CN112540117A - Gas phase in-situ mass spectrum detection device - Google Patents
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Abstract
The invention relates to a gas phase in-situ mass spectrum detection device, which is mainly used for the in-situ detection research of anion gas phase reaction. The device comprises an ion source chamber, an acceleration chamber, a lens chamber and a detection chamber. When the device works, the whole device is in a high vacuum environment, plasma is generated by sputtering a sample with laser, the plasma reacts with other gases through the reaction channel to generate cluster ions, the cluster ions enter the acceleration chamber, are accelerated by the accelerator, pass through the focusing lens, reach the detection chamber, and receive ion information by the detector. Compared with the prior art, the invention has the advantages that: the ion source of the instrument can realize the in-situ detection of the on-line reaction of ions, and the whole instrument has simple and compact design structure, low manufacturing cost, good performance stability and wide range of measured mass-to-charge ratio.
Description
Technical Field
The invention relates to a gas phase in-situ mass spectrum detection device, and belongs to the field of mass spectrum analysis.
Background
The study on the adsorption and reaction of cluster ions is very important for understanding the micro-mechanism of some complex chemical processes such as heterogeneous catalytic reaction process ([1] Muetterties EL.science,1977,196: 839-. The method researches how the cluster evolves from atom and molecule step by step growth and how the geometric, electronic structure and physical and chemical properties of the cluster are gradually changed along with the growth process, and when the specific size grows to be large, the properties can be transited to a macroscopic phase.
There are many mass spectrometric techniques internationally, and recently, the reaction of some transition metal oxide clusters with small molecules such as hydrocarbons and carbon monoxide has been studied by combining cluster mass spectrometric experiments and computational chemistry ([3] Ding XL, Zhao YX, Wu XN, Wang ZC, Ma JB, He sg. Chem Eur J,2010,16: 11463; [4] Ma JB, Wu XN, Zhao XX, Ding He, sg. Phys Chem Phys 2010,12: 12223-.
The existing time-of-flight mass spectrometry device mainly comprises an ion source chamber, an ion acceleration chamber, a lens chamber, a detection chamber and a set of high vacuum system. The ion chamber main chamber generates plasma through laser sputtering and further reacts with small molecules to generate cluster ions. The accelerating chamber is composed of 12 electrode plates, the 1 st, 6 th and 12 th electrode plates are respectively added with-1500V, -1200V and grounded, and cluster ions are pushed out of the accelerating chamber by voltage difference. And four deflection electrodes, namely an upper deflection electrode, a lower deflection electrode, a left deflection electrode, a right deflection electrode and a left deflection electrode, are used for finely adjusting the flight path of cluster ions. The lens chamber mainly comprises three electrode tubes, wherein the first electrode tube and the third electrode tube are grounded, and the second electrode tube is added with-500V, so that scattered cluster ions can be focused. The detection chamber is mainly used for detecting cluster ions with different flight times, the ions generate signals after striking the microchannel plate, the signals are transmitted to the amplifier and then to the acquisition card, and mass spectrum information is acquired and displayed by computer software. The entire set of equipment used three 1500 liter turbo molecular pumps to maintain vacuum and three 4 liter mechanical pumps as backing pumps.
In addition, the design of the existing instrument and equipment has the problem of low resolution, and in the linear time-of-flight mass spectrum, the resolution R of 600 is generally difficult to achieve, and is slightly insufficient compared with the resolution R of 3000 of the reflection time-of-flight mass spectrum.
Disclosure of Invention
The invention aims to provide an in-situ detection device for anion gas phase reaction. The ion source of the instrument can realize the in-situ detection of the gas-phase on-line reaction of cluster ions, and the whole instrument has the advantages of simple and compact design structure, low manufacturing cost, good performance stability and wide range of measured mass-to-charge ratio.
The technical solution of the invention for realizing the above purpose is as follows:
a gas phase in-situ mass spectrum detection device comprises an ion source chamber, an acceleration chamber, a lens chamber and a detection chamber which are sequentially connected, wherein an ion source assembly is arranged in the ion source chamber, an accelerator and an ion deflection unit are arranged in the acceleration chamber, an ion focusing lens is arranged in the lens chamber, and the detection chamber is provided with a gate valve, an ion detector and a linear introducer;
the ion source assembly in the ion source chamber comprises a laser, a focusing lens, a first pulse valve, a second pulse valve, an ion rotating rod, a growth channel, a reaction channel and a nozzle; the sample is positioned in the ion rotating rod, the laser irradiates laser on the sample through the focusing lens, the first pulse valve is arranged above a route between the focusing lens and the sample and used for introducing cooling gas, and the growth channel is positioned below the route between the focusing lens and the sample and opposite to the first pulse valve; the reaction channel is positioned at the lower end of the growth channel, and the second pulse valve is positioned on the side surface of the reaction channel and used for loading reaction gas; the nozzle is located at the lower end of the reaction channel.
