A rapid analysis system and method for secondary ion mass spectrometry

Abstract

The present invention relates to a rapid analysis system and method for secondary ion mass spectrometry, characterized in that the system comprises: a fast pulse mass spectrometry magnet power supply for modulating input power grid energy to obtain a 6-pulse current; and a fast pulse mass spectrometry magnet for providing a magnetic field for deflecting a secondary ion beam based on the obtained 6-pulse current and separating different ion beams. The present invention can ensure that the magnetic field reaches a steady state within a very short time after a rapid change, thereby greatly improving the secondary ion detection rate, improving the sample analysis accuracy, and reducing damage and information destruction caused by long-term bombardment of the sample. The system can be widely used in the field of ion mass spectrometry.

Description

Technical Field

[0001] The present invention relates to the field of ion mass spectrometry, and in particular to a rapid analysis system and method for secondary ion mass spectrometry. Background Art

[0002] Secondary Ion Mass Spectrometry (SIMS) is one of the most frequently used ion spectrometers. It can be used to examine the elemental composition within the submicron region on the surface or inside most solid materials. SIMS uses a low-energy ion beam to bombard the surface of the target sample - these ions are called primary ions. They induce the production of secondary ions on the solid surface, i.e., secondary ions. The composition of the sample surface is obtained by mass spectrometry analysis of the secondary ions. The advantages of SIMS are: 1) it can measure any element (HU) in any solid, including some isotopes with extremely low content; 2) data acquisition is relatively simple; 3) in most cases, only a small amount of test sample is required. However, in actual detection and analysis, the current SIMS generally has problems such as significant sample damage, slow analysis speed, and high sample consumption.

[0003] Traditional secondary ion mass spectrometry (SIMS) uses a mass spectrometer magnet to provide a steady field. This magnetic field changes slowly (on the order of ~2 seconds). This field deflects the secondary ion beam and separates the different ion beams. Prolonged bombardment of the sample by primary ions leads to increased sample damage and rapid sample consumption. Because the fine elemental composition of the sample carries corresponding physical information, the speed of sample analysis switching directly affects the accuracy of the analysis. Current analytical methods significantly restrict the application and analytical capabilities of SIMS for the analysis of rare samples in geology and astronomy.

[0004] To address this limitation, existing technologies typically use solutions such as adding collectors or improving sample preparation standards to reduce analysis time and improve analysis accuracy. However, in practice, these methods have very limited effect in reducing the rapid damage caused by the persistent bombardment of samples by primary ions. Summary of the Invention

[0005] In view of the above problems, the object of the present invention is to provide a rapid analysis system and method for secondary ion mass spectrometry, which can reduce the rapid damage caused by the persistent bombardment of the sample by primary ions.

[0006] To achieve the above objectives, the present invention adopts the following technical solutions: On the one hand, a rapid analysis system for secondary ion mass spectrometry is provided, comprising:

[0007] Fast pulse mass spectrometry magnet power supply, used to modulate the input grid energy to obtain 6-pulse current;

[0008] The fast pulse mass spectrometry magnet is used to provide a magnetic field to deflect the secondary ion beam based on the obtained 6-pulse current and to separate different ion beams.

[0009] Furthermore, the fast pulse mass spectrometry magnet power supply includes:

[0010] The front-end module is used to rectify and store the input grid energy;

[0011] The primary side modulation module is used to perform high-frequency modulation on the grid energy after rectification and energy storage to obtain the three-phase primary side input high voltage;

[0012] Transformer, used to convert three-phase primary input high voltage into three-phase secondary output low voltage;

[0013] The secondary side modulation module is used to modulate the current of the three-phase secondary side output low voltage to achieve 6-pulse frequency multiplication modulation function;

[0014] The filtering module is used to filter the obtained 6-pulse current so that the filtered 6-pulse current obtains the waveform required by the fast pulse mass spectrometry magnet at the load.

[0015] Furthermore, the primary side modulation module adopts IGBT and is composed of a three-phase H bridge.

[0016] Furthermore, the secondary side modulation module is based on a three-phase controlled rectifier modulation method and is composed of reverse resistance type IGBT elements.

[0017] Furthermore, the secondary side modulation module includes three groups of rectifier modulation modules, wherein each of the rectifier modulation modules includes a first reverse resistance type IGBT element and a second reverse resistance type IGBT element connected in series;

[0018] The midpoint of each of the rectifier modulation modules is connected to a phase corresponding to the three-phase secondary output low voltage of the transformer output; all of the first reverse resistance IGBT elements and the second reverse resistance IGBT elements are connected in parallel to the filter module.

