WO2015085577A1 - System and method for analyzing gas sample using secondary ion mass spectrometer - Google Patents

System and method for analyzing gas sample using secondary ion mass spectrometer Download PDF

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Publication number
WO2015085577A1
WO2015085577A1 PCT/CN2013/089380 CN2013089380W WO2015085577A1 WO 2015085577 A1 WO2015085577 A1 WO 2015085577A1 CN 2013089380 W CN2013089380 W CN 2013089380W WO 2015085577 A1 WO2015085577 A1 WO 2015085577A1
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WIPO (PCT)
Prior art keywords
metal plate
hole
gas
mass spectrometer
sample
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PCT/CN2013/089380
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French (fr)
Chinese (zh)
Inventor
唐国强
赵洪
李献华
李秋立
刘宇
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中国科学院地质与地球物理研究所
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Application filed by 中国科学院地质与地球物理研究所 filed Critical 中国科学院地质与地球物理研究所
Priority to CN201380021677.7A priority Critical patent/CN105103265B/en
Priority to PCT/CN2013/089380 priority patent/WO2015085577A1/en
Publication of WO2015085577A1 publication Critical patent/WO2015085577A1/en

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/10Ion sources; Ion guns
    • H01J49/14Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
    • H01J49/142Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers using a solid target which is not previously vapourised

Definitions

  • This invention relates to the field of analytical instrumentation, and more particularly to a system and method for analyzing a gas sample using a secondary ion mass spectrometer. Background technique
  • Secondary ion mass spectrometers are commonly used for in-situ analysis, surface analysis and in-depth analysis of solid samples, which are widely used in materials science, life sciences, geological sciences and other fields.
  • the analysis process of the secondary ion mass spectrometer is to place the solid sample in a vacuum, bombard the solid sample with a specific kind of primary ion, and the sample is sputtered with secondary ions under the bombardment of a certain energy of one ion, and the secondary ion represents Information on the composition of the sample.
  • the secondary ions are separated temporally or spatially using an electric or magnetic field to determine the type and amount of secondary ions in order to enable qualitative and quantitative analysis of solid samples. .
  • the principle of a secondary ion mass spectrometer which generally uses a magnetic field as a mass analyzer, is shown in Figure 1.
  • the primary ion source 1 produces a primary ion 2 .
  • the primary ion 2 is focused by the electric field generated by the ion optical lenses 3, 5, 6 onto the surface of sample 7 (sample 7 is located in the sample chamber), and sample 7 is bombarded.
  • the primary ion 2 and ion optical lenses 3, 5, 6 are located within the vacuum chamber 4.
  • the primary ion 2 bombards the sample 7, and a part of the sample 7 is ionized to generate secondary ions 9.
  • the secondary ions 9 pass through the ion optical lens 10, 11, 12 , an electrostatic field analyzer 13, an ion optical lens 15, a magnetic field analyzer 16, an ion optical lens 18, and reach the receiver 19.
  • Sample 7 and ion optical lenses 10, 11, 12 are located within vacuum chamber 8.
  • the ion optical lens 15 is located within the vacuum chamber 14.
  • the ion optical lens 18 is located within the vacuum chamber 17.
  • the electrostatic field analyzer 13 and the magnetic field analyzer 16 constitute a double focusing structure for achieving angular focusing and energy focusing while achieving mass separation of the secondary ions 9.
  • the intensity of the magnetic field analyzer 16 determines the type of ions received by the receiver 19. Depending on the signal strength received by the receiver 19, the sample 7 can be qualitatively and quantitatively analyzed.
  • the secondary ion mass spectrometer only analyzes the solid sample and does not analyze the gas sample, thus causing the secondary ion mass spectrometer to have certain requirements on the morphology of the sample (that is, the gas sample cannot be analyzed), and the use range has certain limitations. If it is possible to analyze a gas sample using a secondary ion mass spectrometer, it is bound to be able to extend two Application areas of secondary ion mass spectrometers. Summary of the invention
  • the present invention provides a system for analyzing a gas sample using a secondary ion mass spectrometer, comprising: an extraction electrode, a metal plate, and a gas introduction conduit; the extraction electrode and the metal plate are located at In the sample chamber of the secondary ion mass spectrometer, the bow [the outlet is provided with a first through hole for passing primary ions, a second through hole for passing secondary ions, and for introducing through the gas a third through hole of the conduit; the gas introduction conduit passes through the third through hole to guide the gas sample to a surface of the metal plate, and the gas sample forms the under the bombardment of the primary ions a secondary ion; an electric field is formed between the outlet of the bow I and the metal plate, so that the secondary ions fly away from the metal plate through the second through hole into the secondary ion mass spectrometer for mass analysis.
  • the bow [outer ground potential, the secondary ions are negative ions, and the metal plate is connected to a negative voltage such that the secondary ions are repulsed into the secondary ion mass spectrometry
  • the instrument performs quality analysis.
  • the gas sample is bowed [guided to a region of the surface of the metal sheet, the primary ion bombarding the region such that the gas sample in the vicinity of the region is ionized to generate the Secondary ions.
  • the bow [the exit electrode and the metal plate are kept at a certain distance, the sample chamber is in a vacuum state; and the electric field is a uniform electric field.
  • the distance is 5 mm (i.e., mm)
  • the surface of the metal plate is smooth and flat; and the metal plate does not contain an element contained in the gas sample.
  • the second through hole on the extraction pole is located at a center of the extraction pole to form a central hole, and the first through hole and the third through hole are symmetrically distributed in the second through hole. Both sides of the hole.
  • the thickness of the extraction pole is about 2 mm (ie, mm), and the material is a metal material including non-magnetic stainless steel; the first through hole, the second through hole, and the third through hole.
  • the hole has a diameter of about 2 mm (ie, mm); the material of the metal plate includes pure gold or indium or tungsten metal material.
  • the gas introduction conduit further comprises a valve for regulating a flow rate of the gas sample into the sample chamber; the gas introduction conduit is a thin tube made of a metal material, the metal Materials include non-magnetic stainless steel.
  • the gas introduction conduit is grounded, the gas introduction conduit introduces the gas sample from the sample chamber into the sample chamber, the end of the gas introduction conduit and the extraction Extremely flush, the gas introduction conduit has an inner diameter of about 0.5 mm (i.e., mm) and an outer diameter of about 1 mm (i.e., mm;).
  • the primary ion comprises a cesium ion or a gallium ion
  • the gas sample is a non-corrosive gas, including oxygen (ie, 02), nitrogen (ie, N2) or carbon dioxide ( That is, C02)
  • the secondary ion mass spectrometer comprises a magnetic mass spectrometer, a time-of-flight mass spectrometer or a quadrupole mass spectrometer; the secondary ions enter the electric field and/or magnetic field of the secondary ion mass spectrometer for mass analysis.
  • the present invention also provides a method for analyzing a gas sample using a secondary ion mass spectrometer comprising using a bow [exit, metal plate and gas introduction conduit; the extraction pole and the metal plate are located in the secondary ion mass spectrometer a sample chamber having a first through hole for passing primary ions, a second through hole for passing secondary ions, and a third through hole for passing through the gas introduction conduit, It is characterized by the following steps:
  • Step 1 passing the gas introduction conduit through the third through hole, and guiding the gas sample to a surface of the metal plate using the gas introduction conduit;
  • Step 2 using the primary ion pair to bombard the gas sample guided to the surface of the metal plate to form the secondary ion;
  • Step 3 an electric field is formed between the extraction pole and the metal plate, and the secondary ions are passed through the metal plate through the second through hole to enter the secondary ion mass spectrometer for mass analysis.
  • step 3 specifically includes: grounding the extraction pole to a ground potential, and connecting the metal plate to a negative voltage such that the secondary ions are repulsed into the secondary ion mass spectrometer for mass Analysis wherein the secondary ion is an anion.
  • the step 1 comprises: guiding the gas sample to a certain area of the surface of the metal plate; and the step 2 specifically comprises: bombarding the area with the primary ion to make the vicinity of the area The gas sample is ionized to generate the secondary ions.
  • the sample chamber is evacuated; in the step 3, the extraction pole and the metal plate are kept at a certain distance, and the electric field is a uniform electric field.
  • the distance is 5 mm (i.e., mm)
  • the surface of the metal plate is smooth and flat; and the metal plate does not contain an element contained in the gas sample.
  • the second through hole on the extraction pole is located at a center of the extraction pole to form a central hole, and the first through hole and the third through hole are symmetrically distributed in the second through hole. Both sides of the hole.
