CN112697824A - Multi-channel in-situ reaction cabin chip for in-situ transmission electron microscope and use method thereof - Google Patents
Multi-channel in-situ reaction cabin chip for in-situ transmission electron microscope and use method thereof Download PDFInfo
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- CN112697824A CN112697824A CN202011464394.8A CN202011464394A CN112697824A CN 112697824 A CN112697824 A CN 112697824A CN 202011464394 A CN202011464394 A CN 202011464394A CN 112697824 A CN112697824 A CN 112697824A
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- 238000011065 in-situ storage Methods 0.000 title claims abstract description 78
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 61
- 230000005540 biological transmission Effects 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 42
- 238000002474 experimental method Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- 239000000523 sample Substances 0.000 abstract description 66
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 abstract description 5
- 239000013074 reference sample Substances 0.000 abstract description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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Abstract
The invention discloses a multichannel in-situ reaction cabin chip for an in-situ transmission electron microscope, which belongs to the technical field of in-situ transmission electron microscopes and comprises two sets of in-situ reaction cabin systems integrated in one chip, wherein each set of in-situ reaction cabin system comprises a sample inlet, a transmission electron microscope observation window, a liquid outlet and a sample loading groove, and a passage is formed among the sample inlet, the liquid outlet and the sample loading groove. The invention also discloses a using method of the chip. The invention effectively utilizes the chip space of the original reaction cabin, integrates two sets of in-situ reaction cabin chip systems into one chip, and can realize the original transmission electron microscope observation of a plurality of samples. The cost of a single in-situ transmission electron microscope experiment is reduced, and the fault tolerance rate of the original transmission electron microscope experiment sample preparation is improved. Because the two samples are in the same chip, the invention can realize the simultaneous test of the sample to be tested and the reference sample, effectively eliminate the system error in the experiment and more truly reflect the intrinsic information of the sample.
Description
Technical Field
The invention belongs to the technical field of in-situ transmission electron microscopes, and particularly relates to a multi-channel in-situ reaction cabin chip for an in-situ transmission electron microscope.
Background
In recent years, in-situ reaction chamber (reaction cell) technology has been rapidly developed. In the in-situ reaction cabin technology, the original copper mesh micro-grid bearing sample is replaced by the in-situ reaction cabin through transforming a transmission electron microscope sample rod, and meanwhile, the reaction atmosphere is introduced into the closed in-situ reaction cabin, so that the effect of in-situ transmission electron microscope observation is achieved. Because the in-situ reaction cabin is isolated from the electron microscope vacuum chamber, the reaction atmosphere is limited in the reaction cabin, and the vacuum condition of the transmission electron microscope main cabin cannot be influenced. Therefore, the in-situ reaction cabin technology can obtain the microstructure change of the surface of the solid catalyst in the gas-solid catalytic reaction under the real reaction condition, and is helpful for deeply knowing and understanding the nature of the gas-solid catalytic reaction. However, the following problems still remain to be solved in the art: the in-situ reaction cabin chip relates to the field of micro processing, so that the manufacturing cost is high; the sample loading process relates to complex processes of diffusion, sedimentation and the like of particle samples in a solvent, and the rejection rate of sample preparation is high. Considering that the size of an observation area in a transmission electron microscope is almost negligible relative to an in-situ reaction cabin chip, a multichannel sample injection in-situ reaction cabin chip capable of simultaneously testing a plurality of transmission electron microscope samples is designed to solve the two problems.
Disclosure of Invention
The technical problems solved by the invention are as follows: the chip of the transmission electron microscope in-situ reaction cabin has the problems of high price and high rejection rate of sample preparation.
The technical scheme is as follows: in order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the utility model provides a multichannel normal position reaction cabin chip for normal position transmission electron microscope, includes two sets of normal position reaction cabin systems of integration in a chip, and every set of normal position reaction cabin system contains introduction port, transmission electron microscope observation window, liquid outlet and dress appearance groove, form the route between introduction port, liquid outlet and the dress appearance groove.
Preferably, the in-situ reaction cabin chip comprises an upper piece and a lower piece, the sample inlet, the transmission electron microscope observation window and the liquid outlet are arranged on the upper piece, the sample loading groove is arranged on the lower piece, and the transmission electron microscope observation window corresponding to the transmission electron microscope observation window of the upper piece is also arranged on the lower piece.
Preferably, the window of the transmission electron microscope observation window is sealed by a silicon nitride film.
Preferably, the two sample loading grooves are in a trapezoidal structure in a staggered arrangement.
Preferably, the area of the sample inlet is larger than that of the liquid outlet, and the transmission electron microscope observation window is positioned between the sample inlet and the liquid outlet.
Preferably, the total length from the sample inlet to the liquid outlet is 5 mm.
Preferably, the positions of the sample inlet and the liquid outlet of one set of in-situ reaction chamber system are opposite to those of the sample inlet and the liquid outlet of the other set of in-situ reaction chamber system.
