Nanomaterial Preparation and Characterization System

Abstract

The present invention provides a nano material preparation and characterization system, comprising: a beam generating component, which is suitable for generating an initial nano cluster beam; a deposition component, which is suitable for depositing the initial nano cluster beam under the action of an external field to obtain a target nano material; a characterization component, which is suitable for characterizing the chemical properties and physical properties of the target nano material; and a sample transfer component, which is suitable for transporting the target nano material to the characterization component in a vacuum environment, so that the physical or chemical properties of the target nano material remain unchanged during the transfer process, thereby completing the characterization of the physical or chemical properties of the target nano material.

Description

Technical Field

[0001] At least one embodiment of the present invention relates to the technical field of material preparation and characterization, and more specifically to a nanomaterial preparation and characterization system. Background Art

[0002] Multi-scale, in-situ, high-resolution catalytic characterization technology is of great significance for understanding the mechanism of catalytic reactions at the microscopic scale. The synthesis and preparation instruments of catalytic functional materials with unique structures can achieve the goal of constructing catalysts at the atomic level and understanding the mechanism and kinetics of catalytic reactions at the molecular level.

[0003] In the relevant nanomaterial preparation technology, since the nanomaterials need to be spatially transferred to the characterization equipment after preparation, and the physical or chemical properties of the prepared nanomaterials will change during the transfer process, affecting the subsequent characterization and analysis of the nanomaterials, the relevant nanomaterial preparation technology cannot realize the online preparation and online characterization of nanomaterials, and cannot ensure that the background environment for the preparation of nanomaterials and the characterization of nanomaterials are the same. Summary of the invention

[0004] In order to solve at least one of the above-mentioned and other technical problems in the prior art, the present invention provides a nanomaterial preparation and characterization system, which can realize the online preparation and online characterization of nanomaterials, ensure that the background environment of the preparation of nanomaterials and the characterization of nanomaterials is the same, and can realize the manipulation and characterization of nanomaterials at the nanoscale in space and the atomic level in mass resolution.

[0005] According to one aspect of the present invention, a nanomaterial preparation and characterization system is provided, comprising:

[0006] A beam generation assembly, adapted to generate an initial nanocluster beam;

[0007] A deposition component, adapted to deposit the initial nanocluster beam under the action of an external field to obtain a target nanomaterial;

[0008] Characterization components, suitable for characterizing the chemical and physical properties of the above-mentioned target nanomaterials; and

[0009] The sample transfer component is suitable for transporting the above-mentioned target nanomaterial to the above-mentioned characterization component under a vacuum environment, so that the physical and chemical properties of the above-mentioned target nanomaterial remain unchanged during the transfer process, thereby completing the characterization of the physical and chemical properties of the above-mentioned target nanomaterial.

[0010] According to an embodiment of the present invention, the nanomaterial preparation and characterization system further includes:

[0011] A beam shaping component adapted to adjust the size, shape or transmission speed of the initial nanocluster beam; and

[0012] A mass selection component, adapted to perform mass selection on the initial nanocluster beam adjusted by the beam shaping component to obtain a first nanocluster beam containing nanoparticles of a target size;

[0013] Wherein, the first nanocluster beam is deposited through the deposition assembly to form the target nanomaterial.

[0014] According to an embodiment of the present invention, the nanomaterial preparation and characterization system further includes: a low-temperature ion flight tube, which is suitable for temperature control of the first nanocluster beam to maintain the stability of the first nanocluster beam.

[0015] According to an embodiment of the present invention, the nanomaterial preparation and characterization system further includes: a mass spectrometry component adapted to perform mass spectrometry analysis on the first nanocluster beam to obtain the constituent elements and size distribution of the first nanocluster beam.

[0016] According to an embodiment of the present invention, the beam shaping assembly comprises an electrostatic quadrupole deflection lens, and the electrostatic quadrupole deflection lens comprises four symmetrical electrodes.

[0017] By adjusting the voltages applied to the four symmetrical electrodes respectively, a rotationally symmetric electrostatic field is formed, and the electrostatic field is suitable for deflecting and focusing the initial nanocluster beam incident between the four symmetrical electrodes, thereby changing the size, shape or transmission speed of the initial nanocluster beam.

[0018] According to an embodiment of the present invention, the mass selection component is a quadrupole mass selector, and a radio frequency bias electric field is applied to the outside of the mass selection component, so that ions with the target number of atoms can pass through the mass selection component, thereby obtaining the first nanocluster beam containing ions with the target number of atoms.

[0019] According to an embodiment of the present invention, the above-mentioned nanomaterial preparation and characterization system also includes a sample transmission component, and the two ends of the above-mentioned sample transmission component are respectively connected to the above-mentioned deposition component and the above-mentioned mass spectrometry component. The above-mentioned sample transmission component includes a magnetic rod and a manipulator, and the above-mentioned magnetic rod is suitable for transporting the above-mentioned target nanomaterial obtained by the above-mentioned deposition component to the above-mentioned characterization component.

[0020] According to an embodiment of the present invention, the beam generating assembly includes any one or a combination of the following:

[0021] Magnetron sputtering ion source, thermal evaporation ion source, laser ablation ion source, arc discharge ion source, electrospray ion source, matrix-assisted laser desorption ionization source, atmospheric pressure chemical ionization source and atmospheric pressure photoionization source.

[0022] According to an embodiment of the present invention, the nanomaterial preparation and characterization system further includes a sample pretreatment component, which is configured to change the catalytic properties of the target nanomaterial by reacting the external reaction gas input into the sample pretreatment component with the target nanomaterial from the deposition component, and to transport the target nanomaterial with changed catalytic properties to the characterization component.

