CN109979796B - Photoelectron time-of-flight spectrum measurement method - Google Patents
Photoelectron time-of-flight spectrum measurement method Download PDFInfo
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- 238000001228 spectrum Methods 0.000 title claims abstract description 12
- 238000000691 measurement method Methods 0.000 title description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 322
- 239000007788 liquid Substances 0.000 claims abstract description 263
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 161
- 230000003993 interaction Effects 0.000 claims abstract description 53
- 230000005540 biological transmission Effects 0.000 claims abstract description 26
- 238000006073 displacement reaction Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 21
- 230000009467 reduction Effects 0.000 claims abstract description 13
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 39
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 39
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 5
- 239000010410 layer Substances 0.000 claims description 5
- 239000002356 single layer Substances 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 4
- 229910000595 mu-metal Inorganic materials 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 3
- 230000005693 optoelectronics Effects 0.000 claims 1
- 238000011160 research Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 10
- 230000008859 change Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000007704 transition Effects 0.000 description 5
- 230000001502 supplementing effect Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000009941 weaving Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001420 photoelectron spectroscopy Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/227—Measuring photoelectric effect, e.g. photoelectron emission microscopy [PEEM]
- G01N23/2273—Measuring photoelectron spectrum, e.g. electron spectroscopy for chemical analysis [ESCA] or X-ray photoelectron spectroscopy [XPS]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/0027—Methods for using particle spectrometers
- H01J49/0036—Step by step routines describing the handling of the data generated during a measurement
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/06—Electron- or ion-optical arrangements
- H01J49/061—Ion deflecting means, e.g. ion gates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/06—Electron- or ion-optical arrangements
- H01J49/062—Ion guides
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- Spectroscopy & Molecular Physics (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention relates to the field of physical research, in particular to a method for measuring an photoelectron time flight spectrum, which comprises a high-performance liquid chromatograph, a liquid inlet pipe, a recoverer, an interaction cavity, a control rod, a permanent magnet, a displacement table, a nozzle, a shunt, a speed reduction grid, a magnetic shielding cover, a solenoid, a drift tube, a micro-channel disc, a flight cavity, a vacuum pump I, a vacuum pump II, a liquid nitrogen inlet, a support table, a liquid nitrogen cold trap, a cold trap cavity, a gate valve, a vacuum pump III, a liquid nitrogen transmission pipe, a liquid nitrogen Dewar, a lowest liquid level sensor, an alarm sensor, a highest liquid level sensor, a gas-liquid separator, a nitrogen outlet, a laser, a controller and a computer.
Description
Technical Field
The invention relates to the field of physical research, in particular to a photoelectron time-of-flight spectrum measurement method capable of measuring in different working modes by adjusting the collection angle of photoelectrons.
Background
The photoelectron spectroscopy technology is a commonly used technology for measuring the characteristics of substances, and is mainly based on a photoelectron spectrometer, so that the time-resolved photoelectron spectroscopy technology is rapidly developed by adopting an ultrafast laser technology in recent years, and the dynamic process of atoms or molecules can be measured on an attosecond time scale. Two commonly used attosecond techniques based on photoelectron detection are attosecond fringe techniques, in which photoelectrons collected from within a small solid angle are typically analyzed, and two-photon transition interference attosecond pulse reconstruction techniques, and thus a photoelectron spectrometer is required to have a magnetic field-free characteristic; in two-photon transition interference attosecond pulse reconstruction techniques, it is desirable to avoid space-charge effects and to achieve high count rates only by increasing the collection efficiency of the spectrometer, e.g., by using a magnetic field shape design like "magnetic flask". In addition, considering the vacuum environment requirements and stability during operation within the photoelectron spectrometer, it is necessary to install a small liquid nitrogen dewar at some locations within the spectrometer and to use a liquid nitrogen replenishment system to replenish the liquid nitrogen dewar with liquid nitrogen. Defect one of the prior art: the current photoelectron spectrometer cannot change the collection angle of photoelectrons, and the magnetic field state of the photoelectron spectrometer cannot be switched between a magnetic field-free mode and a magnetic bottle mode during operation, namely the photoelectron spectrometer cannot be switched between an attosecond stripe technology and a two-photon transition interference attosecond pulse reconstruction technology; the defects of the prior art are as follows: in a common spectrometer device which needs to test a liquid sample, the vacuum degree in the device is poor due to the influence of a solution to be tested, and if a vacuum pump set with a high pumping speed is adopted, the vibration of the spectrometer is caused, so that the quality of collected data is influenced; defects three in the prior art: the common commercial liquid nitrogen supplementing system is used for a larger Dewar with a volume of more than a few liters, and for a smaller Dewar, a liquid nitrogen transmission pipe and a related sensor are required to be installed in a smaller space and can be influenced by boiling and splashing of liquid nitrogen, so that instability occurs in a liquid nitrogen recharging process, and the photoelectron time flight spectrum measuring method can solve the problem.
Disclosure of Invention
In order to solve the problems, the method of the invention can change the collection angle of photoelectrons in time-of-flight spectrum measurement and switch between a magnetic field-free mode and a magnetic bottle mode by placing a permanent magnet at one end of a drift tube of a spectrometer and adopting a solenoid to generate a uniform magnetic field in the drift region, and in addition, a liquid nitrogen cold trap is adopted to improve the vacuum degree in the spectrometer, and a liquid nitrogen supplementing method with higher stability is adopted to automatically supplement liquid nitrogen to the liquid nitrogen cold trap.
