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CN-122013158-A - Device and method for taking ion reaction, characterization and deposition into consideration

CN122013158ACN 122013158 ACN122013158 ACN 122013158ACN-122013158-A

Abstract

The invention relates to the technical field of ion manipulation and characterization, in particular to a device and a method for simultaneously carrying out ion reaction, characterization and deposition. The device comprises an ion source module, an ion transmission cavity, a quadrupole mass screening cavity, a controllable ion molecule reaction cavity, a mass spectrum characterization cavity, an ion acceleration cavity, a magnetic deflection cavity and an ion deceleration and deposition cavity, wherein ions are screened by using a soft ionization set quadrupole analyzer, reaction synthesis is controlled by a reaction chamber, and reaction product mass spectrum characterization and high-flux preparation are realized by integrating a mass spectrum analyzer and a magnetic field deflector. The invention can realize the integration of ion reaction, characterization and deposition, and has wide application prospect in the fields of organic synthesis mechanism research, high-efficiency preparation of macromolecules or macromolecules and the like.

Inventors

  • JIANG JICHUN
  • HUA LEI
  • ZHANG ZHENYUAN
  • LI JINXU
  • WANG WEIGUO
  • LI HAIYANG

Assignees

  • 中国科学院大连化学物理研究所

Dates

Publication Date
20260512
Application Date
20241111

Claims (10)