[0023] According to an embodiment of the present invention, the deposition assembly comprises:

[0024] A temperature-controlled sample stage, adapted to adjust the deposition temperature of the target nanomaterial and the deposition rate of the target nanomaterial; and

[0025] The displacement component is suitable for adjusting the position of the temperature-controlled sample stage.

[0026] According to an embodiment of the present invention, an initial nanocluster beam is generated by utilizing a beam generating component, an initial nanocluster beam is deposited by utilizing a deposition component under the action of an external field to obtain a target nanomaterial, a characterization component is utilized to characterize the chemical and physical properties of the target nanomaterial, and a sample transfer component is utilized to transport the target nanomaterial to the characterization component under a vacuum environment so that the physical and chemical properties of the target nanomaterial remain unchanged during the transfer process, thereby completing the characterization of the physical and chemical properties of the target nanomaterial, realizing online preparation and online characterization of nanomaterials, ensuring that the background environments for the preparation of nanomaterials and the characterization of nanomaterials are the same, and realizing the manipulation, preparation and characterization of nanomaterials at the nanoscale in space and at the atomic level in mass resolution. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] The above contents and other objects, features and advantages of the present invention will become more apparent through the following description of the embodiments of the present invention with reference to the accompanying drawings, in which:

[0028] Figure 1 A stereogram of a nanomaterial preparation and characterization system according to an embodiment of the present invention is shown;

[0029] Figure 2 A cross-sectional view of a beam generating component, a beam shaping component, and a mass selecting component in a nanomaterial preparation and characterization system according to an embodiment of the present invention is shown;

[0030] Figure 3 A working principle diagram of a nanomaterial preparation and characterization system in a mass spectrometry measurement mode according to an embodiment of the present invention is shown;

[0031] Figure 4 A working principle diagram of a nanomaterial preparation and characterization system in a deposition mode according to an embodiment of the present invention is shown;

[0032] Figure 5 A cross-sectional view of a sample transmission component in a nanomaterial preparation and characterization system according to an embodiment of the present invention is shown;

[0033] Figure 6 A schematic diagram of the vacuum layout of a nanomaterial preparation and characterization system according to an embodiment of the present invention is shown.

[0034] In the above drawings, the meanings of the reference numerals are as follows:

[0035] 1- beam generating assembly;

[0036] 121-magnetron sputtering ion source;

[0037] 1211-target;

[0038] 1212- aperture;

[0039] 1213-Ion guide;

[0040] 122-electrospray ion source;

[0041] 2- beam shaping assembly;

[0042] 21-Electrostatic quadrupole deflection lens;

[0043] 3-Quality selection components;

[0044] 4-Cryogenic ion flight tube;

[0045] 5-Mass spectrometry component;

[0046] 51-Wiley-Mclaren lens set;

[0047] 52-ion acceleration / deceleration lens group;

[0048] 53-microchannel plate detector;

[0049] 54-reflective lens group;

[0050] 6-Deposition assembly;

[0051] 61-temperature controlled sample stage;

[0052] 7- Characterization components;

[0053] 71-confocal Raman microscope;

[0054] 72- Fourier transform infrared spectrometer;

[0055] 73-UV-visible spectrometer;

[0056] 8-sample transmission assembly;

[0057] 81-magnetic rod;

[0058] 82-vacuum gate valve;

[0059] 83-Quick-opening door with window;

[0060] 84- bellows;

[0061] 85-Vacuum load lock;

[0062] 9-sample transfer assembly;

[0063] 10-sample pretreatment component;

[0064] 101-Multistage rotary vane pump;

[0065] 102-worm gear dry vacuum pump;

[0066] 103-Multi-stage Roots pump unit;

[0067] 104-a first turbomolecular pump;

[0068] 105-second worm gear molecular pump;

[0069] 106- the third worm gear molecular pump;

[0070] 107- fourth worm gear molecular pump;

[0071] 108-fifth worm gear molecular pump;

[0072] 109-sixth worm gear molecular pump;

[0073] 110-seventh worm gear molecular pump;

[0074] 111-eighth worm gear molecular pump;

[0075] 112-9th worm gear molecular pump;

[0076] 113-the tenth worm gear molecular pump;

[0077] a-injection cone;

[0078] b-The first nanocluster beam. DETAILED DESCRIPTION

[0079] Below, embodiments of the present invention will be described with reference to the accompanying drawings. However, it should be understood that these descriptions are exemplary only and are not intended to limit the scope of the present invention. In the following detailed description, for ease of explanation, many specific details are set forth to provide a comprehensive understanding of embodiments of the present invention. However, it is apparent that one or more embodiments may also be implemented without these specific details. In addition, in the following description, descriptions of known structures and technologies are omitted to avoid unnecessary confusion of concepts of the present invention.

[0080] The terms used herein are only for describing specific embodiments and are not intended to limit the present invention. The terms "comprise", "include", etc. used herein indicate the existence of the features, steps, operations and / or components, but do not exclude the existence or addition of one or more other features, steps, operations or components.

[0081] All terms (including technical and scientific terms) used herein have the meanings commonly understood by those skilled in the art unless otherwise defined. It should be noted that the terms used herein should be interpreted as having a meaning consistent with the context of this specification and should not be interpreted in an idealized or overly rigid manner.

[0082] When using expressions such as "at least one of A, B, and C, etc.", they should generally be interpreted according to the meaning of the expression commonly understood by those skilled in the art (for example, "a system having at least one of A, B, and C" should include but is not limited to a system having A alone, B alone, C alone, A and B, A and C, B and C, and / or A, B, C, etc.).