  • the thickness of the extraction pole is about 2 mm (ie, mm), and the material is a metal material including non-magnetic stainless steel; the first through hole, the second through hole, and the third through hole.
  • the hole has a diameter of about 2 mm (ie, mm); the material of the metal plate includes pure gold or indium or tungsten metal material.
  • the step 1 further comprises: using a valve included in the gas introduction conduit to adjust a flow rate of the gas sample into the sample chamber; the gas introduction conduit is made of a metal material. Tube, the metal material includes non-magnetic stainless steel.
  • the gas in the step 1 is introduced into a conduit ground potential, and the gas introduction conduit introduces the gas sample from the outside of the sample chamber into the sample chamber, the end of the gas introduction conduit and The extraction is extremely flush, and the gas introduction conduit has an inner diameter of about 0.5 mm (i.e., mm) and an outer diameter of about 1 mm (i.e., mm).
  • the primary ion comprises a cesium ion or a gallium ion
  • the gas sample is a non-corrosive gas, including oxygen (ie, 02), nitrogen (ie, N2) or carbon dioxide ( That is, C02)
  • the secondary ion mass spectrometer comprises a magnetic mass spectrometer, a time-of-flight mass spectrometer or a quadrupole mass spectrometer; the secondary ions in step 3 enter the electric field of the secondary ion mass spectrometer and/or Magnetic field for mass analysis.
  • the present invention has the following advantages over the prior art: Since the gas introduction guide is used to guide the gas sample to the surface of the metal plate for ionization, and through the bow [the electric field between the electrode and the metal plate will be The secondary ion beam I is introduced into the secondary ion mass spectrometer for mass analysis, so that the purpose of analyzing the gas sample using the secondary ion mass spectrometer can be realized, and the application field of the conventional secondary ion mass spectrometer is expanded; further, the present invention can use the mass The primary ion bombards the gas sample. Since the larger mass of primary ions (such as helium ions) is highly efficient in ionization of the gas sample, the sensitivity of the gas sample analysis can be improved, and the analysis effect is better.
  • the gas introduction guide is used to guide the gas sample to the surface of the metal plate for ionization, and through the bow [the electric field between the electrode and the metal plate will be The secondary ion beam I is introduced into the secondary ion mass spectrometer
  • FIG. 1 is a schematic structural view of a conventional secondary ion mass spectrometer
  • FIG. 2 is a schematic view showing the structure of a system for analyzing a gas sample using a secondary ion mass spectrometer of the present invention. detailed description
  • Embodiment 1 of the present invention provides a system for analyzing a gas sample using a secondary ion mass spectrometer, comprising: an extraction pole 22, a metal plate 23, and a gas introduction conduit 28; the extraction pole 22 and the The metal plate 23 is located in the sample chamber 32 of the secondary ion mass spectrometer, and the extraction electrode is provided with a first through hole 34 for passing the primary ions 24 (the path 21 along the primary ion 24) a second through hole 35 through the secondary ion 27 (the secondary ion 27 along the path 29 of the secondary ion), and a third through hole 36 for passing through the gas introduction conduit; the gas introduction conduit 28 Leading the gas sample to a surface of the metal plate after passing through the third through hole, the gas sample forming the secondary ions under bombardment of the primary ions; the extracting pole and the metal An electric field is formed between the plates to cause the secondary ions to fly away from the metal plate through the second through holes into the secondary ion mass spectrometer for mass
  • the gas introduction guide is used to guide the gas sample to the surface of the metal plate for ionization, and the secondary ion bow is introduced into the secondary ion mass spectrometer by the electric field between the electrode and the metal plate, it can be used for mass analysis.
  • the purpose of analyzing a gas sample by a secondary ion mass spectrometer extends the field of application of a conventional secondary ion mass spectrometer; in addition, the present invention is capable of bombarding a gas sample with a large mass of primary ions, Larger mass primary ions (such as helium ions) have high ionization efficiency for gas samples, so the sensitivity of gas sample analysis can be improved, and the analysis effect is better.
  • the extraction pole 22 is grounded at a potential 30, the secondary ion 27 is a negative ion, and the metal plate is connected to a negative voltage 31 such that the secondary ion is repulsed into the secondary ion mass spectrometer for mass analysis.
  • the gas sample 26 is bowed to a certain region 25 of the surface of the metal plate, and the primary ions 24 bombard the region to ionize the gas sample 26 near the region to generate the secondary ions 27.
  • the extraction pole 22 and the metal plate 23 are kept at a certain distance, and the sample chamber is in a vacuum state; the electric field is a uniform electric field.
  • the distance is about 5 mm, and the surface of the metal plate is smooth and flat; the metal plate does not contain elements contained in the gas sample.
  • the second through hole on the extraction pole 22 is located at a center of the extraction pole to form a central hole, and the first through hole and the third through hole are symmetrically distributed on both sides of the second through hole.
  • the lead-out pole 22 has a thickness of about 2 mm and is made of a metal material including non-magnetic stainless steel; the first through hole, the second through hole, and the third through hole have a diameter of about 2 mm; and the material of the metal plate includes pure Gold or indium or tungsten metal materials.
  • the gas introduction conduit 28 further includes a valve 33 for regulating the flow rate of the gas sample into the sample chamber; the gas introduction conduit is a thin tube made of a metal material including a non-magnetic stainless steel.
  • the gas introduction conduit 28 is grounded (here the gas is introduced into the conduit ground potential so that the gas introduction conduit and the extraction pole are connected to the same ground potential to ensure a uniform electric field between the metal plate and the extraction pole), the gas introduction A conduit introduces the gas sample from the sample chamber into the sample chamber.
  • the end of the gas introduction conduit is flush with the outlet pole (eg, the distance between the end of the gas introduction conduit and the metal plate 23 can be made) Consistent with the distance between the extraction pole 22 and the metal plate 23, so that the end of the gas bow I into the conduit is flush with the edge of the bow I, at this time the gas bow [the distance between the end of the inlet conduit and the metal plate is about 5 mm
  • the gas bow [the distance between the end of the inlet conduit and the metal plate is about 5 mm
  • Such a distance can prevent the gas from being randomly diffused into the vacuum due to the excessive distance, and is not easily bombarded into ions, and can also prevent the uniform electric field formed between the metal plate and the extraction electrode from being affected due to the too close distance),
  • This enables the gas introduction duct to be level with the metal plate, so that the gas easily reaches the metal plate, and the extraction pole 22 and the metal plate 2 are secured.
  • the gas introduction conduit has an inner diameter of about 0.5
  • the primary ion 24 includes helium ions or gallium ions;
  • the gas sample 26 is a non-corrosive gas, including oxygen, nitrogen or carbon dioxide;
  • the secondary ion mass spectrometer comprises a magnetic mass spectrometer, a time-of-flight mass spectrometer or A quadrupole mass spectrometer;
  • the secondary ions 27 enter the electric field and/or magnetic field of the secondary ion mass spectrometer for mass analysis.
  • the present invention places a flat metal plate in the sample chamber, and introduces the gas sample through the gas introduction conduit to the surface of the sample, and uses a single ion bombardment of the metal plate to ionize the gas molecules in the vicinity of the metal plate to form. Negative ions, because the metal plate is negatively charged, the negative ions are repulsed into the secondary ion mass spectrometer for mass analysis.
  • the system of the present invention mainly comprises: an extraction pole 22, a metal plate 23, a gas introduction guide 28, a sample chamber 32, and a valve 33.
  • the extraction pole 22, the metal plate 23 is located in the sample chamber 32.
  • the lead-out pole 22 is made of a metal material, and may be a non-magnetic stainless steel having a thickness of about 2 mm.
  • the distance between the lead 22 and the metal plate 23 is about 5 mm.
  • the grounding potential 22 of the extraction pole 22 is connected to the negative voltage of the metal plate 23, and an electric field is formed between the extraction pole 22 and the metal plate 23 so that the secondary ions 27 fly away from the surface of the metal plate 23 through the center hole of the extraction electrode 22.
  • the metal plate 23 may be made of pure gold or a metal material such as indium or tungsten.
  • the metal plate 23 does not contain elements contained in the gas sample 26 to be analyzed, so that the primary ions 24 do not ionize the elements in the metal plate 23, thereby affecting the analysis results.
  • the surface of the metal plate 23 is smooth and flat to ensure a uniform electric field between the extraction pole 22 and the metal plate 23.
  • the gas introduction duct 28 is a thin tube made of a metal material, and may be a non-magnetic stainless steel.
  • the gas is introduced into the conduit 28 to ground potential.
  • the gas introduction conduit 28 introduces the gas sample 26 from the outside of the sample chamber 32 into the surface of the metal plate 23 in the sample chamber 32.
