CN109765255B - Detection and maintenance method of near-normal-pressure XPS system - Google Patents
Detection and maintenance method of near-normal-pressure XPS system Download PDFInfo
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- CN109765255B CN109765255B CN201910056860.XA CN201910056860A CN109765255B CN 109765255 B CN109765255 B CN 109765255B CN 201910056860 A CN201910056860 A CN 201910056860A CN 109765255 B CN109765255 B CN 109765255B
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Abstract
The invention provides a detection and maintenance method of a near-normal-pressure XPS system, which comprises the following steps: aligning a powder sample in the reaction cavity to an information acquisition port of a near-normal pressure XPS system, and detecting the powder sample; after the detection is finished, the air pressure in the reaction cavity and/or the air pressure in the collection cavity are/is adjusted, so that the air pressure in the collection cavity is larger than the air pressure in the reaction cavity, the information collection port and the powder in the collection cavity are adsorbed to the reaction cavity, and the collection cavity is communicated with the information collection port. According to the detection and maintenance method of the near-normal-pressure XPS system, after the powder sample is detected, the air pressure in the reaction cavity and/or the air pressure in the collection cavity are/is adjusted, so that the air pressure in the collection cavity is larger than the air pressure in the reaction cavity, the powder sample in the information collection port and the collection cavity is adsorbed into the reaction cavity by utilizing the air pressure difference between the collection cavity and the reaction cavity, the removal process is simplified, and the removal efficiency is improved.
Description
Technical Field
The invention relates to the technical field of XPS system detection, in particular to a detection and maintenance method of a near-normal-pressure XPS system.
Background
X-ray photoelectron spectroscopy (XPS) uses X-rays to irradiate a sample, and excites the inner electrons or valence electrons of atoms or molecules. The electrons excited by photons are called photoelectrons, the energy of the photoelectrons can be measured, the kinetic energy of the photoelectrons is used as a horizontal coordinate, the relative intensity (pulse/s) is used as a vertical coordinate, and a photoelectron energy spectrogram can be made, so that the information of a sample to be measured can be obtained. The near-normal pressure XPS system is characterized in that a three-stage molecular pump differential system is added between an electron lens and an energy analyzer, so that the environmental pressure of a detection sample can be greatly increased. Therefore, the near-normal pressure XPS system can carry out real-time in-situ analysis on chemical components, oxidation states and electronic structures of solid-gas and liquid-gas interfaces under the atmosphere of near normal pressure. However, in the process of monitoring the catalytic reaction of the powder catalyst in real time, the collection chamber for collecting the sample information is usually in an ultrahigh vacuum environment, while the reaction chamber for performing the catalytic reaction is in a high-temperature high-pressure environment, and because a huge pressure difference exists between the reaction chamber and the collection chamber, the information collection port communicated with the sampling chamber is easy to suck the powder sample and block, so that the information collection port cannot work. The existing method for cleaning the powder sample of the information acquisition port usually needs to disassemble the information acquisition port from the acquisition cavity, the whole cleaning process is complex, and the cleaning efficiency is low.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a detection and maintenance method of a near-normal-pressure XPS system, which is used for directly clearing the powder sample of an information acquisition port under the condition of not dismantling the information acquisition port after the powder sample is detected, so that the clearing process is simplified, and the clearing efficiency is improved.
The specific technical scheme provided by the invention is as follows: the detection and maintenance method of the near-normal pressure and near-normal pressure XPS system is provided, and comprises the following steps:
aligning a powder sample in a reaction cavity to an information acquisition port of the near-normal pressure XPS system, and detecting the powder sample;
after the detection is finished, the air pressure in the reaction cavity and/or the air pressure in the collection cavity are/is adjusted to enable the air pressure in the collection cavity to be larger than the air pressure in the reaction cavity, so that the information collection port and the powder in the collection cavity are adsorbed into the reaction cavity, and the collection cavity is communicated with the information collection port.
Further, adjusting the gas pressure in the reaction chamber and/or the gas pressure in the collection chamber such that the gas pressure in the collection chamber is greater than the gas pressure in the reaction chamber specifically includes:
pressurizing the collection chamber such that a gas pressure in the collection chamber is greater than a gas pressure in the reaction chamber.
Further, adjusting the gas pressure in the reaction chamber and/or the gas pressure in the collection chamber such that the gas pressure in the collection chamber is greater than the gas pressure in the reaction chamber specifically includes:
and vacuumizing the reaction cavity to ensure that the air pressure in the collection cavity is greater than the air pressure in the reaction cavity.
Further, the reaction chamber is vacuumized, and the detection and maintenance method further comprises: and introducing near-atmospheric gas into the acquisition cavity, wherein the gas pressure of the near-atmospheric gas is not less than 100 mbar.
Further, the near-atmospheric gas is an inert gas.
Further, the air pressure in the collection cavity is at least 1 x 10 of the air pressure in the reaction cavity6And (4) doubling.
Further, the diameter of the information acquisition port is 300 um.
Further, the distance between the information collecting port and the powder sample is not more than 40 mm.
Further, in the case where in-situ detection of the powder sample is not required, the detection and maintenance method further comprises: a baffle is inserted between the powder sample and the information acquisition port to shield the powder sample.
According to the detection and maintenance method of the near-normal-pressure XPS system, after a powder sample is detected, the air pressure in the reaction cavity and/or the air pressure in the acquisition cavity are/is adjusted to enable the air pressure in the acquisition cavity to be larger than the air pressure in the reaction cavity, and the powder in the information acquisition port and the powder in the acquisition cavity are adsorbed into the reaction cavity by utilizing the air pressure difference between the acquisition cavity and the reaction cavity, so that the powder blockage of the information acquisition port is directly cleared without dismantling the information acquisition port, the clearing process is simplified, and the clearing efficiency is improved.
Drawings
The technical solution and other advantages of the present invention will become apparent from the following detailed description of specific embodiments of the present invention, which is to be read in connection with the accompanying drawings.
FIG. 1 is a schematic diagram of the structure of an electron lens system of a near atmospheric XPS system;
FIG. 2 is a schematic view of the structure of the information acquisition port and the single crystal sample;
FIG. 3 is a flow chart of a method for detecting and maintaining a near-atmospheric XPS system.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the specific embodiments set forth herein. Rather, these embodiments are provided to explain the principles of the invention and its practical application to thereby enable others skilled in the art to understand the invention for various embodiments and with various modifications as are suited to the particular use contemplated. In the drawings, like reference numerals will be used to refer to like elements throughout.
The detection and maintenance method of the near-normal-pressure XPS system provided by the embodiment comprises the following steps:
aligning a powder sample in the reaction cavity to an information acquisition port of a near-normal pressure XPS system, and detecting the powder sample;
after the detection is finished, the air pressure in the reaction cavity and/or the air pressure in the collection cavity are/is adjusted, so that the air pressure in the collection cavity is larger than the air pressure in the reaction cavity, the information collection port and the powder in the collection cavity are adsorbed to the reaction cavity, and the collection cavity is communicated with the information collection port.
This embodiment is through the atmospheric pressure of adjusting in the reaction chamber and/or gathering the atmospheric pressure in the chamber for gather the atmospheric pressure in the chamber and be greater than the atmospheric pressure in the reaction chamber, utilize the atmospheric pressure difference between gathering chamber and the reaction chamber to adsorb the powder in information acquisition mouth and the collection chamber to the reaction chamber, thereby directly clear away the powder that blocks up the information acquisition mouth under the condition of not demolising the information acquisition mouth, simplified the clearance process, promoted and cleared away efficiency.
Referring to fig. 1 and 2, the near-normal pressure XPS system provided by the present embodiment includes a three-stage differential pumping system 1, an energy analyzer 216, and an electron lens system 3. The electron lens system 3 is used to collect information of the powder sample and send the collected information of the powder sample to the energy analyzer 2 for analysis. The three-stage differential pumping system 1 comprises three cavities equipped with molecular pumps, which are respectively a first cavity 11, a second cavity 12 and a third cavity 13. The first cavity 11 is communicated with the information acquisition port 14, and the second cavity 12 is connected between the first cavity 11 and the third cavity 13. The electronic lens system 3 is located in the first cavity 11 and is opposite to the information acquisition port 14. The three-stage differential pumping system further comprises a valve 15 arranged between the first cavity 11 and the second cavity 12, wherein the valve 15 is a metal angle valve and is used for controlling the connection and disconnection between the first cavity 11 and the second cavity 12 as well as between the first cavity 11 and the third cavity 13, and the first cavity 11 is a collection cavity.
Referring to fig. 3, a detailed description is given below of a detection and maintenance method of the near-normal pressure XPS system in the present embodiment, the detection and maintenance method including the steps of:
and S1, aligning the powder sample in the reaction cavity to the information acquisition port 14 of the near-normal pressure XPS system, and detecting the powder sample.
In step S1, the position of the powder sample in the reaction chamber is first adjusted so that the powder sample in the reaction chamber is aligned with the information collection port 14 of the near-atmospheric XPS system, and the distance between the information collection port 14 and the powder sample is not more than 40 mm. The distance between the information collection port 14 and the powder sample is the optimum distance to obtain the strongest signal of the powder sample.
When the powder sample is detected, the valve 15 is in an open state, the first cavity 11, the second cavity 12 and the third cavity 13 are communicated, and the molecular pumps equipped in the first cavity 11, the second cavity 12 and the third cavity 13 vacuumize the first cavity 11, the second cavity 12 and the third cavity 13, so that the first cavity 11, the second cavity 12 and the third cavity 13 are all in an ultrahigh vacuum environment, for example, the air pressure in the first cavity 11, the second cavity 12 and the third cavity 13 is 1 gamma 10-5mbar. The powder sample in the reaction chamber is at near atmospheric pressure, e.g. the gas pressure in the reaction chamber is 10mbar, the gas pressure in the reaction chamber is 1 gamma 10 of the gas pressure in the collection chamber, i.e. the first chamber 116At this time, due to the air pressure difference between the reaction chamber and the collection chamber, a small amount of the powder sample in the reaction chamber will be adsorbed to the collection chamber, i.e. the first chamber 11 and the information collection port 14.
And S2, after the detection is finished, adjusting the air pressure in the reaction cavity and/or the air pressure in the collection cavity, so that the air pressure in the collection cavity, namely the first cavity 11, is larger than the air pressure in the reaction cavity, and the powder samples in the information collection port 14 and the collection cavity are adsorbed into the reaction cavity.
Referring to fig. 2, in order to facilitate observation of the removal of the powder sample, after the detection is completed, the powder sample is replaced with a single crystal sample, wherein the center of the single crystal sample is opposite to the information collection port 14, and the distance between the single crystal sample and the information collection port 14 is the best to see the information collection port reflection from the surface of the single crystal sample. The air pressure in the reaction cavity and/or the air pressure in the collection cavity are/is adjusted, so that the air pressure in the collection cavity, namely the first cavity 11, is larger than the air pressure in the reaction cavity, the powder samples in the information collection port 14 and the collection cavity are adsorbed into the reaction cavity and fall on the surface of the single crystal sample, and therefore the single crystal sample only needs to be taken out and the powder sample on the surface of the single crystal sample is cleaned.
In step S2, since the filter screen is disposed between the first chamber 11 and the second chamber 12, the dust is only accumulated in the first chamber 11 and on the information collecting port 14 during the detection process. After the detection is completed, the valve 15 is closed and the molecular pump configured in the first cavity 11 is closed, at this time, only the air pressure in the reaction cavity and/or the air pressure in the first cavity 11 is adjusted so that the air pressure in the first cavity 11 is greater than the air pressure in the reaction cavity, and the powder in the first cavity 11 and on the information acquisition port 14 is adsorbed into the reaction cavity and falls on the surface of the single crystal sample through the air pressure difference between the reaction cavity and the first cavity 11.
Adjusting the gas pressure in the reaction chamber and/or the gas pressure in the collection chamber may be by adjusting the gas pressure in the reaction chamber such that the gas pressure in the collection chamber, i.e. the first chamber body 11, is greater than the gas pressure in the reaction chamber. Because the atmospheric pressure in reaction chamber is greater than the atmospheric pressure of gathering the chamber, at this moment, need gather the chamber and pressurize to the atmospheric pressure in making gathering the chamber is greater than the atmospheric pressure in the reaction chamber. Specifically, the pressure in the reaction chamber is maintained unchanged, and high-pressure gas is introduced into the first chamber 11, so that the pressure in the first chamber 11 is greater than the pressure in the reaction chamber.
Adjusting the gas pressure in the reaction chamber and/or the gas pressure in the collection chamber may be by adjusting the gas pressure in the reaction chamber such that the gas pressure in the collection chamber, i.e. the first chamber body 11, is greater than the gas pressure in the reaction chamber. At this time, the reaction chamber needs to be depressurized so that the pressure in the collection chamber is greater than the pressure in the reaction chamber. Specifically, the air pressure in the first cavity 11 is maintained unchanged, the reaction cavity is vacuumized by an external molecular pump, and the reaction cavity is in an ultrahigh vacuum environment, so that the air pressure in the first cavity 11 is greater than the air pressure in the reaction cavity.
Adjusting the gas pressure in the reaction chamber and/or the gas pressure in the collection chamber can be done by adjusting the gas pressure in the collection chamber and the reaction chamber simultaneously, so that the gas pressure in the collection chamber, i.e. the first chamber 11, is also greater than the gas pressure in the reaction chamber. At this time, the pressure of the collection chamber is increased while the pressure of the reaction chamber is decreased, so that the pressure of the collection chamber is greater than the pressure of the reaction chamber. Specifically, the reaction cavity is vacuumized by an external molecular pump, the reaction cavity is in an ultrahigh vacuum environment, and then near-normal-pressure gas is introduced into the first cavity 11, wherein the near-normal-pressure gas refers to gas with the gas pressure not less than 100mbar, so that the gas pressure in the first cavity 11 is greater than the gas pressure in the reaction cavity.