[0019] Furthermore, the filtering module adopts an output filtering capacitor plus inductor method.

[0020] Furthermore, the iron core of the fast pulse mass spectrometry magnet is formed by laminating silicon steel sheets with a thickness of 0.35 mm.

[0021] Furthermore, the core coil of the fast pulse mass spectrometry magnet adopts a copper wire with an inner circle and an outer square with a cross-sectional size of 8mm*8mm and an inner diameter of 4mm, and the number of turns of the single pole is 16 turns.

[0022] In another aspect, a rapid analysis method for secondary ion mass spectrometry is provided, comprising:

[0023] The fast pulse mass spectrometer magnet power supply modulates the input grid energy to obtain a 6-pulse current;

[0024] The fast pulse mass spectrometry magnet provides a magnetic field to deflect the secondary ion beam based on the obtained 6-pulse current and separate different ion beams.

[0025] Furthermore, the fast pulse mass spectrometry magnet power supply modulates the input grid energy to obtain a 6-pulse current, including:

[0026] The front-end module rectifies and stores the input grid energy and then sends it to the primary-side modulation module;

[0027] The primary side modulation module performs high-frequency modulation on the grid energy after rectification and energy storage to obtain the three-phase primary side input high voltage and send it to the transformer;

[0028] The transformer converts the three-phase primary input high voltage into three-phase secondary output low voltage and sends it to the secondary modulation module;

[0029] The secondary side modulation module performs current modulation on the three-phase secondary side output low voltage of the transformer output to obtain a 6-pulse current and sends it to the filtering module;

[0030] The filtering module filters the obtained 6-pulse current so that the filtered 6-pulse current obtains the waveform required by the fast pulse mass spectrometry magnet at the load and sends it to the fast pulse mass spectrometry magnet.

[0031] The present invention has the following advantages due to the adoption of the above technical solution:

[0032] 1. The present invention is provided with a fast pulse mass spectrometry magnet power supply and a fast pulse mass spectrometry magnet, which realizes accurate scanning analysis within the entire element range through precise switching of fast magnetic fields with a large dynamic range, thereby improving the analysis accuracy and speed of SIMS samples.

[0033] 2. The special design of the primary modulation module and transformer of the fast pulse mass spectrometry magnet power supply in the present invention can provide a negative voltage for the load, and can achieve rapid switching of current in the order of hundreds of milliseconds, so that the current can rise and fall quickly.

[0034] 3. The fast pulse mass spectrometry magnet power supply of the present invention adopts high-frequency modulation 6-pulse frequency doubling, which can improve the dynamic response speed of the power supply and enable the current to run quickly in a stable state after dynamic switching.

[0035] 4. The present invention achieves comprehensive, high-resolution reading of sample information through rapid and accurate scanning of the fast-pulse mass spectrometry magnet, reduces the magnet's inductance and core loss under pulsed operation, and, combined with a 6-pulse frequency-doubled fast-pulse mass spectrometry magnet power supply, enables rapid current rise and fall, as well as rapid operation to a stable state after dynamic current switching. The magnetic field switching time is shortened by 10 times compared to traditional SIMS, enabling rapid switching analysis from H to U isotopes, greatly improving sample analysis speed, analytical capabilities, and in-situ resolution accuracy.

[0036] 5. The present invention can shorten the magnetic field conversion time as much as possible, greatly improve the secondary ion detection rate, improve the sample analysis accuracy, reduce the damage and information destruction caused by long-term bombardment of the sample, and realize rapid and accurate scanning of all elements of the sample.

[0037] 6. The fast pulse mass spectrometry magnet of the present invention can directly realize the secondary ion analysis function of the sample, which can improve the analysis accuracy while quickly analyzing the sample and avoiding damage.

[0038] In summary, the present invention can be widely applied in the field of ion mass spectrometry. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] Various other advantages and benefits will become apparent to those skilled in the art upon reading the detailed description of the preferred embodiment below. The accompanying drawings are for illustration purposes only and are not to be considered as limiting the present invention. Throughout the drawings, the same reference numerals are used to denote the same components. In the drawings:

[0040] Figure 1 This is a schematic diagram of the structure of a fast pulse mass spectrometry magnet power supply provided by one embodiment of the present invention;

[0041] Figure 2 1 is a schematic structural diagram of a secondary side modulation module provided by an embodiment of the present invention;

[0042] Figure 3 3 is a schematic diagram of the working mode of a fast pulse mass spectrometry magnet provided by an embodiment of the present invention, wherein the horizontal axis is the magnetic field change time and the vertical axis is the current. DETAILED DESCRIPTION

[0043] Exemplary embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. Although exemplary embodiments of the present invention are shown in the accompanying drawings, it should be understood that the present invention can be implemented in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided to enable a more thorough understanding of the present invention and to fully convey the scope of the present invention to those skilled in the art.