A method for using a multi-channel in-situ reaction cabin chip for an in-situ transmission electron microscope is characterized in that an upper piece and a lower piece of the chip are attached to form a passage between a sample inlet and a sample outlet of the upper piece and a sample loading groove of the lower piece; and (3) dropwise adding the sample to the sample inlet, wherein the solvent can carry the sample to flow from the sample inlet to the liquid outlet, and the sample reaches the liquid outlet to complete sample introduction.
Preferably, the sample loading grooves of the two in-situ reaction cabin systems on the same chip are independent of each other, and the two in-situ transmission electron microscope experiments are simultaneously carried out.
Has the advantages that: compared with the prior art, the invention has the following advantages:
(1) the chip space of the original reaction cabin is effectively utilized, a plurality of in-situ reaction cabin passages are integrated into one chip, two transmission electron microscope samples can be tested simultaneously, and the two samples tested in the same group have comparability.
(2) The preparation process of the chip is not changed, the steps of secondary etching and the like are not required to be additionally introduced, the cost is basically not changed, but the number of samples which can be tested by each chip is increased. The cost required by a single original transmission electron microscope experiment is reduced, and the fault tolerance rate of sample preparation is improved.
(3) Because the two samples are in the same chip, the design can realize the simultaneous test of the sample to be tested and the reference sample, effectively eliminate the system error in the experiment and more truly reflect the intrinsic information of the sample.
Drawings
FIG. 1 is a schematic diagram of a chip-on-chip structure of a multi-channel in-situ reaction chamber for an in-situ transmission electron microscope;
FIG. 2 is a schematic view of a chip lower structure of a multi-channel in-situ reaction chamber for an in-situ transmission electron microscope;
FIG. 3 is a perspective view of a multi-channel in situ reaction chamber chip for use in an in situ transmission electron microscope;
FIG. 4 is a cross-sectional view of a multi-channel in-situ reaction chamber chip for in-situ transmission electron microscopy.
Detailed Description
The present invention will be further illustrated by the following specific examples, which are carried out on the premise of the technical scheme of the present invention, and it should be understood that these examples are only for illustrating the present invention and are not intended to limit the scope of the present invention.
As shown in fig. 1-3, a multi-channel in-situ reaction chamber chip for an in-situ transmission electron microscope, wherein two sets of in-situ reaction chamber systems are integrated in one chip, each set of in-situ reaction chamber system comprises a sample inlet 1, a transmission electron microscope observation window 2, a liquid outlet 3 and a sample containing groove 4, and a passage is formed among the sample inlet 1, the liquid outlet 3 and the sample containing groove 4. The in-situ reaction cabin chip comprises an upper piece 5 and a lower piece 6, wherein a sample inlet 1, a transmission electron microscope observation window 2 and a liquid outlet 3 are integrally arranged on the upper piece 5, a sample loading groove 4 is arranged on the lower piece 6, and the transmission electron microscope observation window 2 corresponding to the transmission electron microscope observation window 2 of the upper piece 5 is also arranged on the lower piece 6.
As shown in fig. 1, which is a schematic structural diagram of the upper plate 5, the area of the sample inlet 1 is larger than the area of the liquid outlet 3, the size of the sample inlet 1 is 1mm × 1mm, in order to balance the local pressure generated by the liquid droplets during sample injection, the size of the liquid outlet 3 is 100 μm × 100 μm, and the total length from the sample inlet 1 to the liquid outlet 3 is 5 mm.
As shown in fig. 1, the transmission electron microscope observation window 2 on the upper plate 5 is located between the sample inlet 1 and the liquid outlet 3. The window of the transmission electron microscope observation window 2 is sealed by a 10-nanometer thick silicon nitride film 7; the size of the observation window 2 of the transmission electron microscope is 30 μm by 30 μm. As shown in FIG. 2, a transmission electron microscope observation window 2 is also provided in the well 4 of the lower plate 6, and the window is closed with a silicon carbide thin film 7 having a thickness of 10 nm, corresponding to the transmission electron microscope observation window 2 of the upper plate 5 in position and having a size of 30 μm by 30 μm. The in-situ reaction cabin chip is made of silicon.
As shown in FIG. 2, in order to fully utilize the space, the two sample loading grooves 4 are in a trapezoidal structure which is arranged in a staggered mode. The sizes of two bottom edges of the trapezoid are respectively 100 mu m and 1mm, the height of the trapezoid is 5mm, and the depth of the two trapezoid sample loading grooves 4 is 1 mu m. After the upper plate 5 and the lower plate 6 are attached, the sample inlet 1 is positioned above one end edge of the trapezoidal sample containing groove 4, the liquid outlet 3 is positioned above the other end edge of the trapezoidal sample containing groove 4, and the total length from the sample inlet 1 to the liquid outlet 3 is 5 mm. The positions of the sample inlet 1 and the liquid outlet 3 of one set of in-situ reaction cabin system are opposite to the positions of the sample inlet 1 and the liquid outlet 3 of the other set of in-situ reaction cabin system, and the space of the chip is fully utilized.