[0083] In the relevant nanomaterial preparation technology, the nanomaterial needs to be spatially transferred to the characterization equipment after preparation, and the physical or chemical properties of the prepared nanomaterial will change during the transfer process, affecting the subsequent characterization and analysis of the nanomaterial. Therefore, the relevant nanomaterial preparation technology cannot achieve the characterization of the nanomaterial while preparing the nanomaterial.

[0084] In view of this, the present invention provides a nanomaterial preparation and characterization system, which generates an initial nanocluster beam by using a beam generating component, deposits the initial nanocluster beam by using a deposition component under the action of an external field to obtain a target nanomaterial, characterizes the chemical properties and physical properties of the target nanomaterial by using a characterization component, and transports the target nanomaterial to the characterization component under a vacuum environment by using a sample transfer component so that the physical and chemical properties of the target nanomaterial remain unchanged during the transfer process, thereby completing the characterization of the physical and chemical properties of the target nanomaterial, realizing online preparation and online characterization of nanomaterials, ensuring that the background environment for the preparation of nanomaterials and the characterization of nanomaterials is the same, and realizing the controlled preparation and characterization of nanomaterials at the nanoscale in space and the atomic level in mass resolution.

[0085] Figure 1 A three-dimensional diagram of a nanomaterial preparation and characterization system according to an embodiment of the present invention is shown.

[0086] According to some embodiments of the present invention, Figure 1 As shown, the nanomaterial preparation and characterization system includes a beam generating component 1, a deposition component 6, a characterization component 7, and a sample transfer component 9. The beam generating component 1 is suitable for generating an initial nanocluster beam; the deposition component 6 is suitable for depositing the initial nanocluster beam under the action of an external field to obtain a target nanomaterial; the characterization component 7 is suitable for characterizing the chemical and physical properties of the target nanomaterial; and the sample transfer component 9 is suitable for transporting the target nanomaterial to the characterization component 7 under a vacuum environment, so that the physical and chemical properties of the target nanomaterial remain unchanged during the transfer process, thereby completing the characterization of the physical and chemical properties of the target nanomaterial.

[0087] According to some embodiments of the present invention, a beam generating component 1 is provided to generate an initial nanocluster beam, a deposition component 6 is used to deposit the initial nanocluster beam under the action of an external field to obtain a target nanomaterial, a characterization component 7 is used to characterize the chemical and physical properties of the target nanomaterial, and a sample transfer component 9 is used to transport the target nanomaterial to the characterization component 7 under a vacuum environment so that the physical and chemical properties of the target nanomaterial remain unchanged during the transfer process, thereby completing the characterization of the physical and chemical properties of the target nanomaterial, realizing online preparation and online characterization of nanomaterials, ensuring that the background environment for the preparation of nanomaterials and the characterization of nanomaterials is the same, realizing the manipulation, preparation and characterization of nanomaterials at the nanoscale in space and the atomic level in mass resolution, and the above-mentioned nanomaterial preparation and characterization system realizes the preparation of nanoparticles with atomic-level precision, the preparation of small molecules and / or large molecules with a determined mass number, online nanoparticle deposition and dispersion control, and multi-scale, in-situ, high-resolution manipulation and characterization.

[0088] According to some embodiments of the present invention, the beam generating component 1, the deposition component 6, the characterization component 7 and the sample transfer component 9 are all placed in an ultra-high vacuum chamber, and the ultra-high vacuum chambers in which they are located are separated and connected by partitions with through holes, and the edges of the partitions are sealed with the ultra-high vacuum chamber.

[0089] According to some embodiments of the present invention, the beam generating assembly 1 includes any one or a combination of the following: a magnetron sputtering ion source, a thermal evaporation ion source, a laser ablation ion source, an arc discharge ion source, an electrospray ion source, a matrix-assisted laser desorption ionization source, an atmospheric pressure chemical ionization source, and an atmospheric pressure photoionization source.

[0090] According to some embodiments of the present invention, when the beam generating assembly 1 is equipped with multiple ion sources, only one of the ion sources is in operation.

[0091] According to some embodiments of the present invention, the beam generating assembly 1 can generate common metals (stable metals such as Au, Ag, Pt, Cu, Ni, Cr, Pb, Sn, Pd, V, Zn, Rh, Nb, Mo, W, Mg, Mn, etc.) / metal oxides (TiO 2 、V 2 O 5 、ZnO、NiO、Fe 2 O 3 SnO 2 , CuO, ZrO 2 Cluster nanoparticle beam of stable solid metal oxides (such as metal oxides) / alloys (alloys can be binary and ternary) / non-metals (stable solid non-metals such as Si, C, B, S, P) / small molecules / macromolecules / organic molecules.

[0092] According to some optional embodiments of the present invention, the beam generating component 1 includes a magnetron sputtering ion source 121 and an electrospray ion source 122. The magnetron sputtering ion source can replace targets of different compositions and ingredients according to demand. Under the joint action of the internal electric field and magnetic field, the target produces metal, metal oxide, alloy, and non-metal cluster nanoparticles; the electrospray ion source 122 transfers different small molecules and macromolecule nanoparticles from the liquid phase to the gas phase and ionizes them through the injection cone a to form an initial nanocluster beam. The magnetron sputtering ion source 121 and the electrospray ion source 122 do not work at the same time. By integrating the beam generating component 1 with multiple ion sources including the magnetron sputtering ion source 121 and the electrospray ion source 122, different ions can be generated to cope with the ions required for different experiments.