[0044] It should be understood that the terms used herein are for the purpose of describing specific example embodiments only and are not intended to be limiting. Unless the context clearly indicates otherwise, the singular forms "one", "an" and "said" as used herein may also be meant to include plural forms. The terms "comprise", "include", "contain" and "have" are inclusive and therefore specify the presence of stated features, steps, operations, elements and / or parts, but do not exclude the presence or addition of one or more other features, steps, operations, elements, parts, and / or combinations thereof. The method steps, processes, and operations described herein are not to be construed as necessarily requiring them to be performed in the specific order described or illustrated, unless the order of execution is clearly indicated. It should also be understood that additional or alternative steps may be used.

[0045] Although the terms first, second, third, etc. can be used in the text to describe multiple elements, components, regions, layers and / or sections, these elements, components, regions, layers and / or sections should not be limited by these terms. These terms can only be used to distinguish an element, component, region, layer or section from another region, layer or section. Unless the context clearly indicates otherwise, terms such as "first", "second" and other numerical terms do not imply order or sequence when used in the text. Therefore, the first element, component, region, layer or section discussed below can be referred to as the second element, component, region, layer or section without departing from the teaching of the example embodiments.

[0046] To address the technical problem of rapid sample damage caused by persistent primary ion bombardment, embodiments of the present invention provide a rapid analysis system and method for secondary ion mass spectrometry. This solution improves sample analysis accuracy by minimizing magnetic field switching time while simultaneously reducing analysis time. Specifically, a fast-pulsed mass spectrometry magnet rapidly and accurately switches between different magnetic field levels, rapidly rising or falling from one operating point to another. This allows for precise scanning of the H-U full element range, thereby enabling comprehensive and accurate elemental analysis within a very small sample, improving analytical capabilities and avoiding loss of important information. This also reduces sample consumption from primary ion bombardment. The present invention relates to a fast-pulsed mass spectrometry magnet for related applications. By combining it with a pulsed, high-frequency, six-pulse power supply, the magnet can achieve a very short time to reach steady state after a rapid magnetic field change, significantly increasing the secondary ion detection rate and sample analysis accuracy while reducing sample loss and information damage.

[0047] Example 1

[0048] like Figure 1As shown, this embodiment provides a rapid analysis system for secondary ion mass spectrometry, including a fast pulse mass spectrometry magnet power supply 1 and a fast pulse mass spectrometry magnet, wherein the fast pulse mass spectrometry magnet power supply 1 includes a front-stage module 11, a primary modulation module 12, a transformer 13, a secondary modulation module 14 and a filter module 15.

[0049] The front-end module 11 is used to rectify and store the input grid energy.

[0050] The primary side modulation module 12 is used to perform high frequency modulation on the grid energy after rectification and energy storage to obtain a three-phase primary side input high voltage.

[0051] The transformer 13 is used to convert the three-phase primary side input high voltage into the three-phase secondary side output low voltage to provide energy to the secondary side modulation module 14 .

[0052] The secondary side modulation module 14 is used to perform current modulation on the three-phase secondary side output low voltage output by the transformer 13 to achieve a 6-pulse frequency multiplication modulation function.

[0053] The filtering module 15 is used to filter the obtained 6-pulse current so that the filtered 6-pulse current obtains the waveform required by the fast pulse mass spectrometry magnet at the load.

[0054] The fast pulse mass spectrometry magnet is used to provide a magnetic field to deflect the secondary ion beam based on the filtered 6-pulse current and to separate different ion beams.

[0055] The present invention provides a fast-switching current to the fast-pulse mass spectrometry magnet through a fast-pulse mass spectrometry magnet power supply 1, and the fast-pulse mass spectrometry magnet generates a fast-switching magnetic field. Through the fast magnetic field with a large dynamic range and precise switching, accurate scanning analysis within the entire element range can be achieved, thereby improving the analysis accuracy and speed of SIMS samples.

[0056] In a preferred embodiment, the primary modulation module 12 is composed of a three-phase H-bridge and uses an IGBT component (insulated gate bipolar transistor) of model FF100R12RT4, which can perform a higher frequency modulation function at a higher front-stage voltage, ensuring that the primary modulation module 12 works reliably.

[0057] In a preferred embodiment, the transformer 13 operates in a three-phase high-frequency AC conversion state, has a small size, and uses a fixed transformation ratio to step down the input high voltage, thereby ensuring reliable operation of the secondary modulation module 14 .