A use method of a multi-channel in-situ reaction cabin chip for an in-situ transmission electron microscope is characterized in that when the chip is used, an upper piece 5 and a lower piece 6 of the chip are attached, so that a passage is formed among a sample inlet 1 and a liquid outlet 3 of the upper piece 5 and a sample containing groove 4 of the lower piece 6; the sample suspension liquid is dripped into the sample inlet 1, the solvent can bring the in-situ transmission electron microscope sample to flow to the liquid outlet 3 from the sample inlet 1, when the liquid outlet 3 sees the liquid, the sample reaches the liquid outlet 3, the sample suspension liquid is diffused to the whole sample loading groove 4, and the sample injection is completed. And then testing is carried out, the sample loading grooves 4 of the two in-situ reaction cabin systems on the same chip are independent, and the two in-situ transmission electron microscope experiments are simultaneously carried out. The method can realize the simultaneous test of the sample to be tested and the reference sample, effectively eliminate the system error in the experiment and truly reflect the intrinsic information of the sample. The in-situ transmission electron microscope observation of two samples can be carried out simultaneously, and the two samples tested in the same group are more comparable.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements should also be considered as the protection scope of the present invention.
Claims (9)
1. A multichannel in-situ reaction cabin chip for an in-situ transmission electron microscope is characterized by comprising: two sets of normal position reaction cabin systems of integrated in a chip, every set of normal position reaction cabin system contains introduction port (1), transmission electron microscope observation window (2), liquid outlet (3) and dress appearance groove (4), form the route between introduction port (1), liquid outlet (3) and dress appearance groove (4).
2. The multi-channel in-situ reaction chamber chip for the in-situ transmission electron microscope according to claim 1, wherein: the in-situ reaction cabin chip comprises an upper piece (5) and a lower piece (6), wherein a sample inlet (1), a transmission electron microscope observation window (2) and a liquid outlet (3) are arranged on the upper piece (5), a sample loading groove (4) is arranged on the lower piece (6), and the transmission electron microscope observation window (2) corresponding to the transmission electron microscope observation window (2) of the upper piece (5) is also arranged on the lower piece (6).
3. The multi-channel in-situ reaction chamber chip for the in-situ transmission electron microscope according to claim 1, wherein: the window of the transmission electron microscope observation window (2) is sealed by a silicon nitride film (7).
4. The multi-channel in-situ reaction chamber chip for the in-situ transmission electron microscope according to claim 1, wherein: the two sample loading grooves (4) are in a trapezoidal structure in staggered arrangement.
5. The multi-channel in-situ reaction chamber chip for the in-situ transmission electron microscope according to claim 1, wherein: the area of the sample inlet (1) is larger than that of the liquid outlet (3), and the transmission electron microscope observation window (2) is positioned between the sample inlet (1) and the liquid outlet (3).
6. The multi-channel in-situ reaction chamber chip for the in-situ transmission electron microscope according to claim 1, wherein: the total length from the sample inlet (1) to the liquid outlet (3) is 5 mm.
7. The multi-channel in-situ reaction chamber chip for the in-situ transmission electron microscope according to claim 1, wherein: the positions of a sample inlet (1) and a liquid outlet (3) of one set of in-situ reaction cabin system are opposite to the positions of a sample inlet (1) and a liquid outlet (3) of the other set of in-situ reaction cabin system.
8. A use method of a multi-channel in-situ reaction cabin chip for an in-situ transmission electron microscope is characterized by comprising the following steps: an upper piece (5) and a lower piece (6) of the chip are jointed, so that a passage is formed among a sample inlet (1) and a liquid outlet (3) of the upper piece (5) and a sample containing groove (4) of the lower piece (6); and (3) dropwise adding the sample into the sample inlet (1), wherein the solvent can drive the sample to flow to the liquid outlet (3) from the sample inlet (1), and the sample reaches the liquid outlet (3) to complete sample introduction.
9. The use method of the multi-channel in-situ reaction chamber chip for the in-situ transmission electron microscope according to claim 8, wherein the chip comprises: the sample loading grooves (4) of the two in-situ reaction cabin systems on the same chip are independent of each other, and the two in-situ transmission electron microscope experiments are simultaneously carried out.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011464394.8A CN112697824A (en) | 2020-12-11 | 2020-12-11 | Multi-channel in-situ reaction cabin chip for in-situ transmission electron microscope and use method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011464394.8A CN112697824A (en) | 2020-12-11 | 2020-12-11 | Multi-channel in-situ reaction cabin chip for in-situ transmission electron microscope and use method thereof |
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| CN112697824A true CN112697824A (en) | 2021-04-23 |
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| CN202011464394.8A Pending CN112697824A (en) | 2020-12-11 | 2020-12-11 | Multi-channel in-situ reaction cabin chip for in-situ transmission electron microscope and use method thereof |
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2020
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Application publication date: 20210423 |
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