In a preferred embodiment of the invention, the laser irradiates the sample, plasma is generated in the growth channel, the plasma enters the reaction channel and reacts with the gas loaded by the second pulse valve to generate cluster ions, and the cluster ions leave the ion source chamber through the nozzle and enter the acceleration chamber.
In the preferred embodiment of the invention, the length, width and height of the first electrode plate of the accelerator are respectively 11-13mm, 11-13mm and 0.5-1.5 mm; the length, width and height of the other electrode plates are the same as those of the first electrode plate, but the center of the electrode plate is a hollow circle with the diameter of 7-9mm for cluster ion flying.
In a preferred embodiment of the invention, the growth channel of the ion source chamber has a diameter of 2.3-2.7mm and a length of 18-22 mm.
In a preferred embodiment of the present invention, the cooling gas introduced by the first pulse valve comprises helium.
In a preferred embodiment of the present invention, an accelerator and a first ion deflection unit are disposed in the acceleration chamber, and an ion deflection direction of the ion deflection unit includes up-down deflection and/or left-right deflection.
In the preferred embodiment of the present invention, the lens chamber includes a first ion focusing lens, a second ion focusing lens and a second ion deflection component, which ensure the focusing and flight directions of cluster ions, the two ends of the first ion focusing lens and the second ion focusing lens are grounded, and a voltage of 400-600V is applied in the middle.
In a preferred embodiment of the invention, the ion deflection direction of the second deflection unit comprises a left-right deflection.
In a preferred embodiment of the invention, the probe is fixed to the linear introducer to adjust its position.
The invention also provides a gas phase in-situ mass spectrum detection method, which adopts the gas phase in-situ mass spectrum detection device, utilizes laser to irradiate a sample through the focusing lens to generate plasma, the plasma is reacted with gas loaded by the second pulse valve through the reaction channel to generate cluster ions, the cluster ions leave the ion source and reach the acceleration chamber, the cluster ions are accelerated and pushed out by the high-voltage double-field pulse of the accelerator, and reach the detection chamber through the ion deflection unit and the ion focusing lens, so that the distribution information of the cluster ions is detected by the detector.
In the preferred embodiment of the invention, the gate valve is closed when the sample is replaced or not in operation to prevent leakage from the ion source chamber and effectively protect the detector.
The invention has the advantages that:
(1) the device has simple integral structure design and is convenient to process; (2) the mass spectrum obtained by detection has good stability and wide mass-to-charge ratio range; (3) the gas-phase online reaction in-situ detection of cluster ions can be completed. In addition, the invention can make resolution up to 650 through comprehensive improvement of multiple aspects.
Drawings
The invention is further illustrated by the following figures and examples.
FIG. 1 is a schematic structural diagram of an in-situ detection device for gas phase reaction of negative ions according to the present invention. 1 is an ion source chamber; 2 is an accelerator; 3 is a first ion deflection unit; 4. 5 is an ion focusing lens; 6 is a second ion deflection unit; 7 is a gate valve; 8, an ion detector; and 9 is a linear introducer.
Fig. 2 is a schematic view of an ion source assembly.
Wherein 10 is a laser; 11 is a focusing lens; 12 is a first pulse valve, 18 is a second pulse valve; 13 is a sample; 14 is an ion rotating rod; 15 is a growth channel; 16 is a reaction channel; and 17 is a nozzle.
FIG. 3 is a mass spectrum of NbOn- + CCl4 collected by the gas in-situ mass spectrometry detection device of the present invention.
Detailed Description
As shown in fig. 1, the present invention is an in-situ detection device for gas phase reaction of negative ions, which comprises an ion source chamber 1, an acceleration chamber, a lens chamber and a detection chamber. Wherein, an ion source component is arranged in the ion source chamber 1. An accelerator 2 and ion deflection units (3, 6) are arranged in the acceleration chamber, two ion focusing lenses 4 and 5 are arranged in the lens chamber, and a gate valve 7, an ion detector 8 and a linear introducer 9 are arranged in the detection chamber.
Wherein, the accelerating chamber is arranged below the outlet of the ion source chamber 1, and the lens chamber and the detecting chamber are respectively arranged on the right side of the accelerating chamber in sequence.