The technical scheme adopted by the invention is as follows:
the photoelectron time flight spectrometer comprises a high performance liquid chromatograph, a liquid inlet pipe, a recoverer, an interaction cavity, a control rod, a permanent magnet, a displacement table, a nozzle, a flow divider, a speed reduction grid mesh, a magnetic shielding cover, a solenoid, a drift tube, a micro-channel disk, a flight cavity, a vacuum pump I, a vacuum pump II, a liquid nitrogen inlet, a support table, a liquid nitrogen cold trap, a cold trap cavity, a gate valve, a vacuum pump III, a liquid nitrogen transmission pipe, a liquid nitrogen Dewar, a lowest liquid level sensor, an alarm sensor, a highest liquid level sensor, a gas-liquid separator, a nitrogen outlet, a laser, a magnetic control valve, a controller and a computer, wherein xyz is a three-dimensional space coordinate system, the interaction cavity is provided with a light transmission window, a laser beam emitted by the laser can be emitted into the interaction cavity along the x-axis direction,the cold trap cavity is connected to the upper surface of the interaction cavity, and the flying cavity is connected to the side surface of the interaction cavity and is separated by the flow divider; the permanent magnet, the displacement table and the nozzle are all positioned in an interaction cavity, the nozzle is arranged on the displacement table and connected with the high performance liquid chromatograph through a liquid inlet pipe, the position of the nozzle can be adjusted through the displacement table, the permanent magnet is provided with an operating rod, a magnetic shielding chamber is arranged in the interaction cavity, the influence of the magnet positioned in the magnetic shielding chamber on a magnetic field outside the magnetic shielding chamber can be shielded, and the permanent magnet can be arranged in the magnetic shielding chamber through adjusting the operating rod; the interaction cavity and the flying cavity are internally provided with magnetometers for monitoring the intensity and the distribution of the magnetic field; the recoverer is connected below the interaction cavity and can collect samples which are ejected by the nozzle and do not interact with the laser; the speed reducing grid mesh, the magnetic shielding cover, the solenoid, the drift tube and the micro-channel disc are all positioned in a flying cavity, the flying cavity is respectively connected with a vacuum pump I and a vacuum pump II, and the highest vacuum degree of the flying cavity can reach 10 under the condition that the vacuum pump I and the vacuum pump II are simultaneously started -8 The level of mbar, the drift tube has beginning and end, the end of the drift tube connects the micro-channel disc, the micro-channel disc cable connects the computer; the side surface of the cold trap cavity is connected with a vacuum pump III through a gate valve, the liquid nitrogen cold trap is a cylindrical container with the height of 15cm and the inner diameter of 10cm, the upper end of the liquid nitrogen cold trap is connected with the cold trap cavity through a supporting table, so that the liquid nitrogen cold trap is positioned in the cold trap cavity, the liquid nitrogen cold trap is connected with a liquid nitrogen Dewar through a supporting table, a liquid nitrogen inlet and a liquid nitrogen transmission pipe, a magnetic control valve is arranged between the liquid nitrogen Dewar and the liquid nitrogen transmission pipe, a lowest liquid level sensor, an alarm sensor and a highest liquid level sensor are arranged in the liquid nitrogen cold trap, the liquid nitrogen cold trap is respectively connected with a controller outside the liquid nitrogen cold trap through cables, the cables penetrate through the supporting table, the controller can control the opening and closing of the magnetic control valve according to the states of the lowest liquid level sensor, the alarm sensor and the highest liquid level sensor, the supporting table is provided with a nitrogen outlet, and the gas-liquid separator is positioned in the liquid nitrogen inlet; one end of the operating rod is positioned outside the interaction cavity and passes through the operating rodThe position of the permanent magnet can be adjusted, the permanent magnet is a cylinder with the diameter of 20mm and the height of 30mm and is coaxial with the aperture of the diverter, the axis of the drift tube is along the z-axis direction, the solenoid is nested outside the drift tube, the length of the solenoid is 380mm, the inner diameter of the solenoid is 33mm, the solenoid is wound by a single-layer coil with 200 turns, the thickness of an insulating layer outside the wire is 0.25mm, the drift tube and the solenoid are both positioned in the magnetic shielding cover, the speed reduction grid is positioned between the diverter and the initial end of the drift tube, the magnetic field intensity near the initial end of the drift tube can be changed by adjusting the current in the solenoid, and different magnetic field shapes are formed among the diverter, the speed reduction grid and the initial end of the drift tube; the speed reducing grid consists of two identical grids, the grids are formed by weaving copper wires, the grids are square with the side length of 5mm, the grids of the grids are square with the side length of 0.2mm, the distance between the two grids is 0.8mm, and the speed reducing grid can reduce photoelectrons with larger kinetic energy; the lowest liquid level sensor is 2cm away from the bottom surface of the liquid nitrogen cold trap, the alarm sensor is 1cm away from the bottom surface of the liquid nitrogen cold trap, the highest liquid level sensor is 1cm away from the top surface of the liquid nitrogen cold trap, the PTFE pipes I, PTFE II and PTFE pipes III with inner diameters of 6mm are respectively sleeved outside the lowest liquid level sensor, the alarm sensor and the highest liquid level sensor, the PTFE pipes I and the PTFE pipes II are respectively provided with an opening at one end and a closing at one end, a cable connected with the lowest liquid level sensor is bent obliquely upwards at the position 1cm away from the lowest liquid level sensor, the cable passes through the closing end of the PTFE pipe I and is sealed, and the opening direction of the PTFE pipe I is an oblique upper 45-degree angle; the cable connected with the alarm sensor passes through the closed end of the PTFE tube II and is sealed, the opening direction of the PTFE tube II is vertical downward, and two through holes with the diameter of 0.4mm are arranged on the closed end. The aperture of the shunt is 0.5mm, the inner diameter of the drift tube is 30mm, the outer diameter is 34mm, the length is 400mm, the length of the solenoid is 380mm, the inner diameter is 33mm, the solenoid is wound by a single-layer coil with 200 turns, the thickness of an insulating layer outside the wire is 0.25mm, and the magnetic shielding cover is a mu-metal tube with the inner diameter of 95mm and the thickness of 3 mm.