[0093] According to some embodiments of the present invention, the magnetron sputtering ion source 121 is mainly used to analyze compounds with low volatility, including materials such as metals and semiconductors. The types of ions generated by the magnetron sputtering ion source 121 include singly charged ions, which are suitable for analysis of inorganic and some organic substances. The magnetron sputtering ion source 121 is usually operated under vacuum conditions, and the pressure and temperature need to be strictly controlled; the magnetron sputtering ion source 121 equipment is relatively complex and requires precise control of the magnetic field and electric field.

[0094] According to some embodiments of the present invention, the electrospray ion source 122 is widely used in the analysis of biomacromolecules, such as proteins, nucleic acids, etc.; the ion types generated by the electrospray ion source 122 include multiply charged ions, which are suitable for analyzing large molecular weight organic molecules; the electrospray ion source 122 needs to operate under atmospheric pressure, and has low environmental requirements, but requires stable liquid flow rate and voltage. The equipment of the electrospray ion source 122 is relatively simple, but requires fine adjustment of the liquid flow rate and spray voltage. According to some optional embodiments of the present invention, the nanoparticles in the initial nanocluster beam generated by the beam generating component 1 generally have a wide size distribution, such as nanoparticles composed of 1-n copper atoms (Cu 1 , Cu 2 ,……,Cu n ).

[0095] According to some optional embodiments of the present invention, the characterization component 7 includes any one or combination of the following: scanning electron microscope, focused ion beam, scanning transmission electron microscope, scanning tunneling microscope, atomic force microscope, X-ray diffractometer, X-ray spectrometer, X-ray photoelectron spectrometer, Auger electron spectrometer, confocal micro-Raman spectroscopy, Fourier transform infrared spectroscopy, ultraviolet-visible spectroscopy and secondary ion mass spectrometry. By setting the characterization component 7 to any one of the above instruments or a combination of several instruments, high-resolution characterization of multiple scales of target nanomaterials is achieved.

[0096] According to some optional embodiments of the present invention, Figure 1 As shown, the characterization component 7 includes a confocal Raman microscope 71 , a Fourier transform infrared spectrometer 72 and a UV-visible spectrometer 73 .

[0097] According to some embodiments of the present invention, the nanomaterial preparation and characterization system further includes a beam shaping component 2 and a mass selection component 3. The beam shaping component 2 is suitable for adjusting the size, shape or transmission speed of the initial nanocluster beam; the mass selection component 3 is suitable for mass selection of the initial nanocluster beam adjusted by the beam shaping component 2 to obtain a first nanocluster beam containing nanoparticles of a target size; wherein the first nanocluster beam is deposited by the deposition component 6 to form the target nanomaterial.

[0098] According to some embodiments of the present invention, the size, shape or transmission speed of the initial nanocluster beam is adjusted by setting a beam shaping component 2, so as to achieve transmission and shaping of the initial nanocluster beam; the mass selection component 3 is used to perform mass selection on the initial nanocluster beam adjusted by the beam shaping component 2 to obtain a first nanocluster beam containing nanoparticles of a target size; the first nanocluster beam is deposited by a deposition component 6 to form a target nanomaterial.

[0099] According to some optional embodiments of the present invention, the beam shaping component 2 includes any one or a combination of the following: an electrostatic quadrupole deflection lens 21, an ion guide, a single lens, a beam deflection lens, a strong focusing lens, an acceleration lens, a deceleration lens, an ion guide, a deflection electrode, an ion funnel and an ion drift tube.

[0100] According to some optional embodiments of the present invention, when the beam generating component 1 is a combination of multiple ion sources, the cluster nanoparticles generated by the multiple ion sources are clustered together to form an initial nanocluster beam, and the beam shaping component 2 is suitable for focusing, offsetting, deflecting, accelerating, decelerating, etc. the initial nanocluster beam.

[0101] According to some optional embodiments of the present invention, the mass selection component 3 includes any one of a quadrupole mass selector, an aerodynamic lens, a transverse flight time mass selector, a magnetic sector mass selector and a quadrupole deflector.

[0102] According to some optional embodiments of the present invention, the mass selection component 3 is a quadrupole mass selector, and a radio frequency bias electric field is applied to the outside of the mass selection component 3, so that ions with a target number of atoms can pass through the mass selection component 3, thereby obtaining a first nanocluster beam containing ions with a target number of atoms.

[0103] According to some embodiments of the present invention, by setting the mass selection component 3 to select and obtain the first nanocluster beam containing ions of the target number of atoms, the relationship between the structure of the target nanomaterial formed by the first nanocluster beam after deposition by the deposition component 6 and the performance of the target nanomaterial can be obtained, and then the target nanomaterial with a specific surface structure and function can be prepared. For example, the target nanomaterial has a catalytic function, and the catalytic activity and selectivity of the prepared target nanomaterial can be controlled by regulating the reaction occurring during the preparation process of the target nanomaterial.

[0104] According to some embodiments of the present invention, since nanoparticles of different sizes have different physical / chemical properties, it is necessary to screen out cluster nanoparticles of the desired atomic number from the initial nanocluster beam with a wide size distribution. The initial nanocluster beam with a wide size distribution generated by the beam generating component 1 is transmitted / shaped by the beam shaping component 2 to the mass selection component 3. The mass selection component 3 can screen out the first nanocluster beam containing ions of the target atomic number.

[0105] According to some embodiments of the present invention, Figure 1 As shown, the nanomaterial preparation and characterization system further includes a low-temperature ion flight tube 4, which is suitable for temperature control of the first nanocluster beam to maintain the stability of the first nanocluster beam.