  • the end of the gas introduction conduit 28 is flush with the extraction pole 22, and the gas introduction conduit 28 has an inner diameter of about 0.5 mm and an outer diameter of about 1 mm so as not to affect the uniformity of the electric field between the extraction pole 22 and the metal plate 23.
  • the sample chamber 32 is in a vacuum state.
  • Valve 33 regulates the flow of gas sample 26 into sample chamber 12.
  • the system of the present invention operates as follows: Primary ions 24 reach the surface of the metal plate 23 along the path 21, It is bombarded on the metal plate 23 with a certain amount of energy. Since the gas sample 26 is generally composed of a non-metal element, the primary ions 24 may be cerium ions or gallium ions or the like, which are liable to ionize non-metal elements.
  • the gas sample 26 to be analyzed is transported through a gas introduction conduit 28 to a surface area 25 of the metal sheet 23 (i.e., the bombardment area 25).
  • the flow rate of the gas sample 26 entering the sample chamber 32 can be controlled by adjusting the valve 33 outside the sample chamber 32.
  • the gas sample 26 can be any non-corrosive gas (oxygen, nitrogen or carbon dioxide, etc.).
  • the primary ions 24 bombard the gas sample 26 to ionize it, thereby converting into secondary ions 27. Due to the electric field between the extraction pole 22 and the metal plate 23, the secondary ions 27 fly away from the bombardment region 25 along the path 29 by the electric field, and enter the electric field or the magnetic field to achieve mass separation.
  • the secondary ion mass spectrometer may be a magnetic mass spectrometer or a time-of-flight mass spectrometer or a quadrupole mass spectrometer.
  • the system of the present invention is capable of qualitative and quantitative analysis of gas samples using a secondary ion mass spectrometer, expanding its field of application.
  • Embodiment 2 of the present invention provides a method for analyzing a gas sample using a secondary ion mass spectrometer, comprising: using an extraction pole, a metal plate, and a gas introduction conduit; the extraction electrode and the metal plate are located in the secondary ion mass spectrometer a sample chamber having a first through hole for passing primary ions, a second through hole for passing secondary ions, and a third through hole for passing through the gas introduction conduit, including The following steps:
  • Step 1 passing the gas introduction conduit through the third through hole, and guiding the gas sample to a surface of the metal plate using the gas introduction conduit;
  • Step 2 using the primary ion pair to bombard the gas sample guided to the surface of the metal plate to form the secondary ion;
  • Step 3 an electric field is formed between the extraction pole and the metal plate, and the secondary ions are passed through the metal plate through the second through hole to enter the secondary ion mass spectrometer for mass analysis.
  • Step 3 specifically includes: placing the extraction pole ground potential 30, connecting the metal plate to a negative voltage such that the secondary ions are repulsed into the secondary ion mass spectrometer for mass analysis, wherein the secondary ions are Negative ions.
  • Step 1 specifically includes: guiding the gas sample to a certain area of the surface of the metal plate;
  • the step 2 specifically includes bombarding the region with the primary ions such that the gas sample in the vicinity of the region is ionized to generate the secondary ions.
  • the sample chamber is further evacuated; in the step 3, the extraction pole and the metal plate are kept at a certain distance, and the electric field is a uniform electric field.
  • the distance is about 5 mm, and the surface of the metal plate is smooth and flat; the metal plate does not contain elements contained in the gas sample.
  • the second through hole on the extraction pole is located at a center of the extraction pole to form a central hole, and the first through hole and the third through hole are symmetrically distributed on both sides of the second through hole.
  • the lead electrode has a thickness of about 2 mm and is made of a metal material including non-magnetic stainless steel; the first through hole, the second through hole, and the third through hole have a diameter of about 2 mm; and the material of the metal plate includes pure Gold or indium or tungsten metal materials.
  • the step 1 further includes using a valve included in the gas introduction conduit to adjust a flow rate of the gas sample into the sample chamber;
  • the gas introduction conduit is a thin tube made of a metal material including a non-magnetic stainless steel.
  • the gas introduction conduit is connected to a potential in step 1, the gas introduction conduit introducing the gas sample from the sample chamber into the sample chamber, the end of the gas introduction conduit being flush with the extraction pole, the gas
  • the introduction catheter has an inner diameter of about 0.5 mm and an outer diameter of about 1 mm.
  • the primary ion comprises a cesium ion or a gallium ion
  • the gas sample is a non-corrosive gas, including oxygen, nitrogen or carbon dioxide
  • the secondary ion mass spectrometer comprises a magnetic mass spectrometer, a time-of-flight mass spectrometer Or a quadrupole mass spectrometer; the secondary ions in step 3 enter the electric field and/or magnetic field of the secondary ion mass spectrometer for mass analysis.
  • Embodiment 4 of the present invention includes the following steps:
  • Step 1 Place the metal plate in the sample chamber of the secondary ion mass spectrometer for general analysis of the position of the solid sample, evacuate the sample chamber, and add a negative voltage to the metal plate 31;
  • Step 2 introducing a gas sample into the sample chamber through a gas introduction conduit;
  • the gas introduction conduit may be made of a metal stainless steel material having an inner diameter of about 0.5 mm and an outer diameter of about 1 mm; and the outlet of the gas introduction conduit is about 5 mm from the surface of the metal plate; Introducing a conduit ground potential;
  • Step 3 Using a single ion bombardment of the metal plate, the gas sample near the metal plate (for example, gas) Ionized, causing it to become a negative ion (ie, a secondary ion);
  • Step 4 The negative ions (ie, secondary ions) are sent to the secondary ion mass spectrometer, and the electric field and the magnetic field of the secondary ion mass spectrometer are used for qualitative and quantitative analysis according to the quality.

Abstract

Provided are a system and method for analyzing a gas sample by using a secondary ion mass spectrometer. The system comprises: an extraction electrode, a metal plate and a gas lead-in pipe, wherein the extraction electrode and the metal plate are located in a sample chamber of the secondary ion mass spectrometer; a first through hole through which primary ions pass, a second through hole through which secondary ions pass, and a third through hole through which the gas lead-in pipe penetrates are provided on the extraction electrode; after penetrating through the third through hole, the gas lead-in pipe leads the gas sample to the surface of the metal plate, and the gas sample is bombarded by the primary ions to form the secondary ions; and an electric field is formed between the extraction electrode and the metal plate, so that the secondary ions pass through the second through hole to depart from the metal plate and enter the secondary ion mass spectrometer for mass analysis.

Description

说 明 书 使用二次离子质谱仪分析气体样品的系统和方法 技术领域  Description System and method for analyzing gas samples using secondary ion mass spectrometry
本发明涉及分析仪器技术领域,特别涉及一种使用二次离子质谱仪分析气体 样品的系统和方法。 背景技术  Field of the Invention This invention relates to the field of analytical instrumentation, and more particularly to a system and method for analyzing a gas sample using a secondary ion mass spectrometer. Background technique
二次离子质谱仪通常用来对固体样品进行微区原位分析,表面分析和深度分 析, 其广泛应用于材料科学、 生命科学、 地质科学等领域的研究。二次离子质谱 仪的分析过程是将固体样品置于真空中,使用特定种类的一次离子对固体样品进 行轰击,样品在一定能量的一次离子的轰击下,溅射出二次离子,二次离子代表 了样品成分的信息。根据溅射出的二次离子质量的不同,使用电场或磁场将二次 离子从时间上或空间上分离开,从而判断出二次离子的种类和数量,以便能够实 现对固体样品的定性和定量分析。  Secondary ion mass spectrometers are commonly used for in-situ analysis, surface analysis and in-depth analysis of solid samples, which are widely used in materials science, life sciences, geological sciences and other fields. The analysis process of the secondary ion mass spectrometer is to place the solid sample in a vacuum, bombard the solid sample with a specific kind of primary ion, and the sample is sputtered with secondary ions under the bombardment of a certain energy of one ion, and the secondary ion represents Information on the composition of the sample. Depending on the quality of the sputtered secondary ions, the secondary ions are separated temporally or spatially using an electric or magnetic field to determine the type and amount of secondary ions in order to enable qualitative and quantitative analysis of solid samples. .
