates to a method for analyzing the distribution of a filler in a polymer, which comprises a method for producing a polymer sample for X-ray 3D image analysis.
The present invention also relates to a method for analyzing the distribution of a filler in a polymer, which comprises observing the polymer sample for X-ray 3D image analysis with an X-ray 3D image apparatus.
Hereinafter, the present invention will be described in more detail by way of non-limiting examples. The embodiments of the present invention described below are by way of example only and the scope of the present invention is not limited to these embodiments. The scope of the present invention is indicated in the claims, and moreover, includes all changes within the meaning and range of equivalency of the claims. In the following Examples and Comparative Examples, "%" and "part" representing the content are on a mass basis unless otherwise specified.
Example
Example 1. Polymer sample preparation for X-ray 3D image analysis
1) Unmodified solution A part of the styrene butadiene rubber (SSBR) was cut with a freezing section (Cryo-microtome, EM FC7, manufactured by Lecia) to prepare a polymer scaffold.
2) A sample of the polymer material was cut with a freezing section to make a polymer sculpture.
3) A polymer sample for X-ray 3D image analysis was prepared by placing the polymer particles on top of the polymer scaffold.
4) The prepared polymer sample was observed with an optical microscope, and the result is shown in FIG.
Example 2. Polymer sample preparation for X-ray 3D image analysis
A polymer sample was prepared in the same manner as in Example 1, except that the modified solution styrene butadiene rubber (SSBR) was used instead of the unmodified solution styrene butadiene rubber (SSBR) in Example 1, 1). The prepared polymer sample was observed with an optical microscope, and the result is shown in FIG.
Application example 1. Analysis of distribution of polymer filler using X-ray 3D image analyzer
The polymer samples prepared in Examples 1 and 2 were observed with a X-ray 3D imaging apparatus (Pohang Accelerator Laboratory, Beamline: 7C-X-ray nanoimage (XNI)) to analyze the distribution of the polymer filler. The results of the analysis are shown in Fig. 4 (Example 1) and Fig. 5 (Example 2).
Claims (7)
2) cutting a part of the polymer with a freezing section to make a polymer piece; And
3) placing the polymeric particles on top of the polymer scaffold
A method for preparing a polymer sample for X-ray 3D image analysis.
Wherein the polymer comprises a filler. ≪ RTI ID = 0.0 > 11. < / RTI >
Wherein the polymer sample for X-ray 3D image analysis is for observing the distribution of the filler in the polymer.
Wherein the polymer sample for X-ray 3D image analysis is for observing distribution of a filler aggregate in a polymer.
Wherein the polymer sculpture has a size of at least 20 mu m < 3 & gt ;.
Wherein the size of the polymer scaffold is larger than the size of the polymer scaffold.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020150091978A KR20170002068A (en) | 2015-06-29 | 2015-06-29 | A manufacturing method of polymer test sample for x-ray 3d imaging analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| KR1020150091978A KR20170002068A (en) | 2015-06-29 | 2015-06-29 | A manufacturing method of polymer test sample for x-ray 3d imaging analysis |
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| Publication Number | Publication Date |
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| KR20170002068A true KR20170002068A (en) | 2017-01-06 |
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| KR1020150091978A KR20170002068A (en) | 2015-06-29 | 2015-06-29 | A manufacturing method of polymer test sample for x-ray 3d imaging analysis |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005326211A (en) | 2004-05-13 | 2005-11-24 | Bridgestone Corp | Sample preparation method |
-
2015
- 2015-06-29 KR KR1020150091978A patent/KR20170002068A/en not_active Application Discontinuation
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005326211A (en) | 2004-05-13 | 2005-11-24 | Bridgestone Corp | Sample preparation method |
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