Transmission electron microscope in-situ chip and preparation method therefor

Abstract

The present disclosure discloses a transmission electron microscope in-situ chip and a preparation method thereof. The transmission electron microscope in-situ chip includes a transmission electron microscope high-resolution in-situ gas phase heating chip, a transmission electron microscope high-resolution in-situ liquid phase heating chip and a transmission electron microscope in-situ electrothermal coupling chip. The transmission electron microscope high-resolution in-situ gas phase heating chip and the transmission electron microscope high-resolution in-situ liquid phase heating chip are respectively suitable for gas samples and liquid samples, and the transmission electron microscope in-situ electrothermal coupling chip realizes the multi-functional embodiment of electrothermal coupling. The three transmission electron microscope in-situ chips have the advantages of high resolution and low sample drift rate.

What is claimed is: 
     
         1 . A transmission electron microscope in-situ liquid phase heating chip, structurally comprising a top chip and a bottom chip combined via a metal bonding layer, the top chip and the bottom chip each comprising a front side and a back side, the front side of the top chip being directly bonded to the front side of the bottom chip via the metal bonding layer to be self-sealed to form a chamber, and the top chip and the bottom chip being each made of a silicon substrate with silicon nitride or silicon oxide on two sides, wherein
 the top chip is provided with two sample injection ports and a first central window, the first central window is located in a center of the top chip, and the two sample injection ports are symmetrically disposed with respect to the first central window;   the bottom chip is provided with a liquid inlet, a runner, a liquid outlet, a heating layer, a second central window and an insulating layer; the heating layer is provided with four contact electrodes and a spiral annular heating wire, the spiral annular heating wire is in a symmetrical shape, inner coils of the spiral annular heating wire are spaced apart and disconnected from each other, and the four contact electrodes are disposed at an edge of the transmission electron microscope in-situ liquid phase heating chip; a heating wire in a center of the heating layer is disposed on the silicon substrate of the bottom chip; in a region with the second central window as a center and being larger than an outer edge of the spiral annular heating wire, a silicon nitride layer or silicon oxide layer is used as a support film, silicon below the silicon nitride layer or the silicon oxide layer is completely etched, and the silicon nitride layer or the silicon oxide layer is reserved to be suspended on a position, in a heating wire center region of the heating layer, of the silicon substrate of the bottom chip and other positions of the silicon substrate of the bottom chip other than the heating wire center region; the position, in the heating wire center region of the heating layer, of the silicon substrate of the bottom chip is separated from the other positions of the silicon substrate of the bottom chip other than the heating wire center region via the silicon nitride layer or silicon oxide layer; the liquid inlet and the liquid outlet are symmetrically disposed with respect to the second central window and communicate via the runner; the second central window is located in the center of the heating layer and is not shielded by a heating material; the insulating layer is disposed on the heating layer and covers an entirety of the heating layer except the four contact electrodes; and   an area of the top chip is smaller than an area of the bottom chip, the first central window of the top chip and second central window of the bottom chip are aligned, and a plurality of pores are provided in the first central window and the second central window.   
     
     
         2 . The transmission electron microscope in-situ liquid phase heating chip according to  claim 1 , wherein an external dimension of the bottom chip is 2 mm*2 mm-10 mm*10 mm. 
     
     
         3 . The transmission electron microscope in-situ liquid phase heating chip according to  claim 1 , wherein a thickness of the metal bonding layer is 50 nm-2000 nm, and the metal bonding layer is made of a metal having a melting point less than 1100° C. 
     
     
         4 . The transmission electron microscope in-situ liquid phase heating chip according to  claim 1 , wherein the metal bonding layer is made of In, Sn or Al. 
     
     
         5 . The transmission electron microscope in-situ liquid phase heating chip according to  claim 1 , wherein a thickness of the silicon substrate is 50 μm-500 μm. 
     
     
         6 . The transmission electron microscope in-situ liquid phase heating chip according to  claim 1 , wherein the first central window and the second central window are square central windows. 
     
     
         7 . The transmission electron microscope in-situ liquid phase heating chip according to  claim 1 , wherein the heating layer is set as two equivalent circuits, and the two equivalent circuits are controlled by separate current source meters and voltage source meters; one of the two equivalent circuits is used for supplying power to produce heat, and a second of the two equivalent circuits is used for monitoring a resistance value of the spiral annular heating wire after heating in real time; and
 the spiral annular heating wire is made of metallic gold, platinum, palladium, rhodium, molybdenum, tungsten, platinum-rhodium alloy or non-metallic molybdenum carbide.   
     
     
         8 . The transmission electron microscope in-situ liquid phase heating chip according to  claim 1 , wherein sizes of the liquid inlet and the liquid outlet are 200 μm*200 μm-1000 μm*1000 μm. 
     
     
         9 . The transmission electron microscope in-situ liquid phase heating chip according to  claim 1 , wherein a width of the support film is 10 nm-500 nm, and a thickness of the silicon nitride layer or the silicon oxide layer used as the support film is 200 nm-5 μm, and a structure of the support film is an approximate circle or square with the second central window as a center and having an inner diameter of 0.15 mm-0.5 mm.