CN114324417B - Device for reducing deformation of in-situ liquid cavity window in negative pressure environment - Google Patents
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Abstract
The invention relates to a device for reducing deformation of an in-situ liquid cavity window in a negative pressure environment, which comprises: the liquid medium input end, the negative pressure system, the liquid sample rod, the liquid cavity and the liquid medium output end; the liquid cavity is arranged on the liquid sample rod, and the internal liquid medium channel is communicated with the liquid sample rod; the liquid medium input end is connected with the input end of the liquid sample rod through the first connecting pipe and is used for inputting the liquid medium into the liquid cavity; the negative pressure system is used for enabling the pressure of the liquid cavity to be in a negative pressure state; the liquid medium output end is connected with the output end of the liquid sample rod through a second connecting pipe and is used for outputting liquid medium in the liquid cavity. By the method, the pressure in the liquid cavity can be reduced from the atmospheric pressure to the negative pressure, and adverse effects caused by deformation of the in-situ liquid cavity window in a negative pressure environment are reduced.
Description
Technical Field
The invention relates to the field of transmission electron microscope characterization test, in particular to a device for reducing deformation of an in-situ liquid cavity window in a negative pressure environment.
Background
Many important reactions in physics, chemistry and biology are carried out in aqueous solutions, and imaging of the subject in liquid media is highly desirable to better understand these reactions at the atomic and molecular level.
In recent years, with development of micro-nano processing technology and transmission electron microscope, in-situ liquid environment transmission electron microscope has become a conventional means for carrying out nano-scale research on liquid samples, the liquid samples are sealed through two layers of silicon nitride films or graphene films and carbon films, liquid cavities are formed and fixed on the heads of common sample rods or special liquid sample rods, and the liquid cavities are placed into electron microscope vacuum columns for observation, so that dynamic processes in the solution can be directly displayed in real time. The development of in-situ liquid environment transmission electron microscopy expands the research scope of the transmission electron microscopy from structural characterization and elemental analysis of solid samples to in-situ observation of nanomaterial behavior in the liquid environment, such as nucleation and growth of nanomaterials, self-assembly behavior of nanocrystals, etching and dissolution of nanocrystals, and structural evolution of nanocrystals under external condition excitation.
Because of the short development time, the in-situ liquid environment transmission electron microscope technology still has much room for improvement. When an in-situ liquid transmission electron microscope images a sample, incident electrons can pass through a window material and a liquid layer to cause electron scattering, so that the imaging resolution of the transmission electron microscope can be influenced, and the thicker the thicknesses of the window material and the liquid layer, the lower the resolution. To increase resolution, researchers have proposed reducing the thickness of window films and liquids as much as possible to reduce electron scattering. For example, zheng et al reduce the window film to 25nm, liquid layer to 200nm (Zheng H, et al, observation ofsingle colloidalplatinumnanocrystal growth trajectories. Science,2009,324 (5932):1309-1312) and Liao et al reduce the window film to 13nm with resolution up to atomic scale (Liao H G, et al, nanoparticle growth.facet development duringplatinumnanocube growth.science,2014,345 (6199):916-919).
In addition to the above-described relatively thick window film and liquid layer, which can reduce the resolution of transmission electron microscopy imaging, a problem is associated. The pressure in the liquid cavity is about 1bar, and in a vacuum environment, the film can bulge outwards due to the difference between the internal pressure and the external pressure, so that the thickness of the liquid layer is thickened, the electron scattering is increased, and the spatial resolution and the service life of a chip are reduced.
Therefore, how to design a device capable of reducing deformation of the in-situ liquid chamber window in a negative pressure environment is a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to provide a device capable of reducing deformation of an in-situ liquid cavity window in a negative pressure environment.
In order to achieve the above object, the present invention provides the following solutions:
an apparatus for reducing deformation of an in-situ liquid chamber window in a negative pressure environment, the apparatus comprising: the liquid medium input end, the negative pressure system, the liquid sample rod, the liquid cavity and the liquid medium output end;
the liquid cavity is arranged on the liquid sample rod, and the internal liquid medium channel is communicated with the liquid sample rod;
the liquid medium input end is connected with the input end of the liquid sample rod through a first connecting pipe and is used for inputting liquid medium into the liquid cavity;
the negative pressure system is used for enabling the pressure of the liquid cavity to be in a negative pressure state;
the liquid medium output end is connected with the output end of the liquid sample rod through a second connecting pipe and is used for outputting the liquid medium in the liquid cavity.