[0106] According to some embodiments of the present invention, the temperature of the first nanocluster beam is controlled by setting a low-temperature ion flight tube 4, thereby maintaining the stability of the first nanocluster beam and being able to study the quantum behavior, interaction and phase change process of the first nanocluster beam in a low-temperature environment.

[0107] According to some embodiments of the present invention, the low-temperature ion flight tube is connected to a cold head, and the cold head cools the low-temperature ion flight tube by directly contacting the low-temperature ion flight tube, thereby reducing the temperature of the low-temperature ion flight tube.

[0108] Figure 2 A cross-sectional view of a beam generating component, a beam shaping component, and a mass selecting component in a nanomaterial preparation and characterization system according to an embodiment of the present invention is shown.

[0109] According to some embodiments of the present invention, Figure 2 As shown, the beam generating component 1 includes a target 1211, an aperture 1212 and an ion guide 1213; the beam shaping component 2 includes an electrostatic quadrupole deflection lens 21; and the mass selection component 3 includes an ion flight tube, which is suitable for screening out a first nanocluster beam containing ions of a target mass-to-charge ratio.

[0110] According to some embodiments of the present invention, the beam shaping component 2 includes an electrostatic quadrupole deflection lens 21, which includes four symmetrical electrodes, wherein a rotationally symmetric electrostatic field is formed by adjusting the voltages applied to the four symmetrical electrodes respectively, and the electrostatic field is suitable for deflecting and focusing the initial nanocluster beam incident between the four symmetrical electrodes, thereby changing the size, shape or transmission speed of the initial nanocluster beam.

[0111] According to some embodiments of the present invention, Figure 2As shown, the magnetron sputtering ion source 121 includes a target material 1211 and an aperture 1212. The aperture of the aperture 1212 is adjustable, and the magnetron sputtering ion source can replace the target material 1211 with different compositions and ingredients according to the needs. The target material 1211 produces metal, metal oxide, alloy, non-metal cluster nanoparticles under the combined action of the internal electric field and magnetic field; the size distribution of the generated cluster nanoparticles is changed by adjusting the aperture of the aperture 1212.

[0112] According to some embodiments of the present invention, the beam generation component 1 is coupled to the mass selection component 3 via an ion guide 1213. The ion guide 1213 is adapted to guide the transmission of the nanocluster beam under the action of an external electric field.

[0113] Figure 3 The figure shows the working principle of the nanomaterial preparation and characterization system in the mass spectrometry measurement mode according to an embodiment of the present invention.

[0114] According to some embodiments of the present invention, Figure 3 As shown, the nanomaterial preparation and characterization system further includes a mass spectrometry component 5, which is suitable for performing mass spectrometry analysis on the first nanocluster beam to obtain the constituent elements and size distribution of the first nanocluster beam.

[0115] According to some embodiments of the present invention, by performing mass spectrometry analysis on the first nanocluster beam using the mass spectrometry component 5, the mass-to-charge ratio of the first nanocluster beam can be obtained, the molecular weight of the first nanocluster beam can be obtained, and the constituent elements, size distribution and proportions of the first nanocluster beam can be obtained.

[0116] According to some optional embodiments of the present invention, the mass spectrometry component 5 is a Wiley-Mclaren time-of-flight mass spectrometry device.

[0117] According to some optional embodiments of the present invention, Figure 3 As shown, the mass spectrometer assembly 5 includes a Wiley-Mclaren lens group 51 , an ion acceleration / deceleration lens group 52 , a microchannel plate detector 53 , and a reflection lens group 54 .

[0118] According to some embodiments of the present invention, the nanomaterial preparation and characterization system operates in a mass spectrometry measurement mode, and a nanocluster beam with a specific mass-to-charge ratio (i.e., the first nanocluster beam b) is transmitted to the low-temperature ion flight tube 4 through the ion guide 1213 for temperature control. The first nanocluster beam b after temperature control by the low-temperature ion flight tube 4 is transmitted to the ion focusing and deflection lens group for focusing and deflection. The first nanocluster beam b after focusing and deflection by the ion focusing and deflection lens group is transmitted to the ion acceleration / deceleration lens group for speed regulation. After the acceleration / deceleration lens group is adjusted to the required kinetic energy, the first nanocluster beam b is transmitted to a time-of-flight mass spectrometer (i.e., mass spectrometry component 5) composed of a Wiley-Mclaren lens group 51, an ion acceleration / deceleration lens group 52, a reflection lens group 54 and a microchannel plate detector 53 for mass spectrometry measurement. The first nanocluster beam b is transmitted by a high-voltage pulse from the Wiley-Mclaren lens group 51 to the reflection lens group 54, and then reflected to the microchannel plate detector 53.

[0119] Figure 4 A working principle diagram of a nanomaterial preparation and characterization system in a deposition mode according to an embodiment of the present invention is shown.

[0120] According to some embodiments of the present invention, Figure 4 As shown, the deposition assembly 6 includes a temperature-controlled sample stage 61 and a displacement assembly. The temperature-controlled sample stage 61 is suitable for adjusting the deposition temperature and deposition rate of the target nanomaterial; the displacement assembly is suitable for adjusting the position of the temperature-controlled sample stage.

[0121] According to some embodiments of the present invention, the deposition temperature of the target nanomaterial can be adjusted in real time by setting a temperature-controlled sample stage 61, which has heating and cooling functions. The deposition environment inside the deposition assembly 6 is regulated by various external fields.