The photoelectron time flight spectrum measuring method comprises the following steps:
opening a gate valve, opening a vacuum pump III to vacuumize a cold trap cavity, and opening a vacuum pump I and a vacuum pump II to vacuumize a flight cavity;
step two, opening a magnetic control valve to enable liquid nitrogen in the liquid nitrogen Dewar to enter a liquid nitrogen cold trap through a liquid nitrogen transmission pipe, and opening a controller to monitor signals of a lowest liquid level sensor, an alarm sensor and a highest liquid level sensor;
step three, moving the nozzle to a position near the diverter in the interaction cavity through the displacement table, and conveying a solution sample to be tested to the nozzle through the liquid inlet pipe by high performance liquid chromatography, wherein the solution sample to be tested forms tiny liquid drops after passing through the nozzle;
turning on the laser to make the laser beam emitted by the laser shoot into the position near the nozzle in the interaction cavity along the x-axis direction, and making the laser interact with the tiny liquid drops of the solution sample to be tested to generate photoelectrons;
step five, when working in a non-magnetic field mode, the permanent magnet is arranged in the magnetic shielding chamber through the adjusting control rod, and no current is applied to the solenoid; when the electromagnetic valve works in a magnetic bottle mode, the position of the permanent magnet is adjusted through the operating rod, current is applied to the solenoid, and the collection angle of photoelectrons is changed through adjusting the position of the permanent magnet and the current of the solenoid;
step six, photoelectrons in the collection angle enter the flight cavity through the diverter, enter the micro-channel disc after sequentially passing through the deceleration grid mesh and the drift tube, and transmit collected data to the computer through the micro-channel disc;
and seventhly, processing the data obtained in the step six by a computer, and analyzing to obtain the relevant characteristics of the sample to be detected.
The beneficial effects of the invention are as follows:
the time-flight spectrum measuring method can adjust the collection angle of photoelectrons, can be suitable for an attosecond stripe technology and a two-photon transition interference attosecond pulse reconstruction technology, has better vacuum during measurement, and has high stability in the liquid nitrogen supplementing process.
Drawings
The following is further described in connection with the figures of the present invention:
FIG. 1 is a schematic illustration of the present invention;
fig. 2 is an enlarged schematic diagram of a liquid nitrogen cold trap.
In the figure, 1, high performance liquid chromatography, 2, feed tube, 3, regenerator, 4, interaction chamber, 5, joystick, 6, permanent magnet, 7, displacement stage, 8, nozzle, 9, shunt, 10, reduction grid, 11, magnetic shield, 12, solenoid, 13, drift tube, 14, microchannel plate, 15, flight chamber, 16, vacuum pump I,17, vacuum pump II,18, liquid nitrogen inlet, 19, support stage, 20, liquid nitrogen cold trap, 21, cold trap chamber, 22, gate valve, 23, vacuum pump III,24, liquid nitrogen transfer tube, 25, liquid nitrogen Dewar, 26, minimum liquid level sensor, 27, alarm sensor, 28, maximum liquid level sensor, 29, gas-liquid separator, 30, nitrogen outlet.
Detailed Description
As shown in fig. 1, the photoelectron time-of-flight spectrometer comprises a high performance liquid chromatograph (1), a liquid inlet pipe (2), a recoverer (3), an interaction cavity (4), a control rod (5), a permanent magnet (6), a displacement table (7), a nozzle (8), a flow divider (9), a reduction grid (10), a magnetic shielding cover (11), a solenoid (12), a drift tube (13), a micro-channel disk (14), a flight cavity (15), a vacuum pump I (16), a vacuum pump II (17), a liquid nitrogen inlet (18), a support table (19), a liquid nitrogen cold trap (20), a cold trap cavity (21), a gate valve (22), a vacuum pump III (23), a liquid nitrogen transmission pipe (24), a liquid nitrogen Dewar (25), a lowest liquid level sensor (26), an alarm sensor (27), a highest liquid level sensor (28), a gas-liquid separator (29), a nitrogen outlet, a laser, a magnetic control valve, a controller and a computer, xyz is a three-dimensional space coordinate system, the interaction cavity (4) has a light transmission window, and laser beams emitted by the laser can enter the interaction cavity (4) along the x-axis direction and are connected to the interaction cavity (4) along the x-axis direction and pass through the interaction cavity (4) and the interaction cavity (4), the aperture of the shunt (9) is 0.5mm; the permanent magnet (6), the displacement table (7) and the nozzle (8) are all positioned in the interaction cavity (4), the nozzle (8) is arranged on the displacement table (7) and is connected with the high-performance liquid chromatograph (1) through the liquid inlet pipe (2), the position of the nozzle (8) can be adjusted through the displacement table (7), the operating lever (5) is arranged in the permanent magnet (6), a magnetic shielding chamber is arranged in the interaction cavity (4), the influence of the magnet positioned in the magnetic shielding chamber on the magnetic field outside the magnetic shielding chamber can be shielded, and the permanent magnet (6) can be arranged in the magnetic shielding chamber through adjusting the operating lever (5); phase (C)Magnetometer is