阅读说明：本技术 一种tem试片检测的金属防扩散方法 (Metal anti-diffusion method for TEM specimen detection ) 是由 胡荣志 储耕颉 陈明志 于 2019-10-12 设计创作，主要内容包括：本发明涉及试片检测技术领域,公开了一种TEM试片检测的金属防扩散方法,包括如下步骤：S1,采用聚焦式粒子束切削薄化制作TEM试片；S2,制备清洗溶液,清洗溶液包括蒸馏水和硫醇；S3,将TEM试片放入清洗溶液中浸泡后取出；S4,将TEM试片放入电浆清洗机中清洗后取出,硫醇的疏基官能团-SH中的H可以由纳米级的Cu或Ag及其氧化物替换,在由电浆清洗机去除硫醇的同时,连同Cu或Ag及其氧化物一起去除脱离TEM试片表面,完成处理,减少后续TEM造影过程中因出现的因Cu或Ag扩散引起的造影浑浊。(The invention relates to the technical field of test piece detection, and discloses a metal anti-diffusion method for TEM test piece detection, which comprises the following steps: s1, manufacturing a TEM specimen by cutting and thinning a focused particle beam; s2, preparing a cleaning solution, wherein the cleaning solution comprises distilled water and mercaptan; s3, putting the TEM specimen into a cleaning solution for soaking and then taking out; s4, the TEM specimen is put into a plasma cleaner for cleaning and then taken out, H in the mercapto functional group-SH of the mercaptan can be replaced by nano-scale Cu or Ag and oxides thereof, the mercaptan is removed by the plasma cleaner, and simultaneously the mercaptan and the Cu or Ag and the oxides thereof are removed and separated from the surface of the TEM specimen to finish treatment, thereby reducing the contrast turbidity caused by Cu or Ag diffusion in the subsequent TEM contrast process.)

1. A metal diffusion prevention method for TEM specimen detection is characterized by comprising the following steps:

s1, manufacturing a TEM specimen by cutting and thinning a focused particle beam;

s2, preparing a cleaning solution, wherein the cleaning solution comprises distilled water and mercaptan;

s3, putting the TEM specimen into the cleaning solution for soaking and then taking out;

s4, putting the TEM specimen into a plasma cleaning machine for cleaning and taking out.

2. A TEM coupon-based method of detecting metals diffusion according to claim 1, wherein the thiol is tert-dodecyl mercaptan.

3. The method for preventing metal diffusion in a TEM coupon according to claim 1, wherein the cleaning solution further comprises toluene in step S2.

4. The method for preventing metal diffusion in a TEM coupon according to claim 1, wherein the cleaning solution further comprises n-hexane in step S2.

5. The method for preventing metal diffusion according to claim 1, wherein the soaking time in step S3 is 5 minutes.

6. The method of claim 5, wherein step S3 further comprises introducing an inert gas into the cleaning solution while immersing the TEM coupon, and applying vibration energy to the container containing the cleaning solution using an ultrasonic device.

7. A TEM specimen-detected metal diffusion prevention method as claimed in claim 6, characterized in that the washing solution is stirred while the TEM specimen is immersed.

Technical Field

The invention relates to the technical field of test piece detection, in particular to a metal anti-diffusion method for TEM test piece detection.

Background

A Transmission Electron Microscope (TEM) is a microscopic structure, which is a microscopic structure less than 0.2um and cannot be seen clearly under an optical Microscope, and the microscopic structure can be obtained clearly by the TEM.

In the existing chip detection industry, in some cases, a sample suitable for TEM observation needs to be prepared for a chip to be detected, and a sample is generally thinned by a Focused Ion Beam (FIB) or a manual grinding and cutting method to prepare a TEM test piece for TEM observation and detection.

However, in the process of sample preparation, because the sample is used as a semiconductor chip, metal materials such as Cu and Ag which are easily oxidized in the atmospheric environment are generally used, and in the microstructure, these metal materials are extremely easily oxidized or diffused, and once oxidized or diffused, a large amount of turbid shadows are caused in the subsequent TEM contrast film, and it is difficult to perform subsequent accurate detection and observation.

Disclosure of Invention

In view of the above problems, an object of the present invention is to provide a metal diffusion preventing method for TEM strip detection, which has the advantage of less turbid contrast of the subsequent strip.