[0122] According to some embodiments of the present invention, the nanomaterial preparation characterization system operates in a mass spectrometry measurement mode, and a nanocluster beam of a specific mass-to-charge ratio (i.e., the first nanocluster beam b) is transmitted to the low-temperature ion flight tube 4 via the ion guide 1213 for temperature control. The first nanocluster beam b after temperature control by the low-temperature ion flight tube 4 is transmitted to the ion focusing and deflection lens group for focusing and deflection. The first nanocluster beam b after focusing and deflecting by the ion focusing and deflection lens group is transmitted to the ion acceleration / deceleration lens group for speed regulation. The first nanocluster beam b after being adjusted to the required kinetic energy by the ion acceleration / deceleration lens group is transmitted to the deposition assembly 6, and the first nanocluster beam b is deposited on the temperature-controlled sample stage 61 to form the target nanomaterial.

[0123] According to some optional embodiments of the present invention, the temperature control range of the temperature-controlled sample stage 61 is -198°C to 1000°C. For example, the temperature that can be controlled by the temperature-controlled sample stage 61 includes -198°C, -192°C, -190°C, -180°C, -170°C, -150°C, -140°C, -120°C, -100°C, -70°C, -50°C, 0°C, 100°C, 300°C, 500°C, 700°C, 900°C, 1000°C, etc.

[0124] According to some embodiments of the present invention, the temperature-controlled sample stage 61 is mounted on a connecting rod inside the sample transfer assembly 9, and can adjust the position of the sample through a displacement assembly under a vacuum environment, and transport the sample to the characterization assembly 7. A sample replacement table is also provided inside the sample transfer assembly 9, which is suitable for placing or replacing different types of temperature-controlled sample stages 61.

[0125] According to some embodiments of the present invention, a sample holder and a substrate are arranged above the temperature-controlled sample stage 61, and the target nanomaterial is deposited on the substrate. The temperature-controlled sample stage 61 has a sample holder clamping and fixing mechanism, which can fix the sample holder grasped by the magnetic rod, and the sample holder includes any one of a fixed standard flag-type sample holder and a disc-type sample holder. The temperature-controlled sample stage 61 can be positionally offset by a manual vacuum hollow introduction device.

[0126] According to some optional embodiments of the present invention, the substrate includes any one of a silicon wafer, a rutile wafer, silicon carbide, titanium dioxide, copper, nickel, aluminum, and other metal materials.

[0127] According to some embodiments of the present invention, Figure 1 It can be seen that the above-mentioned nanomaterial preparation and characterization system also includes a sample transmission component 8, the two ends of which are respectively connected to the deposition component 6 and the mass spectrometry component 5, and the sample transmission component 8 includes a magnetic rod and a manipulator. The magnetic rod is suitable for transporting the target nanomaterial obtained by the deposition component 6 to the characterization component 7.

[0128] According to some embodiments of the present invention, a sample transport component 8 including a magnetic rod is provided to transport the target nanomaterial obtained by the deposition component 6 to the characterization component 7, thereby achieving subsequent characterization of the physical and chemical properties of the target nanomaterial.

[0129] According to some embodiments of the present disclosure, the manipulator is able to perform high-precision sample handling operations in a high-vacuum environment, which is particularly important for precision industries such as semiconductor manufacturing; the design of the manipulator takes into account external interference and load disturbances, and has strong anti-interference capabilities; by setting up the manipulator control system in the sample transfer assembly 8, rapid response can be achieved, shortening the production cycle and improving sample production efficiency.

[0130] According to some embodiments of the present invention, the sample transmission assembly 8 further comprises a sample disc gripping chuck, and the chuck is replaced according to different types of sample discs.

[0131] According to some embodiments of the present invention, after the deposition assembly 6 deposits the target nanomaterial for a period of time, the sample holder is clamped by the magnetic rod of the sample transfer assembly 9 and transferred to the characterization assembly 7 to characterize various properties of the target nanomaterial.

[0132] Figure 5 A cross-sectional view of a sample transmission component in a nanomaterial preparation and characterization system according to an embodiment of the present invention is shown.

[0133] According to some embodiments of the present invention, Figure 5 As shown, the sample transmission component 8 includes: a magnetic rod 81, a vacuum plug valve 82, a quick-opening door with a window 83, a bellows 84 and a vacuum load lock 85. A vacuum plug valve 82 is provided between the cavity of the sample pretreatment component 10 and the cavity of the sample transfer component 9, a vacuum plug valve 82 is provided between the cavity of the sample transfer component 9 and the characterization component 7, a bellows 84 is welded between the sample transfer component 9 and the vacuum plug valve 82, and the characterization component 7 is connected to the vacuum plug valve 82 by the bellows 84. The bellows 84 effectively isolates the vibration of the sample transmission component 8 or the deposition component 6 or other components from being transmitted to the inside of the characterization component 7, thereby reducing vibration noise.

[0134] According to some embodiments of the present invention, when the nanomaterial preparation and characterization system is in an online deposition and characterization mode, the first nanocluster beam is deposited on a sample holder fixed above a temperature-controlled sample stage 61 after being regulated by multiple external fields. When characterization is performed using the characterization component 7, the sample holder is grasped by the magnetic rod 81 and transferred to the interior of the sample pretreatment component 10. The sample processed by the sample pretreatment component 10 is then transferred to the sample transfer component 9 via the magnetic rod, and finally transferred to the sample placement position inside the characterization component 7 via the magnetic rod 81.

[0135] According to some embodiments of the present invention, in a characterization mode in which a nanomaterial preparation and characterization system is in an offline state, samples prepared by conventional physical or chemical methods are captured by a magnetic rod 81 through a windowed quick-opening door 83 on a vacuum load lock 85 and transferred to a sample pretreatment component 10, and then transferred to a sample transfer component 9 through a magnetic rod, and then transferred to a sample holder inside a characterization component 7 through a magnetic rod.