installed in each of the interaction cavity (4) and the flying cavity (15) for monitoring the intensity and distribution of the magnetic field; the recoverer (3) is connected below the interaction cavity (4), and the recoverer (3) can collect samples which are ejected by the nozzle (8) and do not interact with laser; the speed reducing grid (10), the magnetic shielding cover (11), the solenoid (12), the drift tube (13) and the micro-channel disk (14) are all positioned in the flying cavity (15), the magnetic shielding cover (11) is a mu-metal tube with the inner diameter of 95mm and the thickness of 3mm, the flying cavity (15) is respectively connected with the vacuum pump I (16) and the vacuum pump II (17), and the highest vacuum degree of the flying cavity (15) can reach 10 under the condition of simultaneously starting the vacuum pump I (16) and the vacuum pump II (17) -8 In the mbar level, the drift tube (13) is provided with a starting end and a tail end, the tail end of the drift tube (13) is connected with a micro-channel disc (14), and the micro-channel disc (14) is connected with a computer through a cable; the side surface of the cold trap cavity (21) is connected with a vacuum pump III (23) through a gate valve (22), the liquid nitrogen cold trap (20) is a cylindrical container with the height of 15cm and the inner diameter of 10cm, the upper end of the liquid nitrogen cold trap (20) is connected with the cold trap cavity (21) through a supporting table (19), the liquid nitrogen cold trap (20) is positioned in the cold trap cavity (21), the liquid nitrogen cold trap (20) is connected with a liquid nitrogen Dewar (25) through the supporting table (19), a liquid nitrogen inlet (18) and a liquid nitrogen transmission pipe (24), and a magnetic control valve is arranged between the liquid nitrogen Dewar (25) and the liquid nitrogen transmission pipe (24); one end of the operating rod (5) is positioned outside the interaction cavity (4), the position of the permanent magnet (6) can be adjusted through the operating rod (5), the permanent magnet (6) is a cylinder with the diameter of 20mm and the height of 30mm and is coaxial with the aperture of the drift tube (9), the axis of the drift tube (13) is along the z-axis direction, the solenoid (12) is nested outside the drift tube (13), the inner diameter of the drift tube (13) is 30mm, the outer diameter is 34mm and the length is 400mm, the drift tube (13) and the solenoid (12) are both positioned in the magnetic shielding cover (11), the speed reduction grid (10) is positioned between the shunt (9) and the initial end of the drift tube (13), and different magnetic field shapes are formed among the shunt (9), the speed reduction grid (10) and the initial end of the drift tube (13) by adjusting the current in the solenoid (12) so as to change the magnetic field intensity near the initial end of the drift tube (13); the speed reducing grid (10) consists of two identical grids, the grids are formed by weaving copper wires, the grids are square with the side length of 5mm, the grids of the grids are square with the side length of 0.2mm, the distance between the two grids is 0.8mm, and the speed reducing grid (10) can feed photoelectrons with larger kinetic energyAnd (5) decelerating the line.
As shown in fig. 2, which is an enlarged schematic diagram of the liquid nitrogen cold trap, a lowest liquid level sensor (26), an alarm sensor (27) and a highest liquid level sensor (28) are arranged in the liquid nitrogen cold trap (20) and are respectively connected to a controller outside the liquid nitrogen cold trap (20) through cables, the cables pass through a supporting table (19), the controller can control the opening and closing of a magnetic control valve according to the states of the lowest liquid level sensor (26), the alarm sensor (27) and the highest liquid level sensor (28), the supporting table (19) is provided with a nitrogen outlet (30), a gas-liquid separator (29) is arranged in a liquid nitrogen inlet (18), liquid nitrogen in a liquid nitrogen transmission pipe (24) can pass through the gas-liquid separator (29) and enter the liquid nitrogen cold trap (20), but nitrogen in the liquid nitrogen transmission pipe (24) cannot pass through the gas-liquid separator (29), and is discharged outside the liquid nitrogen cold trap (20); the lowest liquid level sensor (26) is 2cm away from the bottom surface of the liquid nitrogen cold trap (20), the alarm sensor (27) is 1cm away from the bottom surface of the liquid nitrogen cold trap (20), the highest liquid level sensor (28) is 1cm away from the top surface of the liquid nitrogen cold trap (20), PTFE pipes I, PTFE pipe II and PTFE pipe III with inner diameters of 6mm are respectively sleeved outside the lowest liquid level sensor (26), the alarm sensor (27) and the highest liquid level sensor (28), the PTFE pipe I and the PTFE pipe II are respectively provided with an opening at one end and a closing at one end, a cable connected with the lowest liquid level sensor (26) is bent obliquely upwards at a position 1cm away from the lowest liquid level sensor (26), the cable penetrates through the closing end of the PTFE pipe I and is sealed, and the opening direction of the PTFE pipe I is obliquely upwards at an angle of 45 degrees; a cable connected with the alarm sensor (27) passes through the closed end of the PTFE tube II and is sealed, the opening direction of the PTFE tube II is vertically downward, and two through holes with the diameter of 0.4mm are formed in the closed end.