Optionally, the negative pressure system includes: the system comprises a first vacuum pump, a second vacuum pump, a first pressure sensor, a second pressure sensor and a vacuum pump pressure controller; the first connection pipe includes: a third connecting pipe, a fourth connecting pipe and a fifth connecting pipe; the second connection pipe includes: a sixth connection pipe, a seventh connection pipe, and an eighth connection pipe;
the first vacuum pump is connected with the liquid medium input end through the third connecting pipe and is connected with the input end of the first pressure sensor through the fourth connecting pipe;
the output end of the first pressure sensor is connected with the input end of the liquid sample rod through a fifth connecting pipe;
the input end of the second pressure sensor is connected with the output end of the liquid sample rod through a sixth connecting pipe;
the second vacuum pump is connected with the output end of the second pressure sensor through a seventh connecting pipe and is connected with the liquid medium output end through an eighth connecting pipe;
and the vacuum pump pressure controller is electrically connected with the first vacuum pump and the second vacuum pump respectively and is used for setting the pressure of the first vacuum pump and the second vacuum pump.
Optionally, the liquid cavity is a flowing liquid cavity.
Optionally, the liquid cavity comprises an upper chip and a lower chip; the upper chip and the lower chip are arranged in parallel and aligned, and a liquid medium channel is arranged between the upper chip and the lower chip.
Optionally, the upper chip and the lower chip are both provided with thin film windows.
Optionally, the thin film window is made of an electron beam transparent material.
Optionally, the first vacuum pump is one of a piston vacuum pump, a liquid ring vacuum pump, a rotary vane vacuum pump, a stator vane vacuum pump, a slide valve vacuum pump, a dry vacuum pump, a molecular vacuum pump or a compound vacuum pump.
Optionally, the second vacuum pump is one of a piston vacuum pump, a liquid ring vacuum pump, a rotary vane vacuum pump, a stator vane vacuum pump, a slide valve vacuum pump, a dry vacuum pump, a molecular vacuum pump or a compound vacuum pump.
Optionally, the first pressure sensor is a vacuum pressure gauge or a vacuum degree tester.
Optionally, the second pressure sensor is a vacuum pressure gauge or a vacuum degree tester.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention provides a device for reducing deformation of an in-situ liquid cavity window in a negative pressure environment, which is characterized in that a negative pressure system is connected to a liquid sample rod, so that the pressure in the liquid cavity can be reduced from the atmosphere to the negative pressure, the bending deformation of the liquid cavity under the action of pressure difference and the thickness change of the liquid layer caused by the bending deformation are reduced, and the scattering of electrons generated when the electrons pass through the liquid layer are reduced, thereby improving the spatial resolution of an in-situ liquid transmission electron microscope and simultaneously improving the reliability of an in-situ liquid chip.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of a device for reducing deformation of an in-situ liquid chamber window in a negative pressure environment according to embodiment 1 of the present invention;
fig. 2 is a cross-sectional view of a liquid chamber.
Symbol description:
1. a liquid medium input; 2. a first vacuum pump; 3. a first pressure sensor; 4. a liquid sample rod; 5. a liquid chamber; 6. a second pressure sensor; 7. a second vacuum pump; 8. a liquid medium output; 9. a vacuum pump pressure controller; 10. a third connection pipe; 11. a fourth connecting pipe, 12 and a fifth connecting pipe; 13. a sixth connection pipe; 14. a seventh connection pipe; 15. an eighth connection pipe; 16. an upper chip; 17. a lower chip; 18. an upper film window; 19. a lower film window; 20. a liquid medium; 21. a film.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention aims to provide a device capable of reducing deformation of an in-situ liquid cavity window in a negative pressure environment.
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of the invention will be rendered by reference to the appended drawings and appended detailed description.