一般采用磁场做质量分析器的二次离子质谱仪的原理如图 1所示,一次离子 源 1产生一次离子 2。 一次离子 2经过离子光学透镜 3, 5, 6产生的电场聚焦到 样品 7 (样品 7位于样品室内) 的表面, 对样品 7进行轰击。 一次离子 2和离子 光学透镜 3, 5, 6位于真空腔 4内。一次离子 2对样品 7进行轰击, 将部分样品 7离子化, 产生二次离子 9。 二次离子 9经过离子光学透镜 10, 11, 12 , 静电场 分析器 13, 离子光学透镜 15, 磁场分析器 16, 离子光学透镜 18, 到达接收器 19。样品 7和离子光学透镜 10, 11, 12位于真空腔体 8内。离子光学透镜 15位 于真空腔体 14内。离子光学透镜 18位于真空腔体 17内。静电场分析器 13和磁 场分析器 16组成双聚焦结构, 在实现二次离子 9的质量分离的同时, 实现角度 聚焦和能量聚焦。 磁场分析器 16的强度决定了接收器 19所接收到的离子种类。 根据接收器 19所接收的信号强度, 就可以对样品 7进行定性和定量分析。  The principle of a secondary ion mass spectrometer, which generally uses a magnetic field as a mass analyzer, is shown in Figure 1. The primary ion source 1 produces a primary ion 2 . The primary ion 2 is focused by the electric field generated by the ion optical lenses 3, 5, 6 onto the surface of sample 7 (sample 7 is located in the sample chamber), and sample 7 is bombarded. The primary ion 2 and ion optical lenses 3, 5, 6 are located within the vacuum chamber 4. The primary ion 2 bombards the sample 7, and a part of the sample 7 is ionized to generate secondary ions 9. The secondary ions 9 pass through the ion optical lens 10, 11, 12 , an electrostatic field analyzer 13, an ion optical lens 15, a magnetic field analyzer 16, an ion optical lens 18, and reach the receiver 19. Sample 7 and ion optical lenses 10, 11, 12 are located within vacuum chamber 8. The ion optical lens 15 is located within the vacuum chamber 14. The ion optical lens 18 is located within the vacuum chamber 17. The electrostatic field analyzer 13 and the magnetic field analyzer 16 constitute a double focusing structure for achieving angular focusing and energy focusing while achieving mass separation of the secondary ions 9. The intensity of the magnetic field analyzer 16 determines the type of ions received by the receiver 19. Depending on the signal strength received by the receiver 19, the sample 7 can be qualitatively and quantitatively analyzed.
传统上二次离子质谱仪只分析固体样品,不分析气体样品, 因此导致二次离 子质谱仪对样品的形态具有一定的要求 (也即无法分析气体样品), 使用范围上 有一定的局限性。如果能够使用二次离子质谱仪分析气体样品,势必能够延伸二 次离子质谱仪的应用领域。 发明内容 Traditionally, the secondary ion mass spectrometer only analyzes the solid sample and does not analyze the gas sample, thus causing the secondary ion mass spectrometer to have certain requirements on the morphology of the sample (that is, the gas sample cannot be analyzed), and the use range has certain limitations. If it is possible to analyze a gas sample using a secondary ion mass spectrometer, it is bound to be able to extend two Application areas of secondary ion mass spectrometers. Summary of the invention
本发明的主要目的是提供一种使用二次离子质谱仪分析气体样品的系统。 本发明的另一目的是提供一种使用二次离子质谱仪分析气体样品的方法。 为了达到上述目的,本发明提供了一种使用二次离子质谱仪分析气体样品的 系统, 其特征在于, 包括: 引出极、 金属板和气体引入导管; 所述引出极和所述 金属板位于所述二次离子质谱仪的样品室内,所述弓 [出极上设有用于通过一次离 子的第一通孔、用于通过二次离子的第二通孔、以及用于穿过所述气体引入导管 的第三通孔;所述气体引入导管穿过所述第三通孔后将所述气体样品引导至所述 金属板的表面,所述气体样品在所述一次离子的轰击下形成所述二次离子;所述 弓 I出极和所述金属板之间形成电场,以使所述二次离子通过所述第二通孔飞离所 述金属板进入所述二次离子质谱仪进行质量分析。  A primary object of the present invention is to provide a system for analyzing a gas sample using a secondary ion mass spectrometer. Another object of the present invention is to provide a method of analyzing a gas sample using a secondary ion mass spectrometer. In order to achieve the above object, the present invention provides a system for analyzing a gas sample using a secondary ion mass spectrometer, comprising: an extraction electrode, a metal plate, and a gas introduction conduit; the extraction electrode and the metal plate are located at In the sample chamber of the secondary ion mass spectrometer, the bow [the outlet is provided with a first through hole for passing primary ions, a second through hole for passing secondary ions, and for introducing through the gas a third through hole of the conduit; the gas introduction conduit passes through the third through hole to guide the gas sample to a surface of the metal plate, and the gas sample forms the under the bombardment of the primary ions a secondary ion; an electric field is formed between the outlet of the bow I and the metal plate, so that the secondary ions fly away from the metal plate through the second through hole into the secondary ion mass spectrometer for mass analysis.
在上述任一方案中优选的是,所述弓 [出极接地电位,所述二次离子为负离子, 所述金属板接负电压使得所述二次离子被推斥进入所述二次离子质谱仪进行质 量分析。  In any of the above aspects, preferably, the bow [outer ground potential, the secondary ions are negative ions, and the metal plate is connected to a negative voltage such that the secondary ions are repulsed into the secondary ion mass spectrometry The instrument performs quality analysis.
在上述任一方案中优选的是,所述气体样品被弓 [导至所述金属板表面的一定 区域,所述一次离子轰击该区域使得该区域附近的所述气体样品离子化而生成所 述二次离子。  In any of the above aspects, it is preferred that the gas sample is bowed [guided to a region of the surface of the metal sheet, the primary ion bombarding the region such that the gas sample in the vicinity of the region is ionized to generate the Secondary ions.
在上述任一方案中优选的是, 所述弓 [出极和所述金属板之间保持一定距离, 所述样品室处于真空状态; 所述电场为均匀电场。  In any of the above aspects, it is preferable that the bow [the exit electrode and the metal plate are kept at a certain distance, the sample chamber is in a vacuum state; and the electric field is a uniform electric field.
在上述任一方案中优选的是, 所述距离为 5毫米 (也即 mm)左右, 所述金属 板的表面光滑平整; 所述金属板内不含所述气体样品所包含的元素。  In any of the above aspects, it is preferable that the distance is 5 mm (i.e., mm), the surface of the metal plate is smooth and flat; and the metal plate does not contain an element contained in the gas sample.
在上述任一方案中优选的是,所述引出极上的第二通孔位于所述引出极的中 央形成中心孔, 所述第一通孔和第三通孔对称分布在所述第二通孔的两侧。  Preferably, in any one of the above aspects, the second through hole on the extraction pole is located at a center of the extraction pole to form a central hole, and the first through hole and the third through hole are symmetrically distributed in the second through hole. Both sides of the hole.
在上述任一方案中优选的是, 所述引出极的厚度约 2毫米 (也即 mm), 材质 为包括无磁不锈钢的金属材质; 所述第一通孔、 第二通孔、 第三通孔直径约 2 毫米 (也即 mm) ; 所述金属板的材质包括纯的金或铟或钨金属材料。 在上述任一方案中优选的是,所述气体引入导管还包括阀门,用于调节所述 气体样品进入所述样品室的流量; 所述气体引入导管选用金属材质制成的细管, 该金属材质包括无磁不锈钢。 Preferably, in any one of the above aspects, the thickness of the extraction pole is about 2 mm (ie, mm), and the material is a metal material including non-magnetic stainless steel; the first through hole, the second through hole, and the third through hole. The hole has a diameter of about 2 mm (ie, mm); the material of the metal plate includes pure gold or indium or tungsten metal material. Preferably, in any one of the above aspects, the gas introduction conduit further comprises a valve for regulating a flow rate of the gas sample into the sample chamber; the gas introduction conduit is a thin tube made of a metal material, the metal Materials include non-magnetic stainless steel.
在上述任一方案中优选的是,所述气体引入导管接地电位,所述气体引入导 管将所述气体样品从所述样品室外引入所述样品室内,所述气体引入导管的末端 与所述引出极齐平, 所述气体引入导管内径约 0.5毫米 (也即 mm), 外径约 1毫 米 (;也即 mm;)。  Preferably, in any of the above aspects, the gas introduction conduit is grounded, the gas introduction conduit introduces the gas sample from the sample chamber into the sample chamber, the end of the gas introduction conduit and the extraction Extremely flush, the gas introduction conduit has an inner diameter of about 0.5 mm (i.e., mm) and an outer diameter of about 1 mm (i.e., mm;).