  1. 1. The device for simultaneously carrying out ion reaction, characterization and deposition is characterized by comprising an ion source module (1), an ion transmission cavity (2), a quadrupole mass screening cavity (3), a controllable ion molecule reaction cavity (4), a mass spectrum characterization cavity (5), an ion acceleration cavity (6), a magnetic deflection cavity (9) and an ion deceleration and deposition cavity (7) which are sequentially arranged; The ion source module (1) is used for ionizing compounds; The ion transmission cavity (2) is internally provided with a high-efficiency ion transmission module (15) used for transmitting ions generated by the ion source module (1) to the quadrupole mass screening cavity (3), the quadrupole mass screening cavity (3) is internally provided with a quadrupole rod separation module (14) used for screening ions and introducing controllable ion molecule reaction cavities (4), the controllable ion molecule reaction cavities (4) are internally provided with an electric field controlled ion molecule reaction module (13) used for controlling ion and molecule reactions and transmitting reaction products to the mass spectrum characterization cavity (5), the mass spectrum characterization cavity (5) is internally provided with a high-resolution mass analyzer module (12) used for carrying out accurate mass-to-charge ratio characterization on the ions of reactants, intermediate products and final products introduced by the controllable ion molecule reaction cavities (4), the ion acceleration cavity (6) is internally provided with an ion acceleration module (11) used for accelerating the introduced ions, the magnetic deflection cavity (9) is internally provided with a magnetic deflector (10) used for deflecting the introduced high-speed ions, the ions with the same energy and different mass-to-charge ratio deflection radiuses can be separated in space and can be reduced in the ion acceleration cavity (7) and the deposition cavity (8) is further provided with a plurality of reduction modules.
  2. 2. The apparatus according to claim 1, wherein the ion source module (1) is one or more of an electrospray ionization source, an atmospheric pressure photo-ionization source, a dielectric barrier discharge ionization source, a paper spray ionization source, and a low pressure ionization source such as an electron bombardment ionization source, a single photon ionization source, a multiphoton ionization source, and a chemical ionization source.
  3. 3. The apparatus of claim 1, wherein the high-efficiency ion transport module (15) is one or more of a radio frequency ion funnel, a radio frequency multipole, a radio frequency profiled multipole, and an electrostatic lens.
  4. 4. The apparatus according to claim 1, wherein the quadrupole rod separation module (14) is a cylindrical or hyperbolic quadrupole rod analyzer with adjustable resolution, and the resolution adjustment range is 0.5-50 amu in half-peak width.
  5. 5. The device for ion reaction, characterization and deposition according to claim 1, wherein the ion molecular reaction module (13) is one of a segmented radio frequency multipole rod, a traveling wave ring electrode group and a special-shaped radio frequency multipole rod, and the working gas pressure can be tuned between 0.1 Pa and 100 Pa.
  6. 6. The apparatus of claim 1, wherein the high resolution mass analyzer module (12) is one of a time-of-flight mass analyzer, an orbitrap analyzer, and a Fourier transform ion cyclotron resonance mass analyzer, and the mass resolution is greater than 10000.
  7. 7. The device for simultaneously carrying out ion reaction, characterization and deposition according to claim 1, wherein the ion acceleration module (11) comprises a plurality of circular ring electrodes, the circular ring electrodes are connected through equivalent resistors, the ions are accelerated by applying voltages to the front end and the rear end of the circular ring electrodes, and the accelerating electric field formed inside the circular ring electrodes has accelerating energy of 1000-10000 eV.
  8. 8. The device for simultaneously carrying out ion reaction, characterization and deposition according to claim 1, wherein the magnetic deflector (10) is composed of a permanent magnet or an electromagnet independently, an auxiliary tuning electrostatic field energy screener is added, the spatial resolution is improved, and the magnetic field strength is 10000-40000 Gs.
  9. 9. The apparatus of claim 1, wherein the multi-channel ion deceleration and deposition module (8) is comprised of a multi-stage electrostatic deceleration lens, a deposition substrate, a current measurement and a luminescent screen imaging combination.
  10. 10. A method of using the apparatus of any one of claims 1-9, wherein the apparatus is configured to perform ion reaction, characterization and deposition simultaneously: the application method comprises the following steps: a. The sample with target reactant molecules enters an ion source module (1), the ion source module (1) ionizes the sample entering the ion source module, and ions generated after ionization are transmitted to an ion transmission cavity (2); b. ions entering the ion transmission cavity (2) are efficiently transmitted to the next-stage quadrupole mass screening cavity (3) under the action of the efficient ion transmission module (15); c. Setting the working mode of a quadrupole rod separation module (14) as ion full-pass, setting an ion molecule reaction module (13) in a controllable ion molecule reaction cavity (4) as ion non-reaction full-pass, enabling ions to directly enter a high-resolution mass analyzer module (12) in a mass spectrum characterization cavity (5) for mass spectrum characterization, and evaluating the generation distribution of reactant ions; d. According to the evaluation result of the high-resolution mass analyzer module (12), regulating and controlling the working voltage of the quadrupole rod separation module (14), namely selecting a target reactant ion mass-to-charge ratio interval for reaction, evaluating again through the high-resolution mass analyzer module (12), and observing the ion purity screened by the quadrupole rod separation module (14); e. the parameters of a quadrupole rod separation module (14) are determined and fixed after being evaluated by a high-resolution mass analyzer module (12), meanwhile, the working voltage, the air pressure and the carrier gas parameters of an ion molecule reaction module (13) in a controllable ion molecule reaction cavity (4) are controlled, the reaction between ions and reaction carrier gas molecules is carried out in the ion molecule reaction module (13), and meanwhile, the ions generated after the reaction are introduced into the high-resolution mass analyzer module (12) in a mass spectrum characterization cavity (5) for mass spectrum characterization, and each parameter of the ion molecule reaction module (13) in the controllable ion molecule reaction cavity (4) is regulated and controlled and determined according to the characterization result; f. After each parameter of an ion molecular reaction module (13) is determined, the ions generated by reaction are introduced into an ion acceleration module (11) in an ion acceleration cavity (6) and accelerated to 1000-10000 eV, the accelerated high-energy ion beam is introduced into a magnetic deflection cavity (9), and different-mass ions are deflected with different radiuses through a magnetic deflector (10) in the magnetic deflection cavity (9) to realize space separation; g. Ions spatially separated by the magnetic deflector (10) enter the ion deceleration and deposition chamber (7), are decelerated by a multistage electrostatic deceleration lens in the ion deceleration and deposition module (8), and are finally deposited on the substrate without damage.

