KR100763732B1 - Sample preparation method of a multi-layer polyolefin film for oveservation using scanning electron microscope - Google Patents
Sample preparation method of a multi-layer polyolefin film for oveservation using scanning electron microscope Download PDFInfo
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- KR100763732B1 KR100763732B1 KR1020000054452A KR20000054452A KR100763732B1 KR 100763732 B1 KR100763732 B1 KR 100763732B1 KR 1020000054452 A KR1020000054452 A KR 1020000054452A KR 20000054452 A KR20000054452 A KR 20000054452A KR 100763732 B1 KR100763732 B1 KR 100763732B1
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- polyolefin
- multilayer film
- acid
- based multilayer
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- 229920000098 polyolefin Polymers 0.000 title claims abstract description 30
- 238000005464 sample preparation method Methods 0.000 title 1
- 238000000034 method Methods 0.000 claims abstract description 26
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims abstract description 9
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003672 processing method Methods 0.000 claims abstract description 5
- 238000005530 etching Methods 0.000 claims description 21
- 238000004626 scanning electron microscopy Methods 0.000 claims description 2
- 239000010410 layer Substances 0.000 abstract description 12
- 238000000926 separation method Methods 0.000 abstract description 5
- 238000004458 analytical method Methods 0.000 abstract description 4
- 239000011229 interlayer Substances 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 33
- 239000000243 solution Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 10
- 239000004743 Polypropylene Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- -1 polypropylene Polymers 0.000 description 5
- 229920001155 polypropylene Polymers 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 238000005266 casting Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000005025 cast polypropylene Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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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
- G01N1/32—Polishing; Etching
-
- 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
- G01N1/2853—Shadowing samples
-
- 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
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
Abstract
본 발명은 폴리올레핀계 다층필름의 주사전자현미경 관찰을 위한 시료 처리방법에 관한 것으로, 보다 상세하게는 액체질소로 파단된 폴리올레핀계 다층필름을 a) 과망간산 또는 크롬산과 b) 인산 및 황산 중 하나 이상인 것으로 이루어지는 용액에 함침시켜 에칭시킨 후, 필름에 남아있는 잔류물을 제거하는 과정을 포함하는 폴리올레핀계 다층필름의 처리방법에 관한 것이다. 본 발명에 의해 폴리올레핀계 다층필름의 층간분리를 명확하게 하여 폴리올레핀계 다층필름의 분석 및 이를 이용한 새로운 용도의 폴리올레핀계 다층필름의 개발을 용이하게 할 수 있다.The present invention relates to a sample processing method for observing a scanning electron microscope of a polyolefin-based multilayer film, and more particularly, to a polyolefin-based multilayer film broken with liquid nitrogen to be at least one of a) permanganic acid or chromic acid and b) phosphoric acid and sulfuric acid. The present invention relates to a method for treating a polyolefin-based multilayer film, which includes a process of removing residues remaining on a film after being immersed in an aqueous solution. According to the present invention, it is possible to clarify the interlayer separation of the polyolefin-based multilayer film, thereby facilitating the analysis of the polyolefin-based multilayer film and the development of the polyolefin-based multilayer film for new use using the same.
폴리올레핀계 다층필름, 층간분리, 전자주사현미경, 시료처리방법Polyolefin multi-layer film, interlayer separation, electron scanning microscope, sample processing method
Description
도 1은 폴리올레핀계 다층 필름의 단층분석 방법을 나타낸 순서도,1 is a flow chart showing a tomographic analysis method of a polyolefin-based multilayer film,
도 2는 비교예 1에 의한 캐스팅 폴리프로필렌 필름의 단면 촬영사진, 및2 is a cross-sectional photograph of the cast polypropylene film according to Comparative Example 1, and
도 3은 실시예 1에 의한 캐스팅 폴리프로필렌 필름의 단면 촬영사진이다.
3 is a cross-sectional photograph of the cast polypropylene film according to Example 1.
본 발명은 주사전자현미경 관찰을 위한 폴리올레핀계 다층필름의 처리방법에 관한 것으로, 보다 상세하게는, 액체질소로 파단된 폴리올레핀계 다층필름을 a) 과망간산 또는 크롬산과 b) 인산 및 황산 중 하나 이상인 것으로 이루어지는 용액에 함침시켜 에칭시킨 후, 필름에 남아있는 잔류물을 제거하는 과정을 포함하는 폴리올레핀계 다층필름의 처리방법에 관한 것이다.The present invention relates to a method for treating a polyolefin-based multilayer film for scanning electron microscopy, and more particularly, to a polyolefin-based multilayer film broken with liquid nitrogen, wherein at least one of a) permanganic acid or chromic acid and b) phosphoric acid and sulfuric acid. The present invention relates to a method for treating a polyolefin-based multilayer film, which includes a process of removing residues remaining on a film after being immersed in an aqueous solution.
전자현미경을 이용한 형태(morphology) 관찰은 시료의 입체적인 정보와 이를 통한 시료의 제조 조건, 특성 등 시료에 대한 많은 정보를 제공하는데, 이때 적절한 시료의 전처리과정을 도입하여 보다 다양하고, 재연성 있는 정보를 얻을 수 있다. 주사전자현미경(Scanning Electron Microscope, SEM)측정에 이용되고 있는 시료의 준비방법은 직접분석이나 간단한 처리에서부터 시간이 많이 소요되는 복잡한 방법에 이르기까지 여러가지 방법이 있다. 구체적으로는 충격시편에 의한 파단면 관찰이나 액체질소를 이용한 저온절단법 등 간단한 방법에서 부터 초박막, 절단, 파쇄, 몰딩 등의 방법을 사용하고 있다. 특히 수십 ㎛의 얇은 고분자 필름의 단면 관찰에는 주로 액체질소를 이용한 저온절단법을 사용하고 있다. 관찰효과를 높이기 위해서 측정시에는 기울임(tilting) 기법을 이용하여 필름 단면에서 나타나는 면 효과(edge effect)와 표면효과를 제거하는 기법 등을 사용하고 있다. 이러한 과정을 통하여 필름의 두께, 층조성 등 고분자 시료의 특성에 관한 정보를 얻을 수 있다.The observation of morphology using an electron microscope provides a lot of information about the sample such as three-dimensional information of the sample and the manufacturing conditions and characteristics of the sample.In this case, a variety of reproducible information can be obtained by introducing an appropriate sample pretreatment process. You can get it. There are various methods for preparing samples used for scanning electron microscope (SEM) ranging from direct analysis or simple processing to time-consuming complex methods. Specifically, methods such as ultra-thin film, cutting, crushing, molding, etc. are used from simple methods such as observing the fracture surface by impact specimen or low temperature cutting method using liquid nitrogen. In particular, low temperature cutting using liquid nitrogen is mainly used for sectional observation of thin polymer films of several tens of micrometers. In order to enhance the observation effect, the edge effect and the surface effect which are removed from the cross section of the film are used by the tilting technique. Through this process it is possible to obtain information about the characteristics of the polymer sample, such as film thickness, layer composition.
그러나 폴리프로필렌 캐스팅필름과 폴리프로필렌 이축연신필름 등과 같이 각 층이 유사한 조성을 갖는 폴리올레핀계 다층 필름의 단면을 관찰할 때에는 액체질소를 이용한 직접절단 관찰방법만으로는 한개의 층으로 이루어진 필름처럼 관찰되어 각 조성층을 구분하여 판단하기가 쉽지않다. 따라서 유사한 조성을 가지는 폴리올레핀계 다층 필름을 관찰하기 위해서 관찰전 시료에 적당한 화학약품이나 기기를 적용하여 층간분리를 명확하게 하는 등의 시료전처리 방법의 개발이 요청된다.
However, when observing the cross section of a polyolefin-based multilayer film having a similar composition, such as a polypropylene casting film and a polypropylene biaxially oriented film, it is observed as a film composed of one layer only by the direct cutting observation method using liquid nitrogen. It is not easy to judge by classifying. Therefore, in order to observe a polyolefin-based multilayer film having a similar composition, development of a sample pretreatment method such as clarifying the separation between layers by applying a suitable chemical or device to the sample before observation is required.
이에 본 발명자는 상기와 같은 문제를 해결하기 위하여 물리적으로 결합된 폴리올레핀계 다층필름의 층을 교란하여 분리해 내는 역활을 하는 적절한 화학약품과 처리조건을 찾아내어 이를 폴리올레핀계 다층필름의 단면분석에 적용하였다.In order to solve the above problems, the present inventors have found appropriate chemicals and treatment conditions that serve to separate and separate layers of physically bonded polyolefin multilayer films and apply them to cross-sectional analysis of polyolefin multilayer films. It was.
즉 본 발명은 주사전자현미경 관찰을 위한 시료 처리방법에 있어서, 액체질소로 파단된 폴리올레핀계 다층필름을 a) 과망간산 또는 크롬산과 b) 인산 및 황산 중 하나 이상인 것으로 이루어지는 용액에 함침하여 에칭시킨 후, 필름에 남아있는 잔류물을 제거하는 과정을 포함하는 폴리올레핀계 다층필름의 처리방법을 제공함을 그 목적으로 한다.That is, in the sample processing method for scanning electron microscope observation, the polyolefin-based multilayer film broken with liquid nitrogen is impregnated and etched in a solution consisting of at least one of a) permanganic acid or chromic acid and b) phosphoric acid and sulfuric acid, It is an object of the present invention to provide a method for treating a polyolefin-based multilayer film including a process of removing residues remaining on a film.
이하에서 본 발명을 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.
도 1은 본 발명의 폴리올레핀 다층필름의 처리방법을 포함하는 다층필름의 시료 전처리 과정을 나타낸 순서도이다. 1 is a flowchart showing a sample pretreatment process of a multilayer film including a method for treating a polyolefin multilayer film of the present invention.
먼저 폴리올레핀계 다층필름을 액체질소 등을 사용하여 파단시킨다.(S1)First, the polyolefin-based multilayer film is broken using liquid nitrogen or the like. (S1)
다음으로 파단된 폴리올레핀계 다층 필름을 에칭용액에 담구어 에칭을 수행한다. 이때 상기에서 언급된 바와 같이 시료의 종류에 따라 과망간산이나 크롬산과 황산 및/또는 인산용액의 조성비를 조절하거나 에칭온도를 20∼50℃사이 이내에서, 또한 에칭시간을 20분에서 120분 사이 이내에서 조절하여 층분리효과를 높일 수 있다. (S2) Next, the broken polyolefin-based multilayer film is immersed in an etching solution to perform etching. At this time, as mentioned above, the composition ratio of permanganic acid, chromic acid, sulfuric acid, and / or phosphoric acid solution is adjusted according to the type of sample, the etching temperature is within 20 to 50 ° C, and the etching time is within 20 to 120 minutes. By adjusting the layer separation effect can be enhanced. (S2)
에칭 후 시료의 에칭용액 등에 의한 오염을 제거하는 과정이 필요하다. 시료의 세척은 다음과 같은 과정을 통하여 이루어질 수 있다. 에칭된 시료를 증류수로 1∼2회 씻어낸 후 과망간산, 크롬산 등의 잔류물을 제거하기 위해서 과산화수소수에 1∼2분간 담구어 둔다. 다음 증류수로 다시 씻어낸 후, 울트라소니케이터를 이용하여 아세톤 혹은 알콜 용액하에서 30∼60분 정도 세척하여 잔류물을 제거한다.(S3)After etching, a process of removing contamination by the etching solution of the sample is necessary. The washing of the sample may be performed through the following procedure. The etched sample is washed once or twice with distilled water and soaked in hydrogen peroxide for 1-2 minutes to remove residues such as permanganic acid and chromic acid. After washing again with distilled water, using an ultrasonicator to remove the residue by washing for 30 to 60 minutes in acetone or alcohol solution. (S3)
상기와 같이 처리된 시료의 단면은 진공상태 하에서 도전성 코팅을 수행한 후 전자현미경으로 관찰할 수 있다.(S4)
The cross section of the sample treated as above can be observed by electron microscopy after conducting the conductive coating under vacuum. (S4)
본 발명에서는 액체질소로 파단된 폴리올레핀계 다층필름을 먼저 a) 과망간산 또는 크롬산과 b) 인산 및 황산 중 하나 이상인 것으로 이루어지는 용액에 함침하여 에칭시켜서 물리적으로 결합되어 있는 폴리올레핀계 다층필름의 층간 계면을 교란시켜서 층간을 분리시키고 있다.In the present invention, the polyolefin-based multilayer film broken with liquid nitrogen is first impregnated and etched into a solution consisting of at least one of a) permanganic acid or chromic acid and b) phosphoric acid and sulfuric acid to disturb the interlayer interface of the polyolefin-based multilayer film physically bonded. To separate the layers.
본 발명에서 사용하는 용액은 특정한 조성하에서 폴리올레핀계 다층필름의 구성층을 선택적으로 교란시켜 분리해낼 수 있는 기능을 발휘하며, 이와 더불어 에칭온도와 시간을 조절하는 것도 중요한 변수로 작용한다. 본 발명의 에칭조건과 화합물의 조성은 폴리올레핀계 다층필름을 구성하는 수지의 종류에 따라서 다르게 적용될 수 있다.The solution used in the present invention exhibits a function of selectively disturbing and separating the constituent layers of the polyolefin multilayer film under a specific composition, and in addition, controlling the etching temperature and time also serves as an important variable. The etching conditions and the composition of the compound of the present invention may be applied differently depending on the type of resin constituting the polyolefin-based multilayer film.
이하에서 사용되는 에칭용액과 에칭조건을 상세하게 설명하면 다음과 같다.Hereinafter, the etching solution and etching conditions used in detail will be described.