在上述任一方案中优选的是,所述一次离子包括铯离子或镓离子;所述气体 样品为无强烈腐蚀性的气体, 包括氧气 (也即 02), 氮气 (也即 N2)或二氧化碳 (也 即 C02) ; 所述二次离子质谱仪包括磁式质谱仪、 飞行时间质谱仪或四极杆质谱 仪; 所述二次离子进入所述二次离子质谱仪的电场和 /或磁场进行质量分析。  In any of the above aspects, it is preferred that the primary ion comprises a cesium ion or a gallium ion; the gas sample is a non-corrosive gas, including oxygen (ie, 02), nitrogen (ie, N2) or carbon dioxide ( That is, C02); the secondary ion mass spectrometer comprises a magnetic mass spectrometer, a time-of-flight mass spectrometer or a quadrupole mass spectrometer; the secondary ions enter the electric field and/or magnetic field of the secondary ion mass spectrometer for mass analysis.
本发明还提供了一种使用二次离子质谱仪分析气体样品的方法,包括采用弓 [ 出极、金属板和气体引入导管;所述引出极和所述金属板位于所述二次离子质谱 仪的样品室内,所述引出极上设有用于通过一次离子的第一通孔、用于通过二次 离子的第二通孔、 以及用于穿过所述气体引入导管的第三通孔,其特征在于,包 括以下步骤:  The present invention also provides a method for analyzing a gas sample using a secondary ion mass spectrometer comprising using a bow [exit, metal plate and gas introduction conduit; the extraction pole and the metal plate are located in the secondary ion mass spectrometer a sample chamber having a first through hole for passing primary ions, a second through hole for passing secondary ions, and a third through hole for passing through the gas introduction conduit, It is characterized by the following steps:
步骤 1, 将所述气体引入导管穿过所述第三通孔, 使用所述气体引入导管将 所述气体样品引导至所述金属板的表面;  Step 1, passing the gas introduction conduit through the third through hole, and guiding the gas sample to a surface of the metal plate using the gas introduction conduit;
步骤 2,采用所述一次离子对引导至所述金属板表面的所述气体样品进行轰 击, 形成所述二次离子;  Step 2, using the primary ion pair to bombard the gas sample guided to the surface of the metal plate to form the secondary ion;
步骤 3, 在所述引出极和所述金属板之间形成电场, 使所述二次离子通过所 述第二通孔飞离所述金属板进入所述二次离子质谱仪进行质量分析。  Step 3, an electric field is formed between the extraction pole and the metal plate, and the secondary ions are passed through the metal plate through the second through hole to enter the secondary ion mass spectrometer for mass analysis.
在上述任一方案中优选的是,步骤 3具体包括:将所述引出极接地电位,将 所述金属板接负电压使得所述二次离子被推斥进入所述二次离子质谱仪进行质 量分析, 其中所述二次离子为负离子。  Preferably, in any one of the above aspects, step 3 specifically includes: grounding the extraction pole to a ground potential, and connecting the metal plate to a negative voltage such that the secondary ions are repulsed into the secondary ion mass spectrometer for mass Analysis wherein the secondary ion is an anion.
在上述任一方案中优选的是,步骤 1具体包括:将所述气体样品被引导至所 述金属板表面的一定区域;步骤 2具体包括:使用所述一次离子轰击该区域使得 该区域附近的所述气体样品离子化而生成所述二次离子。 在上述任一方案中优选的是,步骤 1之前还包括将所述样品室抽真空;步骤 3中所述引出极和所述金属板之间保持一定距离, 所述电场为均匀电场。 In any of the above aspects, it is preferable that the step 1 comprises: guiding the gas sample to a certain area of the surface of the metal plate; and the step 2 specifically comprises: bombarding the area with the primary ion to make the vicinity of the area The gas sample is ionized to generate the secondary ions. Preferably, in any of the above aspects, before the step 1, the sample chamber is evacuated; in the step 3, the extraction pole and the metal plate are kept at a certain distance, and the electric field is a uniform electric field.
在上述任一方案中优选的是, 所述距离为 5毫米 (也即 mm)左右, 所述金属 板的表面光滑平整; 所述金属板内不含所述气体样品所包含的元素。  In any of the above aspects, it is preferable that the distance is 5 mm (i.e., mm), the surface of the metal plate is smooth and flat; and the metal plate does not contain an element contained in the gas sample.
在上述任一方案中优选的是,所述引出极上的第二通孔位于所述引出极的中 央形成中心孔, 所述第一通孔和第三通孔对称分布在所述第二通孔的两侧。  Preferably, in any one of the above aspects, the second through hole on the extraction pole is located at a center of the extraction pole to form a central hole, and the first through hole and the third through hole are symmetrically distributed in the second through hole. Both sides of the hole.
在上述任一方案中优选的是, 所述引出极的厚度约 2毫米 (也即 mm), 材质 为包括无磁不锈钢的金属材质; 所述第一通孔、 第二通孔、 第三通孔直径约 2 毫米 (也即 mm) ; 所述金属板的材质包括纯的金或铟或钨金属材料。  Preferably, in any one of the above aspects, the thickness of the extraction pole is about 2 mm (ie, mm), and the material is a metal material including non-magnetic stainless steel; the first through hole, the second through hole, and the third through hole. The hole has a diameter of about 2 mm (ie, mm); the material of the metal plate includes pure gold or indium or tungsten metal material.
在上述任一方案中优选的是,步骤 1中还包括使用所述气体引入导管包括的 阀门来调节所述气体样品进入所述样品室的流量;所述气体引入导管选用金属材 质制成的细管, 该金属材质包括无磁不锈钢。  Preferably, in any one of the above aspects, the step 1 further comprises: using a valve included in the gas introduction conduit to adjust a flow rate of the gas sample into the sample chamber; the gas introduction conduit is made of a metal material. Tube, the metal material includes non-magnetic stainless steel.
在上述任一方案中优选的是,步骤 1中所述气体引入导管接地电位,所述气 体引入导管将所述气体样品从所述样品室外引入所述样品室内,所述气体引入导 管的末端与所述引出极齐平, 所述气体引入导管内径约 0.5毫米 (也即 mm), 外 径约 1毫米 (也即 mm)。  In any of the above aspects, it is preferred that the gas in the step 1 is introduced into a conduit ground potential, and the gas introduction conduit introduces the gas sample from the outside of the sample chamber into the sample chamber, the end of the gas introduction conduit and The extraction is extremely flush, and the gas introduction conduit has an inner diameter of about 0.5 mm (i.e., mm) and an outer diameter of about 1 mm (i.e., mm).
在上述任一方案中优选的是,所述一次离子包括铯离子或镓离子;所述气体 样品为无强烈腐蚀性的气体, 包括氧气 (也即 02), 氮气 (也即 N2)或二氧化碳 (也 即 C02) ; 所述二次离子质谱仪包括磁式质谱仪、 飞行时间质谱仪或四极杆质谱 仪; 步骤 3 中所述二次离子进入所述二次离子质谱仪的电场和 /或磁场进行质量 分析。  In any of the above aspects, it is preferred that the primary ion comprises a cesium ion or a gallium ion; the gas sample is a non-corrosive gas, including oxygen (ie, 02), nitrogen (ie, N2) or carbon dioxide ( That is, C02); the secondary ion mass spectrometer comprises a magnetic mass spectrometer, a time-of-flight mass spectrometer or a quadrupole mass spectrometer; the secondary ions in step 3 enter the electric field of the secondary ion mass spectrometer and/or Magnetic field for mass analysis.
采用本发明的技术方案后, 相对于现有技术本发明具有以下优点: 由于采用 气体引入导管将气体样品引导到金属板表面进行离子化,并通过弓 [出极和金属板 之间的电场将二次离子弓 I导入二次离子质谱仪进行质量分析,因此可以实现使用 二次离子质谱仪分析气体样品的目的, 扩展了传统二次离子质谱仪的应用领域; 此外,本发明能够使用大质量的一次离子对气体样品进行轰击, 由于较大质量的 一次离子(如铯离子等)对气体样品的离子化效率很高, 因此可以提高对气体样 品分析的灵敏度, 分析效果更好。 附图说明 With the technical solution of the present invention, the present invention has the following advantages over the prior art: Since the gas introduction guide is used to guide the gas sample to the surface of the metal plate for ionization, and through the bow [the electric field between the electrode and the metal plate will be The secondary ion beam I is introduced into the secondary ion mass spectrometer for mass analysis, so that the purpose of analyzing the gas sample using the secondary ion mass spectrometer can be realized, and the application field of the conventional secondary ion mass spectrometer is expanded; further, the present invention can use the mass The primary ion bombards the gas sample. Since the larger mass of primary ions (such as helium ions) is highly efficient in ionization of the gas sample, the sensitivity of the gas sample analysis can be improved, and the analysis effect is better. DRAWINGS
为了更清楚的说明本发明的技术方案,下面将对实施例描述中所需要使用的 附图作简单的介绍,显而易见的,下面描述中的附图仅仅是本发明的一些实施例, 对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些 附图获得其他的附图。  In order to more clearly illustrate the technical solutions of the present invention, the drawings used in the description of the embodiments will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the present invention. For the ordinary technicians, other drawings can be obtained based on these drawings without any creative work.