Description

Device and method for taking ion reaction, characterization and deposition into consideration Technical Field The invention relates to the technical field of ion manipulation and characterization, in particular to a device and a method for simultaneously carrying out ion reaction, characterization and deposition. Background Reaction synthesis, characterization and preparation of organic matter have been hot spots of research in the field of materials, however, precise reaction control, characterization and high-throughput preparation means are lacking for complex, weakly stable and highly active systems. The reaction is accurately controlled, the reaction can be regulated and controlled by selecting ions through mass-to-charge ratio, the characterization can select mass spectrum to carry out accurate mass-to-charge ratio measurement, and the preparation method of the high-purity sample is always a research hot spot. The common preparation methods such as chemical vapor deposition and physical vapor deposition have the characteristics of simple operation and large preparation amount, but are easy to be interfered by gas components in the preparation process and are difficult to be used for in-situ reaction preparation. Preparation of mass Spectrometry (pMS) is a technique for precisely screening and preparing ions with specific mass to charge ratio (m/z) with high purity by using mass Spectrometry as a separation means, and particularly, the ion soft landing (soft-l and i ng) technique (Ana lyst,2012,137,4393) developed in recent decades can maintain the integrity of molecular structure and function during deposition, so as to realize high-selectivity, high-purity and high-fidelity preparation of target molecules in a high-vacuum environment. Therefore, the integrated design of reaction control, characterization and preparation is expected to play an important role in the research of synthesis mechanism. By searching the patent and the paper, the related patent is that the ion soft deposition device is disclosed in the university of academy of sciences of China and the institute of chemical and physical research 2023, 3 and 3 days. According to the invention, ion deposition energy is controlled through ion deceleration, ion visual imaging is performed through the MCP fluorescent screen, so that the deposition efficiency of a unit area is reduced, and the mass spectrum preparation can be assisted to realize more efficient sample preparation. The invention is mainly focused on deposition control, no ion reaction, characterization and high flux deposition schemes. The national academy of sciences Dalian chemical and physical institute 2024, 5 and 21 days discloses a preparation mass spectrum and a use method, which mainly comprise a soft ionization source, an ion transmission system, a quadrupole rod separation system, a high-resolution mass spectrum and a deposition system. The invention uses high-resolution mass spectrum for preparing ion characterization after mass spectrum separation, so that the mass spectrum parameter can be prepared in a feedback and optimization mode, the preparation efficiency is improved, but the invention lacks ion reaction control and the preparation flux of the method is lower. Thus, there is currently a lack of accurate reaction control, characterization and high-throughput preparation means for complex, poorly stable and highly active systems. Disclosure of Invention Aiming at the problems existing in the prior art, the invention aims to provide a device and a method for simultaneously carrying out ion reaction, characterization and deposition, so as to realize the integrated research of the ion reaction, the characterization and the deposition. In order to achieve the above purpose, the present invention adopts the following technical scheme: The invention provides a device for taking ion reaction, characterization and deposition into consideration, which comprises an ion source module, an ion transmission cavity, a quadrupole mass screening cavity, a controllable ion molecule reaction cavity, a mass spectrum characterization cavity, an ion acceleration cavity, a magnetic deflection cavity and an ion deceleration and deposition cavity which are sequentially arranged; The ion source module is used for ionizing the compound; The ion transmission cavity is internally provided with a high-efficiency ion transmission module used for transmitting ions generated by the ion source module to a quadrupole mass screening cavity, the quadrupole mass screening cavity is internally provided with a quadrupole rod separation module used for screening ions and introducing controllable ion molecule reaction cavities, the controllable ion molecule reaction cavities are internally provided with an electric field controlled ion molecule reaction module used for controlling ion and molecule reactions and transmitting reaction products to a mass spectrum characterization cavity, the mass spectrum char