Example 1:
referring to fig. 1, the present invention provides an apparatus for reducing deformation of an in-situ liquid chamber window in a negative pressure environment, the apparatus comprising: a liquid medium input end 1, a negative pressure system, a liquid sample rod 4, a liquid cavity 5 and a liquid medium output end 8;
the liquid cavity 5 is arranged on the liquid sample rod 4, and an internal liquid medium channel is communicated with the liquid sample rod 4;
the liquid medium input end 1 is connected with the input end of the liquid sample rod 4 through a first connecting pipe and is used for inputting liquid medium into the liquid cavity 5;
the negative pressure system is used for enabling the pressure of the liquid cavity 5 to be in a negative pressure state;
in this embodiment, the negative pressure system includes: a first vacuum pump 2, a second vacuum pump 7, a first pressure sensor 3, a second pressure sensor 6, and a vacuum pump pressure controller 9; the first connection pipe includes: a third connection pipe 10, a fourth connection pipe 11, and a fifth connection pipe 12; the second connection pipe includes: a sixth connecting pipe 13, a seventh connecting pipe 14, and an eighth connecting pipe 15;
the first vacuum pump 2 is connected with the liquid medium input end 1 through the third connecting pipe 10 and is connected with the input end of the first pressure sensor 3 through a fourth connecting pipe 11;
the output end of the first pressure sensor 3 is connected with the input end of the liquid sample rod 4 through a fifth connecting pipe 12;
the input end of the second pressure sensor 6 is connected with the output end of the liquid sample rod 4 through a sixth connecting pipe 13;
the second vacuum pump 7 is connected with the output end of the second pressure sensor 6 through a seventh connecting pipe 14 and is connected with the liquid medium output end 8 through an eighth connecting pipe 15;
the vacuum pump pressure controller 9 is electrically connected to the first vacuum pump 2 and the second vacuum pump 7, respectively, and is configured to set the pressures of the first vacuum pump 2 and the second vacuum pump 7.
The liquid medium output end 8 is connected with the output end of the liquid sample rod 4 through a second connecting pipe and is used for outputting the liquid medium in the liquid cavity 5.
Specifically, the liquid chamber 5 is a flowing liquid chamber, so that the reactant can be precisely controlled.
As shown in fig. 2, the liquid chamber 5 includes an upper chip 16 and a lower chip 17; wherein the upper chip 16 and the lower chip 17 are aligned in parallel, and a liquid medium channel is provided between the upper chip 16 and the lower chip 17.
As shown in fig. 2, the upper chip 16 is provided with a silicon nitride upper film window 18; the lower chip 17 is provided with a silicon nitride lower film window 19, wherein the dimensions of the upper film window 18 and the lower film window 19 are 50×50 μm.
Specifically, the upper film window 18 and the lower film window 19 are both made of an electron beam transparent material, including but not limited to one of silicon nitride, graphene, and carbon.
As one possible implementation, the first vacuum pump 2 is one of a piston vacuum pump, a liquid ring vacuum pump, a rotary vane vacuum pump, a stator-type vacuum pump, a slide valve vacuum pump, a dry vacuum pump, a molecular vacuum pump, or a compound vacuum pump. The second vacuum pump 7 is one of a piston vacuum pump, a liquid ring vacuum pump, a rotary vane vacuum pump, a stator vacuum pump, a slide valve vacuum pump, a dry vacuum pump, a molecular vacuum pump or a compound vacuum pump.
In this embodiment, the first vacuum pump 2 and the second vacuum pump 7 are piston vacuum pumps, which have the advantages of low power consumption, small floor space and long service life.
As a possible implementation, the first pressure sensor 3 is a vacuum pressure gauge or a vacuum degree tester. The second pressure sensor 6 is a vacuum pressure gauge or a vacuum degree tester.
In this embodiment, the first pressure sensor 3 and the second pressure sensor 6 are vacuum pressure gauges, and the measuring range is from atmosphere to 10 -3 The mbar has the advantages of analog and digital dual display and multiple pressure unit switching, and the corrosion-resistant material is adopted for the contact part with the gas, so that the mbar can stably work for a long time.
In addition, as one possible implementation, the vacuum pump pressure controller 9 includes, but is not limited to, one of a small pump controller, a multiple pump controller, and the like.
In this embodiment, the vacuum pump pressure controller 9 is a Digitel MPC multi-pump controller, and may control different types of vacuum pumps.