图 1为现有的二次离子质谱仪的结构示意图;  1 is a schematic structural view of a conventional secondary ion mass spectrometer;
图 2为本发明的使用二次离子质谱仪分析气体样品的系统的结构示意图。 具体实施方式  2 is a schematic view showing the structure of a system for analyzing a gas sample using a secondary ion mass spectrometer of the present invention. detailed description
下面将结合本发明实施例中的附图, 对本发明实施例中的技术方案进行清 楚、完整的描述,显然所描述的实施例仅是本发明的一部分实施例,不是全部的 实施例,基于本发明中的实施例,本领域普通技术人员在没有付出创造性劳动前 提下所获得的所有其他实施例, 都属于本发明保护的范围。  The technical solutions in the embodiments of the present invention are clearly and completely described in the following with reference to the accompanying drawings in the embodiments of the present invention, and the embodiments described are only a part of the embodiments of the present invention, not all embodiments, based on the present invention All other embodiments obtained by those skilled in the art without departing from the inventive scope are intended to be within the scope of the invention.
实施例 1  Example 1
如图 2所示,本发明实施例 1提供了一种使用二次离子质谱仪分析气体样品 的系统, 包括: 引出极 22、 金属板 23和气体引入导管 28 ; 所述引出极 22和所 述金属板 23位于所述二次离子质谱仪的样品室 32内,所述引出极上设有用于通 过一次离子 24的第一通孔 34 (—次离子 24沿着一次离子的路径 21)、用于通过 二次离子 27的第二通孔 35 (二次离子 27沿着二次离子的路径 29)、以及用于穿 过所述气体引入导管的第三通孔 36 ;所述气体引入导管 28穿过所述第三通孔后 将所述气体样品引导至所述金属板的表面,所述气体样品在所述一次离子的轰击 下形成所述二次离子;所述引出极和所述金属板之间形成电场,以使所述二次离 子通过所述第二通孔飞离所述金属板进入所述二次离子质谱仪进行质量分析。  As shown in FIG. 2, Embodiment 1 of the present invention provides a system for analyzing a gas sample using a secondary ion mass spectrometer, comprising: an extraction pole 22, a metal plate 23, and a gas introduction conduit 28; the extraction pole 22 and the The metal plate 23 is located in the sample chamber 32 of the secondary ion mass spectrometer, and the extraction electrode is provided with a first through hole 34 for passing the primary ions 24 (the path 21 along the primary ion 24) a second through hole 35 through the secondary ion 27 (the secondary ion 27 along the path 29 of the secondary ion), and a third through hole 36 for passing through the gas introduction conduit; the gas introduction conduit 28 Leading the gas sample to a surface of the metal plate after passing through the third through hole, the gas sample forming the secondary ions under bombardment of the primary ions; the extracting pole and the metal An electric field is formed between the plates to cause the secondary ions to fly away from the metal plate through the second through holes into the secondary ion mass spectrometer for mass analysis.
由于采用气体引入导管将气体样品引导到金属板表面进行离子化, 并通过弓 [ 出极和金属板之间的电场将二次离子弓 [导入二次离子质谱仪进行质量分析,因此 可以实现使用二次离子质谱仪分析气体样品的目的,扩展了传统二次离子质谱仪 的应用领域;此外,本发明能够使用大质量的一次离子对气体样品进行轰击, 由 于较大质量的一次离子(如铯离子等)对气体样品的离子化效率很高, 因此可以 提高对气体样品分析的灵敏度, 分析效果更好。 Since the gas introduction guide is used to guide the gas sample to the surface of the metal plate for ionization, and the secondary ion bow is introduced into the secondary ion mass spectrometer by the electric field between the electrode and the metal plate, it can be used for mass analysis. The purpose of analyzing a gas sample by a secondary ion mass spectrometer extends the field of application of a conventional secondary ion mass spectrometer; in addition, the present invention is capable of bombarding a gas sample with a large mass of primary ions, Larger mass primary ions (such as helium ions) have high ionization efficiency for gas samples, so the sensitivity of gas sample analysis can be improved, and the analysis effect is better.
所述引出极 22接地电位 30, 所述二次离子 27为负离子, 所述金属板接负 电压 31使得所述二次离子被推斥进入所述二次离子质谱仪进行质量分析。  The extraction pole 22 is grounded at a potential 30, the secondary ion 27 is a negative ion, and the metal plate is connected to a negative voltage 31 such that the secondary ion is repulsed into the secondary ion mass spectrometer for mass analysis.
所述气体样品 26被弓 [导至所述金属板表面的一定区域 25,所述一次离子 24 轰击该区域使得该区域附近的所述气体样品 26离子化而生成所述二次离子 27。  The gas sample 26 is bowed to a certain region 25 of the surface of the metal plate, and the primary ions 24 bombard the region to ionize the gas sample 26 near the region to generate the secondary ions 27.
所述引出极 22和所述金属板 23之间保持一定距离,所述样品室处于真空状 态; 所述电场为均匀电场。  The extraction pole 22 and the metal plate 23 are kept at a certain distance, and the sample chamber is in a vacuum state; the electric field is a uniform electric field.
所述距离为 5毫米左右,所述金属板的表面光滑平整;所述金属板内不含所 述气体样品所包含的元素。  The distance is about 5 mm, and the surface of the metal plate is smooth and flat; the metal plate does not contain elements contained in the gas sample.
所述引出极 22上的第二通孔位于所述引出极的中央形成中心孔, 所述第一 通孔和第三通孔对称分布在所述第二通孔的两侧。  The second through hole on the extraction pole 22 is located at a center of the extraction pole to form a central hole, and the first through hole and the third through hole are symmetrically distributed on both sides of the second through hole.
所述引出极 22的厚度约 2毫米, 材质为包括无磁不锈钢的金属材质; 所述 第一通孔、第二通孔、第三通孔直径约 2毫米;所述金属板的材质包括纯的金或 铟或钨金属材料。  The lead-out pole 22 has a thickness of about 2 mm and is made of a metal material including non-magnetic stainless steel; the first through hole, the second through hole, and the third through hole have a diameter of about 2 mm; and the material of the metal plate includes pure Gold or indium or tungsten metal materials.
所述气体引入导管 28还包括阀门 33,用于调节所述气体样品进入所述样品 室的流量;所述气体引入导管选用金属材质制成的细管,该金属材质包括无磁不 锈钢。  The gas introduction conduit 28 further includes a valve 33 for regulating the flow rate of the gas sample into the sample chamber; the gas introduction conduit is a thin tube made of a metal material including a non-magnetic stainless steel.
优化的, 所述气体引入导管 28接地电位 (这里气体引入导管接地电位, 使 得气体引入导管和引出极接同样的地电位,以保证金属板和引出极之间形成均匀 电场), 所述气体引入导管将所述气体样品从所述样品室外引入所述样品室内, 优化的,所述气体引入导管的末端与所述引出极齐平(例如可以使得气体引入导 管末端与金属板 23之间的距离与引出极 22和金属板 23之间的距离一致, 以使 气体弓 I入导管的末端与弓 I出极齐平,此时气体弓 [入导管末端与金属板之间的距离 为 5毫米左右,这样的距离能够防止由于距离过远导致气体随意扩散到真空里而 不易被轰击变成离子,同时也能够防止由于距离过近而对金属板和引出极之间形 成的均匀电场产生影响), 这样能够使气体引入导管末端与金属板保持水平, 使 得气体容易到达金属板,并保证引出极 22和金属板 23之间形成均匀电场;所述 气体引入导管内径约 0.5毫米, 外径约 1毫米。 Optimized, the gas introduction conduit 28 is grounded (here the gas is introduced into the conduit ground potential so that the gas introduction conduit and the extraction pole are connected to the same ground potential to ensure a uniform electric field between the metal plate and the extraction pole), the gas introduction A conduit introduces the gas sample from the sample chamber into the sample chamber. Optimized, the end of the gas introduction conduit is flush with the outlet pole (eg, the distance between the end of the gas introduction conduit and the metal plate 23 can be made) Consistent with the distance between the extraction pole 22 and the metal plate 23, so that the end of the gas bow I into the conduit is flush with the edge of the bow I, at this time the gas bow [the distance between the end of the inlet conduit and the metal plate is about 5 mm Such a distance can prevent the gas from being randomly diffused into the vacuum due to the excessive distance, and is not easily bombarded into ions, and can also prevent the uniform electric field formed between the metal plate and the extraction electrode from being affected due to the too close distance), This enables the gas introduction duct to be level with the metal plate, so that the gas easily reaches the metal plate, and the extraction pole 22 and the metal plate 2 are secured. Forming a uniform electric field between 3; The gas introduction conduit has an inner diameter of about 0.5 mm and an outer diameter of about 1 mm.