The step of introducing near-atmospheric pressure gas into the first cavity 11 specifically comprises: and closing a driving motor of the molecular pump configured in the first cavity 11, and introducing near-normal-pressure gas into the first cavity 11 through the air inlet of the molecular pump in the speed reduction process of the molecular pump until the rotating speed of the molecular pump is zero, wherein at the moment, the first cavity 11 is filled with the near-normal-pressure gas. Since the first chamber 11, the second chamber 12, and the third chamber 13 need to be in an ultra-high vacuum environment during the detection process, the chamber environment needs to be as clean as possible, and the inert gas is not easily adsorbed on the chamber wall, it is preferable that the near-normal-pressure gas in this embodiment is an inert gas, for example, the near-normal-pressure gas is nitrogen or argon.
In order to sufficiently adsorb dust in the collection chamber and on the information collection port 14 into the reaction chamber, the pressure in the collection chamber in this embodiment is at least 1 gamma 10 of the pressure in the reaction chamber6And (4) doubling. For example, the gas pressure in the collection chamber is 100mbar, and the gas pressure in the reaction chamber is gamma 10-4mbar。
The diameter of the information acquisition port 14 in this embodiment example is 300um, and the size of the atmospheric pressure in the collection chamber and the reaction chamber can be determined according to the diameter of the information acquisition port 14 and the distance between the information acquisition port 14 and the powder sample to adsorb the dust in the collection chamber and on the information acquisition port 14 to the reaction chamber as far as possible.
In order to prevent the powder sample from blocking the information acquisition port 14 under the condition that the powder sample is detected only under the high-temperature and high-pressure conditions and the powder sample is not required to be detected in situ, the detection and maintenance method in the embodiment further comprises the following steps:
s10, before the powder sample is tested, a baffle 4 is inserted between the powder sample and the information collection port 14 to isolate the powder sample from the information collection port 14, as shown in fig. 1.
In step S10, a part of the powder is blocked by the blocking plate 4, thereby reducing the powder adsorbed to the collection chamber and the information collection port 14. Wherein the baffle 4 is inserted between the powder sample and the information collecting port 14 by a robot arm.
The foregoing is directed to embodiments of the present application and it is noted that numerous modifications and adaptations may be made by those skilled in the art without departing from the principles of the present application and are intended to be within the scope of the present application.
Claims (4)
1. A detection and maintenance method of a near-normal pressure XPS system, characterized by comprising the steps of:
aligning a powder sample in a reaction cavity to an information acquisition port of the near-normal pressure XPS system, and detecting the powder sample;
after waiting to detect to accomplish, to the reaction chamber carries out the evacuation, lets in nearly atmospheric pressure gas in gathering the chamber, nearly atmospheric pressure gas's atmospheric pressure is not less than 100mbar, wherein, nearly atmospheric pressure gas is inert gas, makes gather atmospheric pressure in the chamber and be greater than atmospheric pressure in the reaction chamber, in order with information acquisition mouth with gather the powder in the chamber and adsorb to in the reaction chamber, gather the chamber with information acquisition mouth intercommunication, gather atmospheric pressure in the chamber and be at least 1 x 10 of atmospheric pressure in the reaction chamber6The step of introducing near-atmospheric pressure gas into the collection cavity specifically comprises the following steps: closing a driving motor of the molecular pump configured in the collection cavity, and introducing near-normal-pressure gas into the collection cavity through an air inlet of the molecular pump until the rotating speed of the molecular pump is reached in the process of decelerating the molecular pumpIs zero.
2. The inspection and maintenance method of claim 1, wherein the diameter of the information acquisition port is 300 um.
3. The inspection and maintenance method of claim 2, wherein the distance between the information collection port and the powder sample does not exceed 40 mm.
4. The inspection and maintenance method of claim 1, wherein without requiring in situ inspection of the powder sample, the inspection and maintenance method further comprises: a baffle is inserted between the powder sample and the information acquisition port to shield the powder sample.
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| US7231324B2 (en) * | 2005-04-29 | 2007-06-12 | Revera Incorporated | Techniques for analyzing data generated by instruments |
| CN201066345Y (en) * | 2007-08-10 | 2008-05-28 | 南京埃森环境技术有限公司 | Wearing-resisting and blockage prevention device for high-temperature smoke content instrument |
| GB2460855B (en) * | 2008-06-11 | 2013-02-27 | Kratos Analytical Ltd | Electron spectroscopy |
| US9080948B2 (en) * | 2013-03-14 | 2015-07-14 | International Business Machines Corporation | Dynamic peak tracking in X-ray photoelectron spectroscopy measurement tool |
| CN104062312B (en) * | 2014-06-09 | 2017-04-12 | 清华大学 | X-ray photoelectron spectroscopy (XPS) analysis method and system for researching interaction of plasma and material surface |
| CN107860783B (en) * | 2017-10-23 | 2019-09-24 | 中国科学院化学研究所 | XPS sampling device |
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