According to the invention, the negative pressure system is connected to the liquid sample rod, so that the pressure in the liquid cavity can be reduced from atmospheric pressure to negative pressure, the bending deformation of the liquid cavity under the action of pressure difference and the thickness change of the liquid layer caused by the bending deformation are reduced, and the scattering of electrons generated when the electrons pass through the liquid layer is reduced, so that the spatial resolution of the in-situ liquid transmission electron microscope is improved, and the reliability of the in-situ liquid chip is improved.
Example 2:
in order to facilitate the understanding of the present invention, a method of reducing deformation of an in situ liquid chamber window in a negative pressure environment is described. The method comprises the following steps:
step one: assembly of a negative pressure system
(1) A liquid cavity 5 with a silicon nitride film window is arranged on a liquid sample rod 4, the liquid cavity 5 is formed by parallel alignment and combination of an upper chip and a lower chip, a liquid medium channel is reserved in the middle, the window size is 50 multiplied by 50 mu m, and then the liquid sample rod 4 is placed in an in-situ liquid transmission electron microscope vacuum column.
(2) The first vacuum pump 2 (piston vacuum pump) is connected to the liquid medium input 1 via a third connection pipe 10, to the first pressure sensor 3 (vacuurand vacuum pressure gauge) via a fourth connection pipe 11, and to the in-situ liquid transmission electron microscope sample rod via a fifth connection pipe 12, the vacuurand vacuum pressure gauge measuring in a range from atmospheric to 10 -3 The mbar has the advantages of analog and digital dual display and multiple pressure unit switching, and the parts contacted with the gas are made of corrosion-resistant materials, so that the pressure-sensitive gas sensor can stably work for a long time.
(3) The second vacuum pump 7 (piston vacuum pump) is connected to the liquid medium outlet 8 via a sixth connection pipe 13, to the second pressure sensor 6 (vacuurand vacuum pressure gauge) via a seventh connection pipe 14, and to the in-situ liquid transmission electron microscope sample rod via an eighth connection pipe 15.
(4) The first vacuum pump 2 and the second vacuum pump 7 are connected to a DigitelMPC multi-pump controller, so that the regulation and control of the liquid cavity pressure are realized.
Step two: application method of negative pressure system
(1) And checking the tightness of connecting pipes among all components of the negative pressure system, and judging whether the negative pressure system can work normally.
(2) The pressures of the first vacuum pump 2 and the second vacuum pump 7 are respectively set in a vacuum pump control system of the Digitel MPC multi-pump controller, so that the pressures of the first vacuum pump 2 and the second vacuum pump 7 are ensured to be the same.
(3) The Digitel MPC multi-pump controller controls the first vacuum pump 2 and the second vacuum pump 7 to operate simultaneously, and when the negative pressure generated by the first vacuum pump 2 and the second vacuum pump 7 is equal, the liquid in the liquid cavity is in a static state due to no pressure difference between the liquid medium input end 1 and the liquid medium output end 8.
(4) The vacuum pump control system of the Digitel MPC multi-pump controller is respectively provided with the pressures of the first vacuum pump 2 and the second vacuum pump 7, so that the negative pressure of the first vacuum pump 2 is lower than that of the second vacuum pump 7, therefore, a pressure difference is formed between the liquid medium input end 1 and the liquid medium output end 8, the liquid in the liquid cavity 5 is in a flowing state, then the reaction process between in-situ observation can be carried out through a transmission electron microscope, and the flowing direction of the liquid in the liquid cavity is shown as a figure 2.
Example 3:
a method for reducing deformation of an in-situ liquid chamber window in a negative pressure environment, comprising the following steps:
step one: measuring liquid layer thickness when liquid sample rod 4 is not connected to a negative pressure system
(1) A liquid chamber 5 with a silicon nitride film window is arranged on a liquid sample rod 4, the liquid chamber 5 is formed by parallel alignment and combination of an upper chip 16 and a lower chip 17, a liquid medium channel is reserved in the middle, the window size is 50 multiplied by 50 mu m, and then the liquid sample rod 4 is placed in an in-situ liquid transmission electron microscope vacuum column.
(2) The liquid medium inlet 1 and the liquid medium outlet 8 are connected to the liquid sample rod 4 via connecting lines, respectively, and the liquid layer thickness is measured using EELS, which is approximately 100nm when the negative pressure system is not connected.
