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Transmission electron microscope high-resolution in-situ liquid phase temperature change chip and production method thereof

An in-situ liquid phase and transmission electron microscopy technology, which is applied in the preparation of test samples, material analysis using radiation, material analysis using wave/particle radiation, etc., can solve the limitations, single state of matter, and inability to achieve alternate transformation And other issues

Pending Publication Date: 2020-10-23
XIAMEN CHIP NOVA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Limited by the frozen state of the sample, we can only observe a single static state when the sample is frozen, and cannot observe the entire three-dimensional dynamic change process of the sample in the real solution environment, which limits our research on the real reaction system. great limitations
The single state of matter after freezing and the inability to achieve alternate transformation are the biggest obstacles limiting its application

Method used

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  • Transmission electron microscope high-resolution in-situ liquid phase temperature change chip and production method thereof
  • Transmission electron microscope high-resolution in-situ liquid phase temperature change chip and production method thereof
  • Transmission electron microscope high-resolution in-situ liquid phase temperature change chip and production method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0145] The preparation method of the upper sheet is as follows:

[0146] S1. Using the photolithography process, the central window pattern is transferred from the photolithography mask to the Si (100) wafer A with silicon nitride or silicon oxide layers on both sides, and then developed in the positive resist developing solution to obtain the wafer A-1;

[0147] Preferably, the photolithography process is exposed in the hard contact mode of the ultraviolet lithography machine; the thickness of the silicon nitride or silicon oxide layer is 5-200nm; the development time is 50s;

[0148] More preferably, the exposure time is 15s;

[0149] S2. Utilize the reactive ion etching process to etch a central window on the silicon nitride layer on the front side of the wafer A-1, then put the front side of the wafer A-1 up into acetone to soak, and finally use a large amount of Rinse with deionized water, remove the photoresist, and obtain wafer A-2;

[0150] S3. Using the ultraviolet...

Embodiment 1

[0201] Example 1: Preparation of a high-resolution in-situ liquid-phase temperature-changing chip by transmission electron microscopy

[0202] The preparation method of the upper sheet is,

[0203] S1. Using the photolithography process (exposure for 15s in the hard contact mode of the UV lithography machine), transfer the central window pattern from the photolithography mask to the Si(100) crystal with silicon nitride or silicon oxide layers on both sides. Circle A is then developed in positive photoresist developer for 50s to obtain wafer A-1; the thickness of the silicon nitride or silicon oxide layer is 5-200nm;

[0204] S2. Utilize the reactive ion etching process to etch a central window on the silicon nitride layer on the front side of the wafer A-1, then put the front side of the wafer A-1 up into acetone to soak, and finally use a large amount of Rinse with deionized water, remove the photoresist, and obtain wafer A-2;

[0205] S3. Using the ultraviolet laser direct...

Embodiment 2

[0231] Example 2: Use of a high-resolution in-situ liquid-phase temperature-changing chip for transmission electron microscopy

[0232] Inject an aqueous solution of supersaturated calcium hydroxide (the solution contains a small amount of calcium hydroxide particles) into the sample injection port of the transmission electron microscope high-resolution in-situ liquid phase temperature change chip prepared in Example 1. Temperature software, set the chip temperature to -30°C, get Figure 7 Electron microscope image from Figure 7 It can be seen from A and B that as the temperature rises, the solution temperature rises, the solubility of the solute gradually decreases, and calcium hydroxide solids are precipitated, and the nanoparticles are calcium hydroxide solids that are precipitated during the temperature rise of the chip. By controlling the amount of energization of the chip, the temperature of the solution in the chip can be monitored and controlled in real time. This t...

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Abstract

The invention discloses a transmission electron microscope high-resolution in-situ liquid phase temperature change chip and a production method thereof. A lower piece of the chip is provided with a supporting layer, a freezing layer, an insulating layer, a heating layer, an insulating layer, a hole channel and a central window; the freezing layer is provided with four contact electrodes, a semiconductor refrigeration film and a conductive metal film; in an area where the central window and the semiconductor refrigeration film are located, the hole channel is reserved after silicon is corroded,and the supporting layer covers the hole channel; the semiconductor refrigeration film and the conductive metal film are both arranged on the supporting layer; a circle of metal film is deposited onthe supporting layer with the central window as a center; a front end of the semiconductor refrigeration film is lapped on the metal film, and the rear end is connected with the four contact electrodes; the freezing layer and the heating layer are separated through the insulating layer; the heating layer is provided with two contact electrodes and a spiral annular heating wire, and the heating wire is located above the semiconductor refrigeration film; and a plurality of small holes are formed in the central window. The chip is large in temperature control range, high in temperature changing speed and capable of achieving in-situ dynamic observation.

Description

technical field [0001] The invention relates to the field of liquid phase chips, in particular to a transmission electron microscope high-resolution in-situ liquid phase variable temperature chip and a preparation method thereof. Background technique [0002] In recent years, a new technology developed in the field of transmission electron microscopy-in-situ chip transmission electron microscopy has been able to observe the morphology evolution and molecular structure changes of substances in the solution environment at the atomic scale under in-situ conditions. The in-situ chip electron microscope technology can observe gas The chemical reaction process in the liquid environment is of great significance for the study of the reaction principle and the control of the reaction process. The existing TEM freezing technology characterization is to quickly cool the sample, the solvent molecules become glassy, ​​and the sample is also instantaneously frozen, so as to obtain a more ...

Claims

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Application Information

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IPC IPC(8): G01N23/02G01N23/2202G01N1/42G01N1/44
CPCG01N23/02G01N23/2202G01N1/42G01N1/44G01N2223/03G01N2223/07G01N2223/3103G01N2223/3106
Inventor 廖洪钢江友红
Owner XIAMEN CHIP NOVA TECH CO LTD
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