[0058] In a preferred embodiment, the secondary side modulation module 14 is based on a three-phase controlled rectifier modulation mode, and is composed of a reverse resistance IGBT element of model SKM300GBD12T4, to achieve 6-pulse frequency multiplication modulation, thereby ensuring a fast response of the output current.

[0059] Specifically, if Figure 2 As shown, the secondary modulation module 14 includes three groups of rectifier modulation modules 2, wherein each rectifier modulation module 2 includes a first reverse-resistance IGBT element 21 and a second reverse-resistance IGBT element 22 connected in series. The midpoint of each rectifier modulation module 2 is connected to a phase corresponding to the three-phase secondary output low voltage output by the transformer 13. The first reverse-resistance IGBT elements 21 of all rectifier modulation modules 2 are connected in parallel to the filter module 15, and the second reverse-resistance IGBT elements 22 of all rectifier modulation modules 2 are connected in parallel to the filter module 15. The first reverse-resistance IGBT elements 21 and the second reverse-resistance IGBT elements 22 are used to current modulate the three-phase secondary output low voltage output by the transformer 13.

[0060] Specifically, the first reverse-blocking IGBT element 21 and the second reverse-blocking IGBT element 22 each include a diode 3 and an IGBT element 4 . The diode 3 is used to block reverse current flow, and the IGBT element 4 is used for forward current flow and current modulation.

[0061] In a preferred embodiment, the filter module 15 adopts an output filter capacitor plus an inductor, wherein the capacitance is 100 μF and the inductance is 46 μH.

[0062] In a preferred embodiment, the fast pulse mass spectrometry magnet is a SIMS mass spectrometry magnet.

[0063] In a preferred embodiment, the core of the fast pulse mass spectrometry magnet is made of laminated silicon steel sheets with a thickness of 0.35 mm, and the end of the fast pulse mass spectrometry magnet is made of 316L stainless steel with relatively low resistivity. The structure of this fast pulse mass spectrometry magnet can effectively block the eddy current circuit on the core of the fast pulse mass spectrometry magnet and reduce the core loss under pulse operation.

[0064] In a preferred embodiment, in order to respond to the rapidly rising magnetic field changes and reduce the difficulty of setting up the fast pulse mass spectrometry magnet power supply 1, the inductance of the fast pulse mass spectrometry magnet needs to be reduced to below a certain value, and the load inductance of the fast pulse mass spectrometry magnet needs to be controlled at about 20mH. Therefore, the iron core coil of the fast pulse mass spectrometry magnet adopts an inner circle and outer square copper wire with a cross-sectional size of 8mm*8mm and an inner diameter of 4mm, and the number of monopole turns is 16 turns.

[0065] Example 2

[0066] This embodiment provides a rapid analysis method for secondary ion mass spectrometry, comprising the following steps:

[0067] 1) The front-end module 11 rectifies and stores the input grid energy and then sends it to the primary-side modulation module 12.

[0068] 2) The primary modulation module 12 performs high-frequency modulation on the grid energy after rectification and energy storage to obtain a three-phase primary input high voltage, and sends it to the transformer 13.

[0069] 3) The transformer 13 converts the three-phase primary side input high voltage into the three-phase secondary side output low voltage and sends it to the secondary side modulation module 14.

[0070] 4) The secondary modulation module 14 performs current modulation on the three-phase secondary output low voltage output by the transformer 13 to obtain a 6-pulse current and sends it to the filtering module 15 .

[0071] 5) The filtering module 15 filters the obtained 6-pulse current so that the filtered 6-pulse current obtains the waveform required by the fast pulse mass spectrometry magnet at the load and is sent to the fast pulse mass spectrometry magnet.

[0072] 6) The fast pulse mass spectrometry magnet provides a magnetic field to deflect the secondary ion beam based on the filtered 6-pulse current and separate different ion beams.

[0073] like Figure 3 Figure 1 shows the operating mode of the fast-pulse mass spectrometry magnet using the present invention. This invention improves ion switching from the order of 1s to the order of 100ms, a reduction of approximately 10 times. The magnetic field change time τ (i.e., the current rapid rise time + the time to reach a stable state) is less than 250ms. The current rise time from 0 to 350A is less than 250ms, and the same applies to the fall time. Secondary ions P1, P2, and P3 are separated at the flat-top magnetic field operating points B, C, and D, respectively (the flat-top magnetic field stable operation time t is typically greater than 2s). The six-pulse current generated by the present invention enables the power supply to provide the fast-pulse mass spectrometry magnet with a current that meets the specified specifications, thereby generating a magnetic field that meets the specified specifications, significantly improving sample analysis speed, analytical capabilities, and in-situ resolution accuracy.

[0074] The above embodiments are only used to illustrate the present invention, wherein the structure, connection mode and manufacturing process of each component can be changed. Any equivalent transformations and improvements based on the technical solution of the present invention should not be excluded from the scope of protection of the present invention.

Claims

1. A rapid analysis system for secondary ion mass spectrometry, characterized in that: include: Fast pulse mass spectrometry magnet power supply, used to modulate the input grid energy to obtain 6-pulse current; A fast pulse mass spectrometry magnet is used to provide a magnetic field for deflecting the secondary ion beam based on the obtained 6-pulse current and to separate different ion beams; The fast pulse mass spectrometry magnet power supply comprises: The front-end module is used to rectify and store the input grid energy; The primary side modulation module is used to perform high-frequency modulation on the grid energy after rectification and energy storage to obtain a three-phase primary side input high voltage. The primary side modulation module uses IGBT components and is composed of a three-phase H-bridge. Transformer, used to convert three-phase primary input high voltage into three-phase secondary output low voltage; The secondary side modulation module is used to modulate the current of the three-phase secondary side output low voltage to achieve a 6-pulse frequency multiplication modulation function. The secondary side modulation module is based on a three-phase controlled rectifier modulation method and is composed of reverse resistance IGBT components; A filtering module, configured to filter the obtained 6-pulse current so that the filtered 6-pulse current obtains the waveform required by the fast pulse mass spectrometry magnet at the load; The secondary side modulation module includes three groups of rectifier modulation modules, wherein each of the rectifier modulation modules includes a first reverse-resistance IGBT element and a second reverse-resistance IGBT element connected in series, and the first reverse-resistance IGBT element and the second reverse-resistance IGBT element each include a diode and an IGBT element; The midpoint of each of the rectifier modulation modules is connected to a phase corresponding to the three-phase secondary output low voltage of the transformer output; all of the first reverse resistance IGBT elements and the second reverse resistance IGBT elements are connected in parallel to the filter module.

2. A rapid analysis system for secondary ion mass spectrometry according to claim 1, characterized in that: The filtering module adopts the method of output filtering capacitor plus inductor.

3. A rapid analysis system for secondary ion mass spectrometry according to claim 1, characterized in that: The iron core of the fast pulse mass spectrometry magnet is formed by laminating silicon steel sheets with a thickness of 0.35 mm.

4. A rapid analysis system for secondary ion mass spectrometry according to claim 1, characterized in that: The iron core coil of the fast pulse mass spectrometry magnet is made of copper wire with a cross-sectional size of 8mm*8mm and an inner diameter of 4mm, and the number of turns of a single pole is 16.

5. A rapid analysis method for secondary ion mass spectrometry, characterized in that: include: The fast pulse mass spectrometer magnet power supply modulates the input grid energy to obtain a 6-pulse current; The fast pulse mass spectrometry magnet provides a magnetic field to deflect the secondary ion beam based on the obtained 6-pulse current and separate different ion beams; The fast pulse mass spectrometry magnet power supply modulates the input grid energy to obtain a 6-pulse current, including: The front-end module rectifies and stores the input grid energy and then sends it to the primary-side modulation module; The primary side modulation module performs high-frequency modulation on the grid energy after rectification and energy storage to obtain three-phase primary side input high voltage and sends it to the transformer. The primary side modulation module uses IGBT components and consists of a three-phase H-bridge. The transformer converts the three-phase primary input high voltage into three-phase secondary output low voltage and sends it to the secondary modulation module; The secondary side modulation module performs current modulation on the three-phase secondary side output low voltage of the transformer to obtain a 6-pulse current and sends it to the filtering module. The secondary side modulation module is based on a three-phase controlled rectifier modulation method and is composed of reverse resistance IGBT components. The filtering module filters the obtained 6-pulse current so that the filtered 6-pulse current obtains the waveform required by the fast pulse mass spectrometry magnet at the load and sends it to the fast pulse mass spectrometry magnet; The secondary side modulation module includes three groups of rectifier modulation modules, wherein each of the rectifier modulation modules includes a first reverse-resistance IGBT element and a second reverse-resistance IGBT element connected in series, and the first reverse-resistance IGBT element and the second reverse-resistance IGBT element each include a diode and an IGBT element; The midpoint of each of the rectifier modulation modules is connected to a phase corresponding to the three-phase secondary output low voltage of the transformer output; all of the first reverse resistance IGBT elements and the second reverse resistance IGBT elements are connected in parallel to the filter module.

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