[0136] According to some embodiments of the present invention, the above-mentioned nanomaterial preparation and characterization system also includes a sample pretreatment component 10, which is configured to change the catalytic properties of the target nanomaterial by reacting the external reaction gas input into the sample pretreatment component 10 with the target nanomaterial from the deposition component 6, and transport the target nanomaterial with changed catalytic properties to the characterization component 7.

[0137] According to some embodiments of the present invention, the beam generating component 1 includes a magnetron sputtering ion source and an electrospray ion source, which are coupled to the above-mentioned nanomaterial preparation and characterization system through an electrostatic quadrupole deflection lens 21 and an ion guide 1213, a quadrupole mass selector is used as a mass selection component 3 for mass selection, a low-temperature ion flight tube 4 is used to temperature-control the nanoparticle ion beam, and online deposition is performed in a deposition component 6 through a series of ion optical devices to achieve decentralized control, or a mass spectrometry component 5 is used for mass spectrometry analysis, and a sample transfer component 8 transfers the target nanomaterial from the mass spectrometry component 5 to the characterization component 7. Samples prepared by conventional physical or chemical methods outside the above-mentioned nanomaterial preparation and characterization system can also be transferred from a vacuum load lock 85 to the characterization component 7 via a sample transfer component 9. According to actual experimental needs, the target nanomaterial will be subjected to certain processing by a sample pretreatment component 10, and the sample transfer component 9 connects the sample pretreatment component 10 with the characterization component 7 to achieve the function of vacuum transition. Some characterization components 7, such as the confocal Raman microscope 71, the UV-visible spectrometer 73, and the Fourier transform infrared spectrometer 72, have two usage modes. They can be coupled to the above-mentioned nanomaterial preparation characterization system through optical fiber, or they can be used to characterize special samples such as some liquids under external non-vacuum conditions.

[0138] According to some embodiments of the present invention, the beam shaping component 2, the mass selection component 3, the low-temperature ion flight tube 4, the mass spectrometry component 5 and the sample transmission component 8 are all placed in an ultra-high vacuum chamber, that is, the entire nanomaterial preparation and characterization system is placed in an ultra-high vacuum chamber, and each component is connected by a partition with a through hole, and the edge of the partition is sealed with the ultra-high vacuum chamber.

[0139] Figure 6 A schematic diagram of the vacuum layout of a nanomaterial preparation and characterization system according to an embodiment of the present invention is shown.

[0140] According to some embodiments of the present invention, the nanomaterial preparation and characterization system operates in a vacuum environment, and the vacuum layout is as follows: Figure 6 As shown, the cavity of the magnetron sputtering ion source 121 is pumped by a first worm gear molecular pump 104 with a pumping speed of not less than 1000 L / s, and its background vacuum environment is less than 5×10 -7mbar, the cavity of the electrospray ion source 122 is pumped by a second worm gear molecular pump 105 with a pumping speed of not less than 600 L / s, and the background vacuum environment is less than 5×10 -7 mbar, pumping speed not less than 50m 3 / h multi-stage rotary vane pump 101 is used as the front stage of the first worm gear molecular pump 104 and the second worm gear molecular pump 105; the electrostatic quadrupole deflection lens 21 and the ion guide cavity are pumped by the third worm gear molecular pump 106 with a pumping speed of not less than 600L / s, and the background vacuum environment is less than 5×10 -7 mbar, the cavity of the mass selection component 3 is pumped by a fourth worm gear molecular pump 107 with a pumping speed of not less than 600 L / s, and the vacuum environment is less than 5×10 -7 mbar, the cavity of the low-temperature ion flight tube 4 is pumped by the fifth worm gear molecular pump 108 with a pumping speed of not less than 600L / s, and its background vacuum environment is less than 5×10 -7 mbar, the mass spectrometer component 5 is pumped by the sixth worm gear molecular pump 109 with a pumping speed of not less than 600 L / s, and its background vacuum environment is less than 5×10 -7 mbar; the deposition assembly 6 is pumped by the seventh worm gear molecular pump 110 with a pumping speed of not less than 300 L / s, and the background vacuum environment is less than 5×10 -8 mbar, the chamber of the vacuum load lock 85 is pumped by the eighth worm gear molecular pump 111 with a pumping speed of not less than 60L / s, and the background vacuum environment is less than 5×10 -6 mbar, the sample transfer assembly 9 is pumped by the ninth worm gear molecular pump 112 with a pumping speed of not less than 60 L / s, and the background vacuum environment is less than 5×10 -8 mbar, pumping speed not less than 90m 3 / h multi-stage Roots pump group 103 is used as the front stage of the third worm gear molecular pump 106, the fourth worm gear molecular pump 107, the fifth worm gear molecular pump 108, the sixth worm gear molecular pump 109, the seventh worm gear molecular pump 110, the eighth worm gear molecular pump 111 and the ninth worm gear molecular pump 112; the characterization component 7 is pumped by the tenth worm gear molecular pump 113 with a pumping speed of not less than 350L / s, and its background vacuum environment is less than 5×10 -6 mbar, pumping speed not less than 15m 3 The worm gear dry vacuum pump 102 with a capacity of / h serves as the front stage of the tenth worm gear molecular pump 113.