More specifically, a first ion deflection unit 3 is arranged in the ion acceleration direction of an accelerator 2 of the acceleration chamber, two ion focusing lenses 4 and 5 are sequentially arranged at an ion outlet of the ion deflection unit 3, a second ion deflection unit 6 is arranged at an ion outlet of the ion focusing lens 5, a gate valve 7 is arranged at an ion outlet end of the second ion deflection unit 6, and an ion detector 8 and a linear introducer 9 are arranged on one side of the ion outlet of the gate valve 7. The length, width and height of the first electrode plate of the accelerator 2 are respectively 12mm, 12mm and 1 mm. The length, width and height of the other electrode plates are the same as those of the first electrode plate, but the center of each electrode plate is a hollow circle with the diameter of 8mm for cluster ions to fly. The accelerating electrode plate has larger size than that of other mass spectrometer instruments, is more favorable for stabilizing an electric field and improving the mass spectrum resolution.
The gate valve 7 is closed when the sample is replaced or not in operation, so that the ion source chamber is prevented from leaking air, and the detector is effectively protected. The position of the probe 8 can be adjusted by fixing it to the linear introducer 9.
As shown in fig. 2, the ion source assembly in the ion source chamber 1 includes a laser 10, a focusing lens 11, a first pulse valve 12, a second pulse valve 18, an ion rotation rod 14, a growth channel 15, a reaction channel 16, and a nozzle 17. Commonly used growth channels are typically 3mm in diameter and 30mm long. The diameter of the growth channel 15 is 2.5mm, and the length is 20mm, and the use result shows that the growth of the plasma is designed to generate small molecular clusters more easily.
Wherein, the wavelength of the laser 10 is 532nm, and the energy is 10-20 mJ.
The focusing lens 11 mainly focuses the laser light on the target surface of the sample 13. The sample 13 is placed in an ion rotation rod 14. The laser of the laser 10 is focused by the focusing lens 11 and then strikes the sample 13 to generate plasma. The laser can effectively hit different positions of the sample surface by rotating the ion rotating rod 14, and the service life of the sample 13 is prolonged.
A first pulse valve 12 is installed above the path between the focusing lens 11 and the sample 13, and is mainly used for introducing helium gas, which plays a role of cooling plasma. The growth channel 15 is located below the line between the focusing lens 11 and the sample 13, opposite the first pulse valve 12; the reaction channel 16 is positioned at the lower end of the growth channel 15, and the second pulse valve 18 is positioned on the side surface of the reaction channel 16; the nozzle 17 is positioned at the lower end of the reaction channel 16; the plasma generated by the sample is sent to the reaction channel 16 by the growth channel 15, and reacts with the reaction gas loaded by the second pulse valve 18 to generate cluster ions, and the cluster ions enter the acceleration chamber through the nozzle 17.
The use principle of the invention is as follows:
a laser sputtering sample 13 generates plasma, helium is loaded into the reaction channel 16 from the growth channel 15 after being cooled by the first pulse valve 12, vaporized carbon tetrachloride is introduced into the reaction channel 16 by the second pulse valve 18 to react with the plasma to generate new cluster ions, the cluster ions enter the accelerator 2 after being cooled by the nozzle 17, are pushed out of the accelerator under double-field high pressure, pass through the ion deflection units (3 and 6) and the ion focusing lenses (4 and 5), reach the detection chamber, are detected by the detector, and transmit cluster ion signals to a computer for processing to obtain a mass spectrogram. By way of example, FIG. 3 shows NbOn- + CCl collected by the gas phase in-situ mass spectrometry detection apparatus of the present invention4Mass spectrum of (2). The resolution of the mass spectrum of the invention can reach 650.
Claims (10)
1. A gas phase in-situ mass spectrometry detection device is characterized in that: the ion source device comprises an ion source chamber, an acceleration chamber, a lens chamber and a detection chamber which are sequentially connected, wherein an ion source assembly is arranged in the ion source chamber, an accelerator and an ion deflection unit are arranged in the acceleration chamber, an ion focusing lens is arranged in the lens chamber, and the detection chamber is provided with a gate valve, an ion detector and a linear introducer;
the ion source assembly in the ion source chamber comprises a laser, a focusing lens, a first pulse valve, a second pulse valve, an ion rotating rod, a growth channel, a reaction channel and a nozzle; the sample is positioned in the ion rotating rod, the laser irradiates laser on the sample through the focusing lens, and the first pulse valve is arranged above a route between the focusing lens and the sample and used for introducing cooling gas; the growth channel is positioned below the route between the focusing lens and the sample, and is opposite to the first pulse valve; the reaction channel is positioned at the lower end of the growth channel, and the second pulse valve is positioned on the side surface of the reaction channel and used for loading reaction gas; the nozzle is located at the lower end of the reaction channel.
2. The gas phase in situ mass spectrometry apparatus of claim 1, wherein: the length, width and height of the first electrode plate of the accelerator are respectively 11-13mm, 11-13mm and 0.5-1.5 mm; the length, width and height of the other electrode plates are the same as those of the first electrode plate, but the center of the electrode plate is a hollow circle with the diameter of 7-9mm for cluster ion flying.
3. The gas phase in situ mass spectrometry apparatus of claim 1, wherein: the diameter of the growth channel of the ion source chamber is 2.3-2.7mm, and the length is 18-22 mm.
4. The gas phase in situ mass spectrometry apparatus of claim 1, wherein: and irradiating the sample by laser, generating plasma in the growth channel, enabling the plasma to enter the reaction channel and react with the gas loaded by the second pulse valve to generate cluster ions, and enabling the cluster ions to leave the ion source chamber through the nozzle and enter the acceleration chamber.
5. The gas phase in situ mass spectrometry apparatus of claim 1, wherein: an accelerator and a first ion deflection unit are arranged in the acceleration chamber, and the ion deflection direction of the ion deflection unit comprises up-down deflection and/or left-right deflection.
6. The gas phase in situ mass spectrometry apparatus of claim 1, wherein: the lens chamber comprises a first ion focusing lens, a second ion focusing lens and a second ion deflection unit, the focusing and flying directions of cluster ions are ensured, two ends of the first ion focusing lens and the second ion focusing lens are grounded, and a voltage of 400-600V is applied in the middle.
7. The apparatus according to claim 6, wherein the mass spectrometer comprises: the ion deflection direction of the second deflection unit includes left and right deflection.
8. The gas phase in situ mass spectrometry apparatus of claim 1, wherein: the probe is fixed to the linear introducer to adjust its position.
9. A gas phase in-situ mass spectrometry detection method is characterized in that a gas phase in-situ mass spectrometry detection device of any one of claims 1 to 8 is adopted, a sample is irradiated by laser through a focusing lens to generate plasma, the plasma is reacted with gas loaded by a second pulse valve through a reaction channel to generate cluster ions, the cluster ions leave an ion source and reach an acceleration chamber, the cluster ions are accelerated and pushed out by high-voltage double-field pulses of an accelerator, and the cluster ions reach a detection chamber through an ion deflection unit and an ion focusing lens, so that distribution information of the cluster ions is detected by a detector.
10. The method of claim 9, wherein the gate valve is closed during sample replacement or non-operation to prevent leakage from the ion source chamber and effectively protect the detector.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113380596A (en) * | 2021-06-07 | 2021-09-10 | 中国科学院化学研究所 | Low kinetic energy pulse ion source based on photoionization |
| CN113933374A (en) * | 2021-10-12 | 2022-01-14 | 中国原子能科学研究院 | Detection device and method |
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| CN103531432A (en) * | 2013-09-30 | 2014-01-22 | 中国地质科学院地质研究所 | Pulsed ion source, mass spectrometer and method for generating ions |
| CN107727730A (en) * | 2017-11-29 | 2018-02-23 | 厦门大学 | A kind of dual reflective flight time mass spectrum optoelectronic speed imager |
| CN111739785A (en) * | 2020-06-30 | 2020-10-02 | 中国科学院上海应用物理研究所 | Dual ion source slow electron speed imaging device |
| CN211654767U (en) * | 2019-12-17 | 2020-10-09 | 厦门大学 | Linear time-of-flight mass spectrometry vertical photoelectron velocity imager |
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2020
- 2020-11-26 CN CN202011347227.5A patent/CN112540117A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103531432A (en) * | 2013-09-30 | 2014-01-22 | 中国地质科学院地质研究所 | Pulsed ion source, mass spectrometer and method for generating ions |
| CN107727730A (en) * | 2017-11-29 | 2018-02-23 | 厦门大学 | A kind of dual reflective flight time mass spectrum optoelectronic speed imager |
| CN211654767U (en) * | 2019-12-17 | 2020-10-09 | 厦门大学 | Linear time-of-flight mass spectrometry vertical photoelectron velocity imager |
| CN111739785A (en) * | 2020-06-30 | 2020-10-02 | 中国科学院上海应用物理研究所 | Dual ion source slow electron speed imaging device |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113380596A (en) * | 2021-06-07 | 2021-09-10 | 中国科学院化学研究所 | Low kinetic energy pulse ion source based on photoionization |
| CN113380596B (en) * | 2021-06-07 | 2024-01-30 | 中国科学院化学研究所 | Low kinetic energy pulse ion source based on photoionization |
| CN113933374A (en) * | 2021-10-12 | 2022-01-14 | 中国原子能科学研究院 | Detection device and method |
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Application publication date: 20210323 |