所述一次离子 24包括铯离子或镓离子;所述气体样品 26为无强烈腐蚀性的 气体,包括氧气, 氮气或二氧化碳;所述二次离子质谱仪包括磁式质谱仪、 飞行 时间质谱仪或四极杆质谱仪; 所述二次离子 27进入所述二次离子质谱仪的电场 和 /或磁场进行质量分析。  The primary ion 24 includes helium ions or gallium ions; the gas sample 26 is a non-corrosive gas, including oxygen, nitrogen or carbon dioxide; the secondary ion mass spectrometer comprises a magnetic mass spectrometer, a time-of-flight mass spectrometer or A quadrupole mass spectrometer; the secondary ions 27 enter the electric field and/or magnetic field of the secondary ion mass spectrometer for mass analysis.
实施例 2 Example 2
与实施例 1相似,本发明在样品室内放置一块表面平整的纯金属板,将气体 样品通过气体引入导管引至样品表面,使用一次离子轰击金属板,将金属板附近 的气体分子离子化,形成负离子, 由于金属板带负电, 负离子被推斥进入二次离 子质谱仪进行质量分析。  Similar to the first embodiment, the present invention places a flat metal plate in the sample chamber, and introduces the gas sample through the gas introduction conduit to the surface of the sample, and uses a single ion bombardment of the metal plate to ionize the gas molecules in the vicinity of the metal plate to form. Negative ions, because the metal plate is negatively charged, the negative ions are repulsed into the secondary ion mass spectrometer for mass analysis.
如图 2所示, 本发明的系统主要包括: 引出极 22、 金属板 23、 气体引入导 管 28、 样品室 32、 阀门 33。 引出极 22, 金属板 23位于样品室 32内。 引出极 22为金属材质, 可以是无磁不锈钢, 厚度约 2毫米, 其上有三个直径 2毫米左 右的孔, 一次离子 24的路径 21, 二次离子 27的路径 29和气体引入导管 28分 别通过这三个孔。 引出极 22和金属板 23之间距离大约 5毫米左右。 引出极 22 接地电位 30, 金属板 23接负电压, 引出极 22和金属板 23之间形成电场, 以使 二次离子 27通过引出极 22的中心孔飞离金属板 23的表面。  As shown in Fig. 2, the system of the present invention mainly comprises: an extraction pole 22, a metal plate 23, a gas introduction guide 28, a sample chamber 32, and a valve 33. The extraction pole 22, the metal plate 23 is located in the sample chamber 32. The lead-out pole 22 is made of a metal material, and may be a non-magnetic stainless steel having a thickness of about 2 mm. There are three holes having a diameter of about 2 mm, a path 21 of the primary ion 24, a path 29 of the secondary ion 27, and a gas introduction duct 28 passing through respectively. These three holes. The distance between the lead 22 and the metal plate 23 is about 5 mm. The grounding potential 22 of the extraction pole 22 is connected to the negative voltage of the metal plate 23, and an electric field is formed between the extraction pole 22 and the metal plate 23 so that the secondary ions 27 fly away from the surface of the metal plate 23 through the center hole of the extraction electrode 22.
金属板 23可以是纯的金或铟或钨等金属材料制成。优选地,金属板 23内不 能含有待分析气体样品 26所含有的元素, 以免一次离子 24将金属板 23内的元 素离子化, 影响分析结果。 优选地, 金属板 23的表面要光滑平整, 保证引出极 22和金属板 23之间形成均匀电场。  The metal plate 23 may be made of pure gold or a metal material such as indium or tungsten. Preferably, the metal plate 23 does not contain elements contained in the gas sample 26 to be analyzed, so that the primary ions 24 do not ionize the elements in the metal plate 23, thereby affecting the analysis results. Preferably, the surface of the metal plate 23 is smooth and flat to ensure a uniform electric field between the extraction pole 22 and the metal plate 23.
气体引入导管 28选用金属材质制成的细管, 可以是无磁不锈钢。 气体引入 导管 28接地电位。 气体引入导管 28将气体样品 26从样品室 32外引入样品室 32内的金属板 23的表面。 优选地, 气体引入导管 28的末端与引出极 22齐平, 气体引入导管 28内径 0.5毫米左右, 外径 1毫米左右, 以免影响引出极 22和金 属板 23之间电场的均匀性。 优选地, 样品室 32处于真空状态。 阀门 33可以调 节气体样品 26进入样品室 12的流量。  The gas introduction duct 28 is a thin tube made of a metal material, and may be a non-magnetic stainless steel. The gas is introduced into the conduit 28 to ground potential. The gas introduction conduit 28 introduces the gas sample 26 from the outside of the sample chamber 32 into the surface of the metal plate 23 in the sample chamber 32. Preferably, the end of the gas introduction conduit 28 is flush with the extraction pole 22, and the gas introduction conduit 28 has an inner diameter of about 0.5 mm and an outer diameter of about 1 mm so as not to affect the uniformity of the electric field between the extraction pole 22 and the metal plate 23. Preferably, the sample chamber 32 is in a vacuum state. Valve 33 regulates the flow of gas sample 26 into sample chamber 12.
本发明的系统工作过程如下: 一次离子 24沿路径 21到达金属板 23表面, 以一定的能量轰击在金属板 23上。 由于气体样品 26—般为非金属元素组成,所 以一次离子 24可以是铯离子或镓离子等, 它们易于使非金属元素离子化。 待分 析的气体样品 26通过气体引入导管 28运送到金属板 23的表面一定区域 25 (也 即轰击区域 25)。 通过调节样品室 32外的阀门 33可以控制进入样品室 32内的 气体样品 26的流量。优选地,气体样品 26,可以是任何无强烈腐蚀性的气体(氧 气,氮气或二氧化碳等)。在轰击区域 25处,一次离子 24轰击气体样品 26使其 离子化, 从而转变成二次离子 27。 由于引出极 22和金属板 23之间存在电场, 二次离子 27在电场的作用下, 沿路径 29飞离轰击区域 25, 进入电场或磁场实 现质量分离。 The system of the present invention operates as follows: Primary ions 24 reach the surface of the metal plate 23 along the path 21, It is bombarded on the metal plate 23 with a certain amount of energy. Since the gas sample 26 is generally composed of a non-metal element, the primary ions 24 may be cerium ions or gallium ions or the like, which are liable to ionize non-metal elements. The gas sample 26 to be analyzed is transported through a gas introduction conduit 28 to a surface area 25 of the metal sheet 23 (i.e., the bombardment area 25). The flow rate of the gas sample 26 entering the sample chamber 32 can be controlled by adjusting the valve 33 outside the sample chamber 32. Preferably, the gas sample 26 can be any non-corrosive gas (oxygen, nitrogen or carbon dioxide, etc.). At the bombardment region 25, the primary ions 24 bombard the gas sample 26 to ionize it, thereby converting into secondary ions 27. Due to the electric field between the extraction pole 22 and the metal plate 23, the secondary ions 27 fly away from the bombardment region 25 along the path 29 by the electric field, and enter the electric field or the magnetic field to achieve mass separation.