The above object of the present invention is achieved by the following technical solutions:

a metal diffusion prevention method for TEM specimen detection comprises the following steps:

s1, manufacturing a TEM specimen by cutting and thinning a focused particle beam;

s2, preparing a cleaning solution, wherein the cleaning solution comprises distilled water and mercaptan;

s3, putting the TEM specimen into the cleaning solution for soaking and then taking out;

s4, putting the TEM specimen into a plasma cleaning machine for cleaning and taking out.

Through the technical scheme, H in the mercapto functional group-SH of the mercaptan can be replaced by nano-scale Cu or Ag and oxides thereof, and the mercaptan is removed by the plasma cleaning machine and simultaneously removed together with the Cu or Ag and the oxides thereof to separate from the surface of the TEM specimen to finish treatment, so that the contrast turbidity caused by Cu or Ag diffusion in the subsequent TEM contrast process is reduced.

The invention is further configured to: the mercaptan is tert-dodecyl mercaptan.

By adopting the technical scheme, the tertiary dodecyl mercaptan is adopted, so that the nano-scale Cu or Ag can replace H in the mercapto functional group-SH of the mercaptan, and the diffused Cu or Ag can be effectively adsorbed.

The invention is further configured to: in step S2, the cleaning solution further includes toluene.

Through above-mentioned technical scheme, toluene can be mutually soluble with the grease on the test block, and clean test block surface reduces impurity.

The invention is further configured to: in step S2, the cleaning solution further includes n-hexane.

Through the technical scheme, the n-ethane can decompose the grease, and the influence of the grease on the subsequent radiography of the test piece is greatly reduced.

The invention is further configured to: in step S3, the soaking time is 5 minutes.

Through the technical scheme, the cleaning solution can be fully contacted with the surface of the test piece.

The invention is further configured to: step S3 further includes, while immersing the TEM specimen, introducing an inert gas into the cleaning solution, and applying vibration energy to a container containing the cleaning solution by using an ultrasonic device.

Through above-mentioned technical scheme, inert gas's the letting in can produce a large amount in cleaning solution, and the cooperation vibrations energy can make cleaning solution and test piece produce contact more closely to promote abluent effect.

The invention is further configured to: and stirring the cleaning solution while soaking the TEM specimen.

Through the technical scheme, the cleaning solution is further promoted to be contacted with the test piece.

Compared with the prior art, the invention has the beneficial effects that:

h in the mercapto functional group-SH of the mercaptan can be replaced by nano-scale Cu or Ag and oxides thereof, and the mercaptan is removed by a plasma cleaner and simultaneously removed and separated from the surface of the TEM specimen together with the Cu or Ag and the oxides thereof to finish treatment, so that the contrast turbidity caused by Cu or Ag diffusion in the subsequent TEM contrast process is reduced.

Detailed Description

The present invention will be described in detail with reference to examples.

A metal diffusion prevention method for TEM specimen detection comprises the following steps:

s1, manufacturing a TEM specimen by cutting and thinning a focused particle beam;

s2, preparing a cleaning solution, wherein the cleaning solution comprises distilled water and mercaptan;

s3, putting the TEM specimen into a cleaning solution for soaking and then taking out;

s4, the TEM specimen is taken out after being cleaned in the plasma cleaning machine.

H in the mercapto functional group-SH of the mercaptan can be replaced by nano-scale Cu or Ag and oxides thereof, and the mercaptan is removed by a plasma cleaner and simultaneously removed and separated from the surface of the TEM specimen together with the Cu or Ag and the oxides thereof to finish treatment, so that contrast turbidity caused by Cu or Ag diffusion in the subsequent TEM contrast process is reduced.

In the present example, tert-dodecyl mercaptan is adopted as mercaptan, so that nano-scale Cu or Ag can replace H in mercapto functional group-SH of mercaptan, and diffused Cu or Ag can be effectively adsorbed.

In step S2, the cleaning solution further includes toluene and n-hexane. Toluene can be mutually dissolved with grease on the test piece, so that the surface of the test piece is cleaned, and impurities are reduced. The n-ethane can decompose the grease, and the influence of the grease on the subsequent radiography of the test piece is greatly reduced.

In step S3, the immersion time was 5 minutes, which allowed sufficient contact between the cleaning solution and the surface of the test piece, and while immersing the TEM test piece, inert gas was introduced into the cleaning solution, and vibration energy was applied to the container containing the cleaning solution using an ultrasonic device. The inert gas can be introduced into the cleaning solution to generate a large amount of inert gas, and the cleaning solution can be in closer contact with the test piece by matching with vibration energy, so that the cleaning effect is improved. The cleaning solution can be stirred at the same time, so that the cleaning solution is further contacted with the test piece.

The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.