[0141] According to some embodiments of the present invention, the above-mentioned nanomaterial preparation and characterization system is connected through vacuum interconnection technology, which provides a new platform for the research and manufacture of nanomaterials. The free path in the vacuum environment is significantly increased, up to 3 orders of magnitude, which greatly reduces the probability of collision between the generated cluster nanoparticles and other particles in the background atmosphere, thereby effectively avoiding possible contamination and chemical reactions during sample preparation, such as oxidation. With the support of vacuum interconnection technology, samples can be accurately, quickly and smoothly transferred between different devices without being exposed to the atmosphere. This ultra-high vacuum environment (vacuum better than 10 -10 mbar) is critical to maintaining an atomically clean surface that can be maintained for hours, enabling atomic layer growth, surface / interface control, and intrinsic property characterization. In addition, freshly prepared samples can be transported directly from the deposition assembly 6 to the characterization assembly 7, protecting the sample surface from oxidation or other structural or chemical changes associated with atmospheric exposure.

[0142] The nanomaterial preparation and characterization system provided by the present invention has comprehensive research types and can study metals, alloys, metal oxides and non-metallic clusters, as well as macromolecules and protein materials, to achieve the preparation of nanoparticles with atomic-level precision scale control, and the preparation of small molecules and macromolecule samples with determined mass numbers; the nanomaterial preparation and characterization system provided by the present invention can achieve online generation of cluster nanoparticles, and can achieve online deposition and dispersion control through multi-external field regulation; the nanomaterial preparation and characterization system provided by the present invention utilizes a vacuum load lock 85 and a sample transfer component 9, which can not only achieve full-online nanoparticle generation, deposition, and characterization, but also enable the system to have the material and processing and vacuum interlock loading functions required for the conventional physical and chemical offline preparation sample testing functions outside the system, which can not only complete the full-online sample preparation, manipulation, and characterization functions of the system characteristics, but also take into account the comprehensive testing needs of conventional non-online preparation samples, and realize the general platform function.

[0143] It will be appreciated by those skilled in the art that the features described in the various embodiments and / or claims of the present invention may be combined and / or combined in various ways, even if such combinations and / or combinations are not explicitly described in the present invention. In particular, the features described in the various embodiments and / or claims of the present invention may be combined and / or combined in various ways without departing from the spirit and teachings of the present invention. All of these combinations and / or combinations fall within the scope of the present invention.

[0144] The embodiments of the present invention are described above. However, these embodiments are only for the purpose of illustration, and are not intended to limit the scope of the present invention. Although each embodiment is described above, it does not mean that the measures in each embodiment cannot be used in combination. The scope of the present invention is defined by the attached claims and their equivalents. Without departing from the scope of the present invention, those skilled in the art may make various substitutions and modifications, which should all fall within the scope of the present invention.

Claims

1. A nanomaterial preparation and characterization system, characterized in that: include: A beam generation assembly, adapted to generate an initial nanocluster beam; A beam shaping component, adapted to adjust the size, shape or transmission speed of the initial nanocluster beam; A mass selection component, adapted to perform mass selection on the initial nanocluster beam adjusted by the beam shaping component to obtain a first nanocluster beam containing nanoparticles of a target size; A low temperature ion flight tube, adapted to control the temperature of the first nanocluster beam to maintain the stability of the first nanocluster beam; A deposition component, adapted to deposit the first nanocluster beam under the action of an external field to obtain a target nanomaterial; A characterization component, suitable for characterizing the chemical and physical properties of the target nanomaterial; A sample transfer component, adapted to transfer the target nanomaterial to the characterization component under a vacuum environment, so that the physical and chemical properties of the target nanomaterial remain unchanged during the transfer process, thereby completing the characterization of the physical and chemical properties of the target nanomaterial; The beam shaping component includes an electrostatic quadrupole deflection lens, which includes four symmetrical electrodes. By adjusting the voltages applied to the four symmetrical electrodes respectively, a rotationally symmetrical electrostatic field is formed. The electrostatic field is suitable for deflecting and focusing the initial nanocluster beam incident between the four symmetrical electrodes, thereby changing the size, shape or transmission speed of the initial nanocluster beam.

2. The nanomaterial preparation and characterization system according to claim 1, characterized in that: Also includes: The mass spectrometry component is adapted to perform mass spectrometry analysis on the first nanocluster beam to obtain the constituent elements and size distribution of the first nanocluster beam.

3. The nanomaterial preparation and characterization system according to claim 1, characterized in that: The mass selection component is a quadrupole mass selector, and a radio frequency bias electric field is applied to the mass selection component, so that ions with a target atomic number can pass through the mass selection component, thereby obtaining the first nanocluster beam containing ions with the target atomic number.

4. The nanomaterial preparation and characterization system according to claim 2, characterized in that: It also includes a sample transmission component, the two ends of which are respectively connected to the deposition component and the mass spectrometry component. The sample transmission component includes a magnetic rod and a manipulator. The magnetic rod is suitable for transporting the target nanomaterial obtained by the deposition component to the characterization component.

5. The nanomaterial preparation and characterization system according to claim 1, characterized in that: The beam generating assembly includes any one or a combination of the following: Magnetron sputtering ion source, thermal evaporation ion source, laser ablation ion source, arc discharge ion source, electrospray ion source, matrix-assisted laser desorption ionization source, atmospheric pressure chemical ionization source and atmospheric pressure photoionization source.

6. The nanomaterial preparation and characterization system according to claim 1, characterized in that: It also includes a sample pretreatment component, which is configured to change the catalytic properties of the target nanomaterial by reacting an external reaction gas input into the sample pretreatment component with the target nanomaterial from the deposition component, and transport the target nanomaterial with changed catalytic properties to the characterization component.

7. The nanomaterial preparation and characterization system according to claim 1, characterized in that: The deposition assembly comprises: A temperature-controlled sample stage, adapted to adjust the deposition temperature of the target nanomaterial and the deposition rate of the target nanomaterial; and The displacement component is suitable for adjusting the position of the temperature-controlled sample stage.

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