所述二次离子质谱仪可以采用磁式质谱仪,也可以采用飞行时间质谱仪或四 极杆质谱仪。本发明的系统能够使用二次离子质谱仪对气体样品进行定性定量分 析, 拓展了其应用领域。 实施例 3  The secondary ion mass spectrometer may be a magnetic mass spectrometer or a time-of-flight mass spectrometer or a quadrupole mass spectrometer. The system of the present invention is capable of qualitative and quantitative analysis of gas samples using a secondary ion mass spectrometer, expanding its field of application. Example 3
本发明实施例 2提供了一种使用二次离子质谱仪分析气体样品的方法,包括 采用引出极、金属板和气体引入导管;所述引出极和所述金属板位于所述二次离 子质谱仪的样品室内,所述引出极上设有用于通过一次离子的第一通孔、用于通 过二次离子的第二通孔、以及用于穿过所述气体引入导管的第三通孔,包括以下 步骤:  Embodiment 2 of the present invention provides a method for analyzing a gas sample using a secondary ion mass spectrometer, comprising: using an extraction pole, a metal plate, and a gas introduction conduit; the extraction electrode and the metal plate are located in the secondary ion mass spectrometer a sample chamber having a first through hole for passing primary ions, a second through hole for passing secondary ions, and a third through hole for passing through the gas introduction conduit, including The following steps:
步骤 1, 将所述气体引入导管穿过所述第三通孔, 使用所述气体引入导管将 所述气体样品引导至所述金属板的表面;  Step 1, passing the gas introduction conduit through the third through hole, and guiding the gas sample to a surface of the metal plate using the gas introduction conduit;
步骤 2,采用所述一次离子对引导至所述金属板表面的所述气体样品进行轰 击, 形成所述二次离子;  Step 2, using the primary ion pair to bombard the gas sample guided to the surface of the metal plate to form the secondary ion;
步骤 3, 在所述引出极和所述金属板之间形成电场, 使所述二次离子通过所 述第二通孔飞离所述金属板进入所述二次离子质谱仪进行质量分析。  Step 3, an electric field is formed between the extraction pole and the metal plate, and the secondary ions are passed through the metal plate through the second through hole to enter the secondary ion mass spectrometer for mass analysis.
步骤 3具体包括: 将所述引出极接地电位 30, 将所述金属板接负电压使得 所述二次离子被推斥进入所述二次离子质谱仪进行质量分析,其中所述二次离子 为负离子。  Step 3 specifically includes: placing the extraction pole ground potential 30, connecting the metal plate to a negative voltage such that the secondary ions are repulsed into the secondary ion mass spectrometer for mass analysis, wherein the secondary ions are Negative ions.
步骤 1具体包括:将所述气体样品被引导至所述金属板表面的一定区域;步 骤 2具体包括:使用所述一次离子轰击该区域使得该区域附近的所述气体样品离 子化而生成所述二次离子。 Step 1 specifically includes: guiding the gas sample to a certain area of the surface of the metal plate; The step 2 specifically includes bombarding the region with the primary ions such that the gas sample in the vicinity of the region is ionized to generate the secondary ions.
步骤 1之前还包括将所述样品室抽真空;步骤 3中所述引出极和所述金属板 之间保持一定距离,所述电场为均匀电场。所述距离为 5毫米左右,所述金属板 的表面光滑平整; 所述金属板内不含所述气体样品所包含的元素。  Before the step 1, the sample chamber is further evacuated; in the step 3, the extraction pole and the metal plate are kept at a certain distance, and the electric field is a uniform electric field. The distance is about 5 mm, and the surface of the metal plate is smooth and flat; the metal plate does not contain elements contained in the gas sample.
该方法中所述引出极上的第二通孔位于所述引出极的中央形成中心孔,所述 第一通孔和第三通孔对称分布在所述第二通孔的两侧。 所述引出极的厚度约 2 毫米, 材质为包括无磁不锈钢的金属材质;所述第一通孔、 第二通孔、 第三通孔 直径约 2毫米; 所述金属板的材质包括纯的金或铟或钨金属材料。  In the method, the second through hole on the extraction pole is located at a center of the extraction pole to form a central hole, and the first through hole and the third through hole are symmetrically distributed on both sides of the second through hole. The lead electrode has a thickness of about 2 mm and is made of a metal material including non-magnetic stainless steel; the first through hole, the second through hole, and the third through hole have a diameter of about 2 mm; and the material of the metal plate includes pure Gold or indium or tungsten metal materials.
步骤 1 中还包括使用所述气体引入导管包括的阀门来调节所述气体样品进 入所述样品室的流量;所述气体引入导管选用金属材质制成的细管,该金属材质 包括无磁不锈钢。  The step 1 further includes using a valve included in the gas introduction conduit to adjust a flow rate of the gas sample into the sample chamber; the gas introduction conduit is a thin tube made of a metal material including a non-magnetic stainless steel.
步骤 1中所述气体引入导管接电位,所述气体引入导管将所述气体样品从所 述样品室外引入所述样品室内,所述气体引入导管的末端与所述引出极齐平,所 述气体引入导管内径约 0.5毫米, 外径约 1毫米。  The gas introduction conduit is connected to a potential in step 1, the gas introduction conduit introducing the gas sample from the sample chamber into the sample chamber, the end of the gas introduction conduit being flush with the extraction pole, the gas The introduction catheter has an inner diameter of about 0.5 mm and an outer diameter of about 1 mm.
该方法中所述一次离子包括铯离子或镓离子;所述气体样品为无强烈腐蚀性 的气体,包括氧气, 氮气或二氧化碳;所述二次离子质谱仪包括磁式质谱仪、 飞 行时间质谱仪或四极杆质谱仪;步骤 3中所述二次离子进入所述二次离子质谱仪 的电场和 /或磁场进行质量分析。  In the method, the primary ion comprises a cesium ion or a gallium ion; the gas sample is a non-corrosive gas, including oxygen, nitrogen or carbon dioxide; and the secondary ion mass spectrometer comprises a magnetic mass spectrometer, a time-of-flight mass spectrometer Or a quadrupole mass spectrometer; the secondary ions in step 3 enter the electric field and/or magnetic field of the secondary ion mass spectrometer for mass analysis.
实施例 4 Example 4
与实施例 3相似, 本发明实施例 4中采用的方法包括以下步骤:  Similar to Embodiment 3, the method used in Embodiment 4 of the present invention includes the following steps:
步骤 1、 将金属板放置在二次离子质谱仪的样品室内用于一般分析固体样品 的位置, 将样品室抽真空, 并将金属板加负电压 31 ;  Step 1. Place the metal plate in the sample chamber of the secondary ion mass spectrometer for general analysis of the position of the solid sample, evacuate the sample chamber, and add a negative voltage to the metal plate 31;
步骤 2、 将气体样品通过气体引入导管引入样品室内; 气体引入导管可为金 属不锈钢材料制成, 内径 0.5毫米左右, 外径 1毫米左右; 气体引入导管的出口 距离金属板表面 5毫米左右; 气体引入导管接地电位;  Step 2: introducing a gas sample into the sample chamber through a gas introduction conduit; the gas introduction conduit may be made of a metal stainless steel material having an inner diameter of about 0.5 mm and an outer diameter of about 1 mm; and the outlet of the gas introduction conduit is about 5 mm from the surface of the metal plate; Introducing a conduit ground potential;
步骤 3、 使用一次离子轰击金属板, 将金属板附近的气体样品 (例如气体分 子) 离子化, 使其变为负离子 (也即二次离子); Step 3. Using a single ion bombardment of the metal plate, the gas sample near the metal plate (for example, gas) Ionized, causing it to become a negative ion (ie, a secondary ion);
步骤 4、 负离子 (也即二次离子) 被送入二次离子质谱仪中, 采用二次离子 质谱仪的电场和磁场根据质量进行定性定量分析。  Step 4. The negative ions (ie, secondary ions) are sent to the secondary ion mass spectrometer, and the electric field and the magnetic field of the secondary ion mass spectrometer are used for qualitative and quantitative analysis according to the quality.
通过以上的实施方式的描述,本领域的技术人员可以清楚地了解到本发明还 可以通过其他结构来实现,本发明的特征并不局限于上述较佳的实施例。任何熟 悉该项技术的人员在本发明的技术领域内,可轻易想到的变化或修饰,都应涵盖 在本发明的专利保护范围之内。  From the above description of the embodiments, those skilled in the art can clearly understand that the present invention can be implemented by other structures, and the features of the present invention are not limited to the above preferred embodiments. Any changes or modifications that may be readily conceived by those skilled in the art in the field of the invention are intended to be included within the scope of the invention.

Claims

权 利 要 求 书 Claim
1. 一种使用二次离子质谱仪分析气体样品的系统, 其特征在于, 包括: 引 出极、金属板和气体引入导管;所述引出极和所述金属板位于所述二次离子质谱 仪的样品室内,所述引出极上设有用于通过一次离子的第一通孔、用于通过二次 离子的第二通孔、以及用于穿过所述气体引入导管的第三通孔;所述气体引入导 管穿过所述第三通孔后将所述气体样品引导至所述金属板的表面,所述气体样品 在所述一次离子的轰击下形成所述二次离子;所述弓 [出极和所述金属板之间形成 电场,以使所述二次离子通过所述第二通孔飞离所述金属板进入所述二次离子质 谱仪进行质量分析。 A system for analyzing a gas sample using a secondary ion mass spectrometer, comprising: an extraction electrode, a metal plate, and a gas introduction conduit; the extraction electrode and the metal plate being located in the secondary ