WO2018000350A1 - 一种柔性膜脆断方法 - Google Patents

一种柔性膜脆断方法 Download PDF

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WO2018000350A1
WO2018000350A1 PCT/CN2016/087957 CN2016087957W WO2018000350A1 WO 2018000350 A1 WO2018000350 A1 WO 2018000350A1 CN 2016087957 W CN2016087957 W CN 2016087957W WO 2018000350 A1 WO2018000350 A1 WO 2018000350A1
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silicon wafer
flexible film
brittle
composite
frozen
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PCT/CN2016/087957
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French (fr)
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周肇梅
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周肇梅
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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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  • This invention relates to chemistry, and more particularly to a flexible membrane brittle method.
  • the present invention has devised a new flexible membrane brittle breaking method for solving the above technical problems, and the method comprises the following steps:
  • the composite silicon wafer is placed in liquid nitrogen and immersed to be sufficiently cooled to obtain a frozen silicon wafer;
  • the frozen silicon wafer is brittle and a brittle broken flexible film is obtained.
  • the method is used to make the flexible film brittle, which has the following advantages: Firstly, the area of the silicon wafer is relatively large, and it is convenient to perform the operation manually, which overcomes the problem that the sample used in the preparation of the electron microscope sample is difficult to be supported by the tweezers; When the fracture is broken, the section is unevenly stressed. It may be uneven, but in this method, the silicon wafer has a prior scribe line, and suddenly breaks when it breaks.
  • the nearby film is stressed and concentrated, which is easy to cause a flat section, which overcomes the problem of unevenness of the obtained section;
  • the flexible film is generally brittle at normal temperature at normal temperature, but does not mean complete brittleness for many samples, and the flexible film brittle method provided by the present invention is easy to form a brittle fracture because the silicon wafer breaks suddenly and rapidly. It can be overcome that some samples are relatively flexible at liquid nitrogen temperatures and may not be able to break.
  • the step B of the method may also be: attaching the flexible film to the pre-etched silicon wafer, and then attaching the conductive double-sided adhesive to the flexible film to obtain a composite silicon wafer, wherein the composite silicon wafer is The sandwich structure, wherein the bottom layer is a silicon wafer, the middle layer is a flexible film, and the upper layer is a conductive double-sided tape.
  • This sandwich structure is specially designed for electron microscope observation.
  • the conductive double-sided tape here is a carbon conductive double-sided tape commonly used in electron mirror preparation. In this way, the flexible film can be directly applied to the experimental observation after the brittle fracture, and the flexible film is attached to the observation dish without re-attaching the conductive double-sided tape.
  • the silicon wafer is pre-etched using a glass cutter in step A.
  • the silicon wafer used in the flexible film brittle method is elongated, and the ratio of the length to the width of the silicon wafer is greater than 2:1. Only when the aspect ratio of the silicon wafer is larger than a certain value, it is convenient to clamp and break the silicon wafer with the tweezers, and the silicon wafer structure whose aspect ratio is too short is inconvenient to concentrate stress.
  • the flexible film and the conductive double-sided tape used in the flexible film brittle method are the same in size as the silicon wafer.
  • the same size facilitates the bonding of the flexible film and the silicon wafer.
  • the silicon wafer may be brittle and may cause brittle fracture on the portion of the flexible film where only the silicon wafer overlaps, and the portion wider than the silicon wafer. There is no fracture or plastic fracture, which is particularly worthy of emphasis in polymer flexible membranes.
  • the time during which the composite silicon wafer is immersed in liquid nitrogen in step C is greater than 120 seconds. Sufficient time to ensure that the flexible film is completely embrittled without plastic deformation.
  • step D the frozen silicon wafer is taken out using tweezers.
  • Other tools can also be used to remove the frozen silicon wafer.
  • step E the frozen silicon wafer is clamped using tweezers.
  • Other tools can also be used to clamp and apply pressure to the frozen wafer.
  • the method is used to obtain the brittle fracture cross section of the flexible film to overcome the three problems mentioned above.
  • the area of the silicon wafer is relatively large, which is convenient for manual operation, and overcomes the difficulty in the preparation of the small sample tweezers in the preparation of the electron microscope sample.
  • the common method is uneven because of the uneven force of the section when it is broken.
  • the silicon wafer is broken due to the prior engraving, and the film is weak and concentrated in the vicinity, which is easy to cause.
  • the flat section overcomes the problem of unevenness of the obtained section; although the flexible film is generally brittle at normal temperature at low temperatures, it does not mean complete brittleness for many samples, and the flexible membrane brittle fracture method provided by the present invention is used. Because the silicon wafer breaks suddenly and rapidly, it is easier to form a brittle fracture, which can overcome the problem that some samples are relatively flexible at liquid nitrogen temperature and may not be broken.
  • 1 is a pre-etched silicon wafer provided by an embodiment of the present invention.
  • FIG. 2 is a schematic view showing a sandwich structure of a composite silicon wafer according to an embodiment of the present invention.
  • FIG. 3 is a schematic diagram of the force applied to the composite silicon wafer according to the embodiment of the present invention.
  • FIG. 4 is a schematic view of a composite silicon wafer after brittle fracture according to an embodiment of the present invention.
  • a polymer flexible film is prepared, and the polymer flexible film is cut into a size similar to that of the elongated silicon wafer.
  • the polymer flexible film, the conductive double-sided tape, and the silicon wafer are sequentially pasted into a sandwich structure to form a composite silicon wafer.
  • the composite silicon wafer is immersed in liquid nitrogen for two minutes, and is sufficiently cooled to obtain a frozen silicon wafer.
  • the frozen silicon structure is taken out with a long tweezers, and the two tweezers are placed on both sides, and the opposite direction of the film is forced to be brittle.
  • the specific direction is shown in Figure 3.
  • the method of the present embodiment is used to obtain the brittle fracture cross section of the flexible film to overcome the three problems mentioned above.
  • the area of the silicon wafer is relatively large, which is convenient for manual operation, and overcomes the small sample used in the preparation of the electron microscope sample.
  • the problem that the scorpion is difficult to buck; the commonly used method may be uneven because of the uneven force of the section when the rupture occurs, but in this method, the silicon wafer is suddenly ruptured due to the prior scribe line, and the nearby film is stressed and concentrated. It is easy to cause a flat section, which overcomes the problem of uneven section; although the flexible membrane is generally brittle at normal temperature at low temperatures, it does not mean complete brittleness for many samples.
  • the flexible film brittle breaking method provided by the invention, since the silicon wafer breaks suddenly and rapidly, it is easy to form a brittle fracture, which can overcome the problem that some samples are relatively flexible at liquid nitrogen temperature and cannot be disconnected.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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Abstract

一种柔性膜脆断方法，包括以下步骤：A．对硅片进行预刻槽处理；B．将柔性膜贴在硅片上；C．将上述B步骤得到的复合硅片投入液氮中浸没放置使其充分冷却；D．将其从液氮中取出；E．夹住硅片两侧，同时向硅片预刻槽的面施加力；F．使得硅片连同贴在硅片上薄膜发生脆断；使用本方法来获得柔性膜脆断截面的面积比较大，比较方便人工进行操作，克服了制备电镜制样中样品小用镊子难以加持的问题；而常用的方法因为断裂的时候断面受力不均，可能不平，但是本方法中硅片因为有预先的刻线，断裂的时候突然断裂，附近的薄膜受力大且集中，较易造成平整的断面，克服了制得的断面不平整的问题。

Description

一种柔性膜脆断方法 技术领域
本发明涉及化学，特别涉及一种柔性膜脆断方法。
背景技术
在研究中常常需要将柔性膜断面在扫描电镜中观察，但是如果用剪刀剪或者用力撕断则可能发生塑性变形，破坏了已有形貌。目前通常比较有效的方法是将薄膜剪成小条然后浸泡入液氮中，液氮温度大约为-195℃，待样品充分冷却变脆后用两个镊子夹住条状物，然后向中间弯曲，使样品脆断，从而得到断面样品。但是这存在三个问题，一是样品小用镊子难以加持，二是断面往往不平整，不利于电镜分析，三是有些样品在液氮温度下还是比较柔韧，不一定能断开。
发明内容
本发明为解决上述技术问题而设计了一种新的柔性膜脆断方法，该方法包括以下步骤：
A.对硅片进行预刻处理，得到带有槽的硅片；
B.将柔性膜贴在上述硅片上，得复合硅片；
C.将复合硅片投入液氮中浸没放置使其充分冷却，得冷冻硅片；
D.将冷冻硅片从液氮中取出；
E.固定冷冻硅片两侧，同时向复合硅片带有槽的面施加力；
F.使得冷冻硅片发生脆断，得到脆断的柔性膜。
使用本方法使柔性膜发生脆断，具有以下优点：首先，硅片的面积比较大，比较方便人工进行操作，克服了制备电镜制样中样品小用镊子难以加持的问题；而常用的方法因为断裂的时候断面受力不均， 可能不平，但是本方法中硅片因为有预先的刻线，断裂的时候突然断裂，附近的薄膜受力大且集中，较易造成平整的断面，克服了制得的断面不平整的问题；虽然柔性膜在低温下一般都较常温下脆，但是对很多样品不意味着完全的脆性，而使用本发明提供的柔性膜脆断方法，因为硅片断裂时突然、迅猛，较易形成脆性断口，可以克服有些样品在液氮温度下还是比较柔韧，不一定能断开的问题。
作为本方法的改进：该方法的B步骤也可以是：将柔性膜贴在经过预刻的硅片上，然后在柔性膜上贴导电双面胶，得到复合硅片，所述复合硅片为三明治结构，其中最下一层为硅片，中间一层为柔性膜，最上面一层为导电双面胶。这种三明治结构是专门为电镜观察而设计的，这里的导电双面胶是电镜制样常用的碳导电双面胶。这样柔性膜发生脆断只后可以直接应用于实验观测，将柔性膜贴在观察皿中，而不需要再次贴导电双面胶。
作为本方法的改进：步骤A中使用玻璃刀对硅片进行预刻处理。
作为本方法的改进：所述柔性膜脆断方法中用到的硅片为长条状，所述硅片的长度与宽度之比大于2：1。只有当硅片的长宽比大于一定数值时才方便用镊子将硅片夹住并掰断，长宽比太短的硅片结构不方便集中应力。
作为本方法的改进：所述柔性膜脆断方法中用到的所述柔性膜和所述导电双面胶的尺寸与所述硅片相同。相同的尺寸方便柔性膜和硅片贴合，如果柔性膜的宽度大于硅片宽度，硅片脆断时可能使得柔性膜上只有硅片重合的部分发生脆性断裂，而比硅片宽的部分 则没有断裂或者发生塑性断裂，这一点在高分子柔性膜中尤其值得强调。
作为本方法的改进：步骤C中复合硅片浸入液氮的时间大于120秒。足够的时间以确保柔性膜完全脆化，不会发生塑性变形。
作为本方法的改进：步骤D中使用镊子将冷冻硅片取出。也可以使用其他工具将冷冻硅片取出。
作为本方法的改进：步骤E中使用镊子将冷冻硅片夹住。也可以使用其他工具将冷冻硅片夹住并施加压力。
使用本方法来获得柔性膜脆断截面克服了之前提到的三个问题，第一：硅片的面积比较大，比较方便人工进行操作，克服了制备电镜制样中样品小用镊子难以加持的问题；而常用的方法因为断裂的时候断面受力不均，可能不平，但是本方法中硅片因为有预先的刻线，断裂的时候突然断裂，附近的薄膜受力大且集中，较易造成平整的断面，克服了制得的断面不平整的问题；虽然柔性膜在低温下一般都较常温下脆，但是对很多样品不意味着完全的脆性，而使用本发明提供的柔性膜脆断方法，因为硅片断裂时突然、迅猛，较易形成脆性断口，可以克服有些样品在液氮温度下还是比较柔韧，不一定能断开的问题。
附图说明
图1是本发明实施例提供的经过预刻的硅片。
图2是本发明实施例提供的复合硅片的三明治结构示意图。
图3是本发明实施例提供的复合硅片的受力示意图。
图4是本发明实施例提供的发生脆断后的复合硅片示意图。
具体实施方式
下面详细说明本发明的具体实施方案。
以制备用于扫描电子显微镜的高分子柔性膜脆断面为例。
首先，如图1所示，我们准备一个长条状的硅片，硅片长2cm，宽5mm，长宽比远远大于2：1，满足了限制条件，然后在硅片长条中间的一侧用玻璃刀预刻，得到一个一面带有凹槽的硅片。
然后准备高分子柔性薄膜，将高分子柔性薄膜剪成跟长条形硅片相仿的尺寸。
第三步，如图2所示，将高分子柔性薄膜、导电双面胶、硅片依次粘贴成三明治结构，成为复合硅片。
第四步，将复合硅片投入液氮中浸没，放置两分钟，待其充分冷却，得到冷冻硅片。
第五步，用长镊子将冷冻硅片结构取出，用两个镊子居两侧，用力朝膜的反向弯，待其脆断。具体方向见图3。
然后就能得到如图4所示的发生脆断的高分子柔性膜断面。
使用本具体实施例中方法来获得柔性膜脆断截面克服了之前提到的三个问题，第一：硅片的面积比较大，比较方便人工进行操作，克服了制备电镜制样中样品小用镊子难以加持的问题；而常用的方法因为断裂的时候断面受力不均，可能不平，但是本方法中硅片因为有预先的刻线，断裂的时候突然断裂，附近的薄膜受力大且集中，较易造成平整的断面，克服了制得的断面不平整的问题；虽然柔性膜在低温下一般都较常温下脆，但是对很多样品不意味着完全的脆性，而使 用本发明提供的柔性膜脆断方法，因为硅片断裂时突然、迅猛，较易形成脆性断口，可以克服有些样品在液氮温度下还是比较柔韧，不一定能断开的问题。
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说明，不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干简单推演或替换，都应当视为属于本发明的保护范围。

Claims (8)

  1. 一种柔性膜脆断方法，其特征在于：该方法包括以下步骤：
    A.对硅片进行预刻处理，得到带有槽的硅片；
    B.将柔性膜贴在上述硅片上，得复合硅片；
    C.将复合硅片投入液氮中浸没放置使其充分冷却，得冷冻硅片；
    D.将冷冻硅片从液氮中取出；
    E.固定冷冻硅片两侧，同时向复合硅片带有槽的面施加力；
    F.使得冷冻硅片发生脆断，得到脆断的柔性膜。
  2. 根据权利要求1所述的柔性膜脆断方法，其特征在于：该方法的B步骤也可以是：将柔性膜贴在经过预刻的硅片上，然后在柔性膜上贴导电双面胶，得到复合硅片，所述复合硅片为三明治结构，其中最下一层为硅片，中间一层为柔性膜，最上面一层为导电双面胶。
  3. 根据权利要求1或2所述的柔性膜脆断方法，其特征在于：步骤A中使用玻璃刀对硅片进行预刻处理。
  4. 根据权利要求2所述柔性膜脆断方法，其特征在于：所述柔性膜脆断方法中用到的硅片为长条状，所述硅片的长度与宽度之比大于2：1。
  5. 根据权利要求4所述柔性膜脆断方法，其特征在于：所述柔性膜脆断方法中用到的所述柔性膜和所述导电双面胶的尺寸与所述硅片相同。
  6. 根据权利要求1所述柔性膜脆断方法，其特征在于：步骤C中复合硅片浸入液氮的时间大于120秒。
  7. 根据权利要求1所述柔性膜脆断方法，其特征在于：步骤D中使用镊子将冷冻硅片取出。
  8. 根据权利要求1所述柔性膜脆断方法，其特征在于：步骤E中使用镊子将冷冻硅片夹住。
PCT/CN2016/087957 2016-06-30 2016-06-30 一种柔性膜脆断方法 WO2018000350A1 (zh)

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CN109708944A (zh) * 2019-02-19 2019-05-03 大连理工大学 一种硅的损伤层透射电镜原位纳米压痕方法
CN110514490A (zh) * 2019-07-31 2019-11-29 东莞维科电池有限公司 一种制作极片截面的方法及装置
CN111039254A (zh) * 2018-10-15 2020-04-21 无锡华润上华科技有限公司 Mems样品纵向截面的制备方法及形貌观察方法
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CN109708944A (zh) * 2019-02-19 2019-05-03 大连理工大学 一种硅的损伤层透射电镜原位纳米压痕方法
CN109708944B (zh) * 2019-02-19 2021-03-26 大连理工大学 一种硅的损伤层透射电镜原位纳米压痕方法
CN110514490A (zh) * 2019-07-31 2019-11-29 东莞维科电池有限公司 一种制作极片截面的方法及装置
CN110514490B (zh) * 2019-07-31 2022-04-08 东莞维科电池有限公司 一种制作极片截面的方法及装置
CN116500071A (zh) * 2023-06-30 2023-07-28 国家电投集团氢能科技发展有限公司 一种增强型复合膜材料的截面扫描电镜样品制备方法
CN116500071B (zh) * 2023-06-30 2023-12-26 国家电投集团氢能科技发展有限公司 一种增强型复合膜材料的截面扫描电镜样品制备方法

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