Step two: measuring liquid layer thickness when liquid sample rod 4 is connected to negative pressure system
(1) Example 2 was repeated, and a negative pressure system was installed, and the pressures of the first vacuum pump 2 and the second vacuum pump 7 were set in the vacuum pump control system of the Digitel MPC multi-pump controller, respectively, so that the negative pressure of the first vacuum pump 2 was lower than the negative pressure of the second vacuum pump 7.
(2) The liquid layer thickness is measured through EELS, and when the liquid sample rod 4 is connected with the negative pressure system, the liquid layer thickness is about 30nm, so that the thickness of the liquid layer is greatly reduced, the scattering of electrons generated when passing through the liquid layer is reduced, and the spatial resolution of the in-situ liquid transmission electron microscope and the reliability of the in-situ liquid chip are improved.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other.
The principles and embodiments of the present invention have been described herein with reference to specific examples, the description of which is intended only to assist in understanding the methods of the present invention and the core ideas thereof; also, it is within the scope of the present invention to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the invention.
Claims (9)
1. A device for reducing deformation of an in-situ liquid chamber window in a negative pressure environment, comprising: the liquid medium input end, the negative pressure system, the liquid sample rod, the liquid cavity and the liquid medium output end;
the liquid cavity is arranged on the liquid sample rod, and the internal liquid medium channel is communicated with the liquid sample rod;
the liquid medium input end is connected with the input end of the liquid sample rod through a first connecting pipe and is used for inputting liquid medium into the liquid cavity;
the negative pressure system is used for enabling the pressure of the liquid cavity to be in a negative pressure state;
the liquid medium output end is connected with the output end of the liquid sample rod through a second connecting pipe and is used for outputting the liquid medium in the liquid cavity;
the negative pressure system includes: the system comprises a first vacuum pump, a second vacuum pump, a first pressure sensor, a second pressure sensor and a vacuum pump pressure controller; the first connection pipe includes: a third connecting pipe, a fourth connecting pipe and a fifth connecting pipe; the second connection pipe includes: a sixth connection pipe, a seventh connection pipe, and an eighth connection pipe;
the first vacuum pump is connected with the liquid medium input end through the third connecting pipe and is connected with the input end of the first pressure sensor through the fourth connecting pipe;
the output end of the first pressure sensor is connected with the input end of the liquid sample rod through a fifth connecting pipe;
the input end of the second pressure sensor is connected with the output end of the liquid sample rod through a sixth connecting pipe;
the second vacuum pump is connected with the output end of the second pressure sensor through a seventh connecting pipe and is connected with the liquid medium output end through an eighth connecting pipe;
and the vacuum pump pressure controller is electrically connected with the first vacuum pump and the second vacuum pump respectively and is used for setting the pressure of the first vacuum pump and the second vacuum pump.
2. A device for reducing deformation of an in-situ liquid chamber window in a negative pressure environment as defined in claim 1, wherein the liquid chamber is a flowable liquid chamber.
3. The apparatus for reducing deformation of an in-situ liquid chamber window in a negative pressure environment of claim 1, wherein the liquid chamber comprises an upper die and a lower die; the upper chip and the lower chip are arranged in parallel and aligned, and a liquid medium channel is arranged between the upper chip and the lower chip.
4. A device for reducing deformation of an in-situ liquid chamber window in a negative pressure environment as set forth in claim 3, wherein said upper die and said lower die are each provided with a thin film window.
5. The apparatus of claim 4 wherein said thin film window is an electron beam transparent material.
6. The apparatus of claim 1, wherein the first vacuum pump is one of a piston vacuum pump, a liquid ring vacuum pump, a rotary vane vacuum pump, a stator vane vacuum pump, a slide valve vacuum pump, a dry vacuum pump, a molecular vacuum pump, or a compound vacuum pump.
7. The apparatus of claim 1, wherein the second vacuum pump is one of a piston vacuum pump, a liquid ring vacuum pump, a rotary vane vacuum pump, a stator vane vacuum pump, a slide valve vacuum pump, a dry vacuum pump, a molecular vacuum pump, or a compound vacuum pump.
8. The apparatus for reducing deformation of an in-situ liquid chamber window in a negative pressure environment of claim 1, wherein the first pressure sensor is a vacuum gauge or a vacuum tester.
9. The apparatus for reducing deformation of an in-situ liquid chamber window in a negative pressure environment of claim 1, wherein the second pressure sensor is a vacuum gauge or a vacuum tester.
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