The photoelectron time flight spectrometer comprises a high performance liquid chromatograph (1), a liquid inlet pipe (2), a recoverer (3), an interaction cavity (4), an operating rod (5), a permanent magnet (6), a displacement table (7), a nozzle (8), a shunt (9), a deceleration grid (10), a magnetic shielding cover (11), a solenoid (12), a drift tube (13), a micro-channel disk (14), a flight cavity (15), a vacuum pump I (16), a vacuum pump II (17), a liquid nitrogen inlet (18), a supporting table (19), a liquid nitrogen cold trap (20), a cold trap cavity (21), a gate valve (22), a vacuum pump III (23), a liquid nitrogen transmission pipe (24), a liquid nitrogen Dewar (25), a minimum liquid level sensor (26), an alarm sensor (27) and a maximum liquid level sensorThe device comprises a device (28), a gas-liquid separator (29), a nitrogen outlet, a laser, a magnetic control valve, a controller and a computer, wherein xyz is a three-dimensional space coordinate system, an interaction cavity (4) is provided with a light transmission window, a laser beam emitted by the laser can be emitted into the interaction cavity (4) along the x-axis direction, a cold trap cavity (21) is connected onto the interaction cavity (4), and a flying cavity (15) is connected onto the side surface of the interaction cavity (4) and is separated by a shunt (9); the permanent magnet (6), the displacement table (7) and the nozzle (8) are all positioned in the interaction cavity (4), the nozzle (8) is arranged on the displacement table (7) and is connected with the high-performance liquid chromatograph (1) through the liquid inlet pipe (2), the position of the nozzle (8) can be adjusted through the displacement table (7), the operating lever (5) is arranged in the permanent magnet (6), a magnetic shielding chamber is arranged in the interaction cavity (4), the influence of the magnet positioned in the magnetic shielding chamber on the magnetic field outside the magnetic shielding chamber can be shielded, and the permanent magnet (6) can be arranged in the magnetic shielding chamber through adjusting the operating lever (5); magnetometer is installed in each of the interaction cavity (4) and the flying cavity (15) for monitoring the intensity and distribution of the magnetic field; the recoverer (3) is connected below the interaction cavity (4), and the recoverer (3) can collect samples which are ejected by the nozzle (8) and do not interact with laser; the speed reducing grid (10), the magnetic shielding cover (11), the solenoid (12), the drift tube (13) and the micro-channel disk (14) are all positioned in the flying cavity (15), the flying cavity (15) is respectively connected with the vacuum pump I (16) and the vacuum pump II (17), and under the condition that the vacuum pump I (16) and the vacuum pump II (17) are simultaneously started, the highest vacuum degree of the flying cavity (15) can reach 10 -8 In the mbar level, the drift tube (13) is provided with a starting end and a tail end, the tail end of the drift tube (13) is connected with a micro-channel disc (14), and the micro-channel disc (14) is connected with a computer through a cable; the side of the cold trap cavity (21) is connected with a vacuum pump III (23) through a gate valve (22), the liquid nitrogen cold trap (20) is a cylindrical container with the height of 15cm and the inner diameter of 10cm, the upper end of the liquid nitrogen cold trap (20) is connected with the cold trap cavity (21) through a supporting table (19), the liquid nitrogen cold trap (20) is positioned in the cold trap cavity (21), the liquid nitrogen cold trap (20) is connected with a liquid nitrogen dewar (25) through the supporting table (19), a liquid nitrogen inlet (18) and a liquid nitrogen transmission pipe (24), a magnetic control valve is arranged between the liquid nitrogen dewar (25) and the liquid nitrogen transmission pipe (24), and a lowest liquid level sensor (26), an alarm sensor (27) and a highest liquid level sensor (28) are arranged in the liquid nitrogen cold trap (20) and are respectively connected to a control outside the liquid nitrogen cold trap (20) through cablesThe cable passes through the supporting table (19), the controller can control the opening and closing of the magnetic control valve according to the states of the lowest liquid level sensor (26), the alarm sensor (27) and the highest liquid level sensor (28), the supporting table (19) is provided with a nitrogen outlet (30), the gas-liquid separator (29) is positioned in the liquid nitrogen inlet (18), liquid nitrogen in the liquid nitrogen transmission pipe (24) can pass through the gas-liquid separator (29) and enter the liquid nitrogen cold trap (20), but nitrogen in the liquid nitrogen transmission pipe (24) cannot pass through the gas-liquid separator (29), and is therefore excluded from the liquid nitrogen cold trap (20); one end of the operating rod (5) is positioned outside the interaction cavity (4), the position of the permanent magnet (6) can be adjusted through the operating rod (5), the permanent magnet (6) is a cylinder with the diameter of 20mm and the height of 30mm and is coaxial with the aperture of the drift tube (9), the axis of the drift tube (13) is along the z-axis direction, the solenoid (12) is nested outside the drift tube (13), the length of the solenoid (12) is 380mm and the inner diameter is 33mm, the solenoid (12) is wound by 200 turns of single-layer coils, the thickness of an insulating layer outside the wire is 0.25mm, the drift tube (13) and the solenoid (12) are both positioned in the magnetic shielding cover (11), the speed reduction grid (10) is positioned between the shunt (9) and the initial end of the drift tube (13), and the magnetic field intensity near the initial end of the drift tube (13) can be changed by adjusting the current in the solenoid (12), and different magnetic field shapes are formed among the shunt (9), the speed reduction grid (10) and the initial end of the drift tube (13); the speed reducing grid (10) consists of two identical grids, the grids are formed by weaving copper wires, the grids are square with the side length of 5mm, the grids of the grids are square with the side length of 0.2mm, the distance between the two grids is 0.8mm, and the speed reducing grid (10) can reduce photoelectrons with larger kinetic energy; the lowest liquid level sensor (26) is 2cm away from the bottom surface of the liquid nitrogen cold trap (20), the alarm sensor (27) is 1cm away from the bottom surface of the liquid nitrogen cold trap (20), the highest liquid level sensor (28) is 1cm away from the top surface of the liquid nitrogen cold trap (20), PTFE pipes I, PTFE pipe II and PTFE pipe III with inner diameters of 6mm are respectively sleeved outside the lowest liquid level sensor (26), the alarm sensor (27) and the highest liquid level sensor (28), the PTFE pipe I and the PTFE pipe II are respectively provided with an opening at one end and a closing at one end, a cable connected with the lowest liquid level sensor (26) is bent obliquely upwards at a position 1cm away from the lowest liquid level sensor (26), the cable penetrates through the closing end of the PTFE pipe I and is sealed, and the opening direction of the PTFE pipe I is obliquely upwards at an angle of 45 degrees;a cable connected with the alarm sensor (27) passes through the closed end of the PTFE tube II and is sealed, the opening direction of the PTFE tube II is vertically downward, and two through holes with the diameter of 0.4mm are formed in the closed end. The aperture of the shunt (9) is 0.5mm, the inner diameter of the drift tube (13) is 30mm, the outer diameter is 34mm, the length of the drift tube is 400mm, the length of the solenoid (12) is 380mm, the inner diameter of the solenoid is 33mm, the solenoid (12) is wound by a single-layer coil with 200 turns, the thickness of an insulating layer outside the wire is 0.25mm, and the magnetic shielding cover (11) is a mu-metal tube with the inner diameter of 95mm and the thickness of 3 mm.