사용되는 에칭 용액의 조성은 a) 과망간산 또는 크롬산 0.1∼12 중량% 및 b) 인산 및 황산 중 하나 이상이 99.9∼88 중량%의 조성비로 이루어지는 것이 바람직하며, 상기 범위를 벗어나는 경우 다층필름의 분리효과가 좋지 못하다.The composition of the etching solution used is preferably a composition of a) permanganic acid or chromic acid 0.1 to 12% by weight and b) at least one of phosphoric acid and sulfuric acid at a composition ratio of 99.9 to 88% by weight. Is not good
에칭조건은 에칭시간이 20분 내지 120분, 에칭온도가 20∼50℃가 되도록 함이 바람직하다. 20분 미만 또는 20℃ 미만 조건에서 에칭하는 경우 층분리효과가 충분히 나타나지 않고, 120분 초과 또는 50℃ 초과 조건에서 에칭하는 경우 시료의 손상을 가져올 염려가 있다.The etching conditions are preferably such that the etching time is 20 minutes to 120 minutes and the etching temperature is 20 to 50 ° C. If the etching is less than 20 minutes or less than 20 ℃ conditions are not sufficiently separated, there is a fear that the sample is damaged if the etching is more than 120 minutes or more than 50 ℃ conditions.
또한, 상기 용액에서 인산과 황산이 함께 사용되는 경우 그 몰농도비를 1:3 내지 2:3로 하는 것이 효과가 좋다.
In addition, when phosphoric acid and sulfuric acid are used together in the solution, the molar concentration ratio is 1: 3 to 2: 3.
비교예 1Comparative Example 1
3층으로 구성된 폴리프로필렌 캐스팅필름을 종래의 방법에 따라 액체질소로 파단한 후 도전성 코팅을 행하여 주사전자현미경으로 관찰하였다.
The polypropylene casting film composed of three layers was broken with liquid nitrogen according to a conventional method, and then subjected to conductive coating and observed with a scanning electron microscope.
실시예 1Example 1
비교예에서 사용한 것과 동일한 3층으로 구성된 폴리프로필렌 캐스팅 필름을 액체질소로 파단한 후, 1중량%의 과망간산과 황산과 인산을 1:1 몰비로 혼합한 용액 99중량%로 이루어진 에칭용액을 사용하여 30℃에서 20분동안 에칭시켰다. 에칭된 시료를 증류수로 2회 씻어낸 후 과망간산 등의 잔류물제거를 위하여 과산화수소수에 2분간 담구어 두었다. 다음 증류수로 씻어낸 후 울트라소니케이터를 이용하여 아세톤 혹은 알콜 용액하에서 30분 세척하여 시료를 채취하였다. 채취된 시료에 도 전성코팅을 행하여 주사전자현미경으로 관찰하였다.
After breaking the polypropylene casting film composed of the same three layers as used in the comparative example with liquid nitrogen, using an etching solution consisting of 99% by weight of a solution in which 1% by weight of permanganic acid, sulfuric acid and phosphoric acid were mixed in a 1: 1 molar ratio. Etched at 30 ° C. for 20 minutes. The etched sample was washed twice with distilled water and then immersed in hydrogen peroxide for 2 minutes to remove residues such as permanganic acid. Next, washed with distilled water and then washed with an ultrasonicator under acetone or alcohol solution for 30 minutes to take a sample. Conducting coating was performed on the collected samples and observed with a scanning electron microscope.
도 2와 3은 각각 비교예 1과 실시예 1에 의한 폴리프로필렌 캐스팅필름의 단면을 촬영한 사진으로, 비교예 1에는 나타나지 않았던 내외면의 표면층이 실시예 1에서 선명하게 나타남을 알 수 있다. 이는 본 발명의 처리방법에 의해 물리적으로 결합된 필름사이가 교란되어 층의 분리현상이 나타나고 있음을 보여주는 것이다.
2 and 3 are photographs taken in cross section of the polypropylene casting film according to Comparative Example 1 and Example 1, respectively, it can be seen that the surface layer of the inner and outer surfaces that did not appear in Comparative Example 1 is clearly shown in Example 1. This shows that the separation of the layers appears due to the disturbance between the physically bonded film by the treatment method of the present invention.
본 발명에 의한 폴리올레핀계 다층필름의 처리방법에 의하면 유사한 조성을 갖는 폴리올레핀계 다층 필름의 층간 계면이 교란되어 각 층에 관해서 보다 정확하게 분석할 수 있다.According to the treatment method of the polyolefin multilayer film according to the present invention, the interlayer interface of the polyolefin multilayer film having a similar composition is disturbed, and each layer can be analyzed more accurately.
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| KR102291672B1 (en) | 2019-11-21 | 2021-08-24 | 한국생산기술연구원 | Cellulose nano fiber surface ceramic modifing method for and ceramic coating solution manufactring method using thereof |
| KR102240133B1 (en) | 2019-11-21 | 2021-04-15 | 한국생산기술연구원 | CONDUCTIVITY BASE FILM FOR Scanning Electron Microscope ANALYSIS |
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