Principle of change in collection angle of photoelectrons:
since the photoelectrons generated after the interaction of the laser and the tiny liquid drops of the solution sample to be tested are dispersed in all directions in the space, the collection angle of the photoelectrons in the device is defined as: taking the interaction position of the laser and the tiny liquid drop of the solution sample to be measured as a vertex, and generating a solid angle corresponding to part of photoelectrons which can enter the flying cavity (15) in the photoelectrons; the position of the permanent magnet (6) is adjusted through the operating rod (5) so as to change the magnetic field intensity near the diverter (9) in the interaction cavity (4), meanwhile, the current in the solenoid (12) is adjusted so as to change the magnetic field intensity near the starting end of the drift tube (13), different magnetic field shapes are formed among the diverter (9), the deceleration grid (10) and the starting end of the drift tube (13), and different bunching effects are generated after the interaction of the laser and tiny liquid drops of a solution sample to be tested, so that the collection angle of photoelectrons can be changed.
Principle of preventing magnetic control valve from being opened or closed by mistake in the process of automatically supplementing liquid nitrogen:
because the shells of the lowest liquid level sensor (26), the alarm sensor (27) and the highest liquid level sensor (28) have higher heat conductivity, the splashing of liquid nitrogen is easier to trigger the sensors to generate false signals and transmit the false signals to a controller in the process of filling liquid nitrogen into a liquid nitrogen cold trap (20), and then a magnetic control valve is opened by mistake; in order to ensure that nitrogen can volatilize from liquid nitrogen without triggering a lowest liquid level sensor (26), the opening direction of a PTFE tube outside the lowest liquid level sensor (26) is a 45-degree angle obliquely upwards, the opening direction of the PTFE tube outside an alarm sensor (27) is vertically downwards, and two through holes are formed in the upper surface of the sleeve so that volatilized nitrogen can go out of the PTFE tube when the alarm sensor (27) is just immersed in liquid nitrogen.
Based on the design, when the liquid nitrogen level in the liquid nitrogen cold trap (20) is lower than the lowest liquid level sensor (26), the lowest liquid level sensor (26) can generate a trigger signal to the controller to open the magnetic control valve, and the process of transmitting the liquid nitrogen in the liquid nitrogen dewar (25) to the liquid nitrogen cold trap (20) is started; when the liquid level of the liquid nitrogen in the liquid nitrogen cold trap (20) exceeds the position of the highest liquid level sensor (28), the highest liquid level sensor (28) can generate a trigger signal to the controller to close the magnetic control valve, so that the liquid nitrogen in the liquid nitrogen Dewar (25) is stopped from being transmitted to the liquid nitrogen cold trap (20); when a special condition is met, when the liquid level of liquid nitrogen in the liquid nitrogen cold trap (20) is lower than the alarm sensor (27), the alarm sensor (27) generates a trigger signal to the controller to give an alarm.
Examples: the lowest liquid LEVEL sensor (26) and the highest liquid LEVEL sensor (28) are both resistance type temperature sensors with platinum protective layers on the outer sides, the model is Pt100 manufactured by KGW Isotherm company, the specific model of the alarm sensor (27) is LS2 type liquid nitrogen liquid LEVEL sensor manufactured by Teragon Research company, the controller is LEVEL CONTROL LN2 type liquid nitrogen liquid LEVEL controller manufactured by KGW Isotherm company, the high performance liquid chromatography (1) is JAI LC-9104 type, the permanent magnet (6) is samarium cobalt magnet, and the solution sample to be detected is aqueous solution of sodium chloride with the concentration of 0.05 mol/liter; the laser emits laser with the wavelength of 532nm and the power of 1mw, the permanent magnet (6) is 30mm away from the shunt (9), and the current in the solenoid (12) is 4 amperes.
The photoelectron time flight spectrum measuring method comprises the following steps:
opening a gate valve (22), opening a vacuum pump III (23) to vacuumize a cold trap cavity (21), and opening a vacuum pump I (16) and a vacuum pump II (17) to vacuumize a flight cavity (15);
step two, opening a magnetic control valve to enable liquid nitrogen in the liquid nitrogen Dewar (25) to enter a liquid nitrogen cold trap (20) through a liquid nitrogen transmission pipe (24), and opening a controller to monitor signals of a lowest liquid level sensor (26), an alarm sensor (27) and a highest liquid level sensor (28);
step three, moving a nozzle (8) to a position near a flow divider (9) in an interaction cavity (4) through a displacement table (7), and conveying a solution sample to be detected to the nozzle (8) through a liquid inlet pipe (2) by the high performance liquid chromatography (1), wherein the solution sample to be detected forms tiny liquid drops after passing through the nozzle (8);
turning on the laser to enable the laser beam emitted by the laser to be emitted into a position near a nozzle (8) in the interaction cavity (4) along the x-axis direction, and enabling the laser to interact with micro liquid drops of the solution sample to be detected to generate photoelectrons;
step five, when working in a non-magnetic field mode, the permanent magnet (6) is arranged in the magnetic shielding chamber through the adjusting control lever (5), and the solenoid (12) is not supplied with current; when the device works in a magnetic bottle mode, the position of the permanent magnet (6) is adjusted through the operating rod (5), current is applied to the solenoid (12), and the collection angle of photoelectrons is changed by adjusting the position of the permanent magnet (6) and the current of the solenoid (12);
step six, photoelectrons in the collection angle enter a flight cavity (15) through a diverter (9), enter a micro-channel disc (14) after sequentially passing through a deceleration grid mesh (10) and a drift tube (13), and the micro-channel disc (14) transmits collected data to a computer;
and seventhly, processing the data obtained in the step six by a computer, and analyzing to obtain the relevant characteristics of the sample to be detected.
The invention adopts a method of combining a permanent magnet and a solenoid to generate magnetic fields with different shapes in an interaction area of laser and a sample molecule to be detected, thereby changing the collection angle of photoelectrons in time-of-flight spectrum measurement, and the magnetic field in a spectrometer can be switched between a magnetic field-free mode and a magnetic bottle mode so as to be suitable for an attosecond stripe technology and a two-photon transition interference attosecond pulse reconstruction technology.
Claims (1)
1. An optoelectronic time-of-flight spectrum measuring method comprises a high performance liquid chromatograph (1), a liquid inlet pipe (2), a recoverer (3), an interaction cavity (4), a control rod (5), a permanent magnet (6), a displacement table (7), a nozzle (8), a shunt (9), a reduction grid (10), a magnetic shielding cover (11), a solenoid (12), a drift tube (13), a micro-channel disk (14), a flight cavity (15), a vacuum pump I (16), a vacuum pump II (17), a liquid nitrogen inlet (18), a support table (19), a liquid nitrogen cold trap (20), a cold trap cavity (21), a gate valve (22), a vacuum pump III (23), a liquid nitrogen transmission pipe (24), a liquid nitrogen Dewar (25), a lowest liquid level sensor (26), an alarm sensor (27), a highest liquid level sensor (28), a gas-liquid separator (29), a nitrogen outlet, a laser, a magnetic control valve, a controller and a computer, wherein xyz is a three-dimensional space coordinate system, the interaction cavity (4) has a light transmission window, and laser beam emitted by the laser can enter the interaction cavity (4) along the x-axis direction, the flying cavity (15) is connected to the side surface of the interaction cavity (4) and is separated by the flow divider (9); the permanent magnet (6), the displacement table (7) and the nozzle (8) are all positioned in the interaction cavity (4), the nozzle (8) is arranged on the displacement table (7) and is connected with the high-performance liquid chromatograph (1) through the liquid inlet pipe (2), the position of the nozzle (8) can be adjusted through the displacement table (7), the operating lever (5) is arranged in the permanent magnet (6), a magnetic shielding chamber is arranged in the interaction cavity (4), the influence of the magnet positioned in the magnetic shielding chamber on the magnetic field outside the magnetic shielding chamber can be shielded, and the permanent magnet (6) can be arranged in the magnetic shielding chamber through adjusting the operating lever (5); magnetometer is installed in each of the interaction cavity (4) and the flying cavity (15) for monitoring the intensity and distribution of the magnetic field; the recoverer (3) is connected below the interaction cavity (4), and the recoverer (3) can collect samples which are ejected by the nozzle (8) and do not interact with laser; the speed reducing grid (10), the magnetic shielding cover (11), the solenoid (12), the drift tube (13) and the micro-channel disk (14) are all positioned in the flying cavity (15), the flying cavity (15) is respectively connected with the vacuum pump I (16) and the vacuum pump II (17), and the vacuum pump I (16) and the vacuum pump II (17) are simultaneously startedUnder the condition of (1), the vacuum degree of the flying cavity (15) can reach 10 at the highest -8 In the mbar level, the drift tube (13) is provided with a starting end and a tail end, the tail end of the drift tube (13) is connected with a micro-channel disc (14), and the micro-channel disc (14) is connected with a computer through a cable; the side of the cold trap cavity (21) is connected with a vacuum pump III (23) through a gate valve (22), the liquid nitrogen cold trap (20) is a cylindrical container with the height of 15cm and the inner diameter of 10cm, the upper end of the liquid nitrogen cold trap (20) is connected with the cold trap cavity (21) through a supporting table (19), the liquid nitrogen cold trap (20) is positioned in the cold trap cavity (21), the liquid nitrogen cold trap (20) is connected with a liquid nitrogen Dewar (25) through the supporting table (19), a liquid nitrogen inlet (18) and a liquid nitrogen transmission pipe (24), a magnetic control valve is arranged between the liquid nitrogen Dewar (25) and the liquid nitrogen transmission pipe (24), a lowest liquid level sensor (26), an alarm sensor (27) and a highest liquid level sensor (28) are respectively arranged in the liquid nitrogen cold trap (20) and are respectively connected to a controller outside the liquid nitrogen cold trap (20) through cables, the cables penetrate through the supporting table (19), the controller can control the state of the liquid nitrogen cold trap (20) according to the lowest liquid level sensor (26), the alarm sensor (27) and the highest liquid nitrogen sensor (28), the liquid nitrogen inlet (24) and the liquid nitrogen separator (29) can be separated from the liquid nitrogen inlet (24) through the liquid nitrogen transmission pipe (24), the device is excluded from a liquid nitrogen cold trap (20), one end of an operating rod (5) is positioned outside an interaction cavity (4), the position of a permanent magnet (6) can be adjusted through the operating rod (5), the permanent magnet (6) is a cylinder with the diameter of 20mm and the height of 30mm and is coaxial with the aperture of a diverter (9), the axis of a drift tube (13) is along the z-axis direction, a solenoid (12) is nested outside the drift tube (13), the drift tube (13) and the solenoid (12) are both positioned in a magnetic shielding cover (11), a speed reduction grid (10) is positioned between the diverter (9) and the initial end of the drift tube (13), the magnetic field intensity near the initial end of the drift tube (13) can be changed by adjusting the current in the solenoid (12), and different magnetic field shapes are formed among the diverter (9), a speed reduction grid (10) and the initial end of the drift tube (13); the speed reducing grid (10) consists of two identical grids which are woven by copper wires, the grids are square with the side length of 5mm, the grids of the grids are square with the side length of 0.2mm, the distance between the two grids is 0.8mm, and the speed is reducedThe speed grid mesh (10) can decelerate photoelectrons with larger kinetic energy; the lowest liquid level sensor (26) is 2cm away from the bottom surface of the liquid nitrogen cold trap (20), the alarm sensor (27) is 1cm away from the bottom surface of the liquid nitrogen cold trap (20), the highest liquid level sensor (28) is 1cm away from the top surface of the liquid nitrogen cold trap (20), PTFE pipes I, PTFE pipe II and PTFE pipe III with inner diameters of 6mm are respectively sleeved outside the lowest liquid level sensor (26), the alarm sensor (27) and the highest liquid level sensor (28), the PTFE pipe I and the PTFE pipe II are respectively provided with an opening at one end and a closing at one end, a cable connected with the lowest liquid level sensor (26) is bent obliquely upwards at a position 1cm away from the lowest liquid level sensor (26), the cable penetrates through the closing end of the PTFE pipe I and is sealed, and the opening direction of the PTFE pipe I is obliquely upwards at an angle of 45 degrees; a cable connected with an alarm sensor (27) passes through the closed end of the PTFE tube II and is sealed, the opening direction of the PTFE tube II is vertically downward, and two through holes with the diameter of 0.4mm are formed in the closed end; the aperture of the shunt (9) is 0.5mm, the inner diameter of the drift tube (13) is 30mm, the outer diameter is 34mm, the length is 400mm, the length of the solenoid (12) is 380mm, the inner diameter is 33mm, the solenoid (12) is wound by a single-layer coil with 200 turns, the thickness of an insulating layer at the outer side of the wire is 0.25mm, the magnetic shielding cover (11) is a mu-metal tube with the inner diameter of 95mm and the thickness of 3mm,
the method is characterized in that: the photoelectron time flight spectrum measuring method comprises the following steps:
opening a gate valve (22), opening a vacuum pump III (23) to vacuumize a cold trap cavity (21), and opening a vacuum pump I (16) and a vacuum pump II (17) to vacuumize a flight cavity (15);
step two, opening a magnetic control valve to enable liquid nitrogen in the liquid nitrogen Dewar (25) to enter a liquid nitrogen cold trap (20) through a liquid nitrogen transmission pipe (24), and opening a controller to monitor signals of a lowest liquid level sensor (26), an alarm sensor (27) and a highest liquid level sensor (28);
step three, moving a nozzle (8) to a position near a flow divider (9) in an interaction cavity (4) through a displacement table (7), and conveying a solution sample to be detected to the nozzle (8) through a liquid inlet pipe (2) by the high performance liquid chromatography (1), wherein the solution sample to be detected forms tiny liquid drops after passing through the nozzle (8);
turning on the laser to enable the laser beam emitted by the laser to be emitted into a position near a nozzle (8) in the interaction cavity (4) along the x-axis direction, and enabling the laser to interact with micro liquid drops of the solution sample to be detected to generate photoelectrons;
step five, when working in a non-magnetic field mode, the permanent magnet (6) is arranged in the magnetic shielding chamber through the adjusting control lever (5), and the solenoid (12) is not supplied with current; when the device works in a magnetic bottle mode, the position of the permanent magnet (6) is adjusted through the operating rod (5), current is applied to the solenoid (12), and the collection angle of photoelectrons is changed by adjusting the position of the permanent magnet (6) and the current of the solenoid (12);
step six, photoelectrons in the collection angle enter a flight cavity (15) through a diverter (9), enter a micro-channel disc (14) after sequentially passing through a deceleration grid mesh (10) and a drift tube (13), and the micro-channel disc (14) transmits collected data to a computer;
and seventhly, processing the data obtained in the step six by a computer, and analyzing to obtain the relevant characteristics of the sample to be detected.
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| JPH01251541A (en) * | 1988-03-31 | 1989-10-06 | Res Dev Corp Of Japan | High ionization ion source chamber |
| DE102007021701A1 (en) * | 2006-07-31 | 2008-02-07 | Bruker Daltonik Gmbh | Method for filling target volume with ions of different masses in time-of-flight mass spectrometer, involves ordering of ions either by mass-sequential extraction from storage device or by rearranging flight order of ions by bunching |
| CN101943664A (en) * | 2009-07-08 | 2011-01-12 | 中国科学院半导体研究所 | Spin dependent transport measurement system under strong magnetic field environment and liquid nitrogen temperature |
| CN109187458A (en) * | 2018-08-15 | 2019-01-11 | 金华职业技术学院 | A kind of gas molecule in space fluorometric investigation method |
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| JPH01251541A (en) * | 1988-03-31 | 1989-10-06 | Res Dev Corp Of Japan | High ionization ion source chamber |
| DE102007021701A1 (en) * | 2006-07-31 | 2008-02-07 | Bruker Daltonik Gmbh | Method for filling target volume with ions of different masses in time-of-flight mass spectrometer, involves ordering of ions either by mass-sequential extraction from storage device or by rearranging flight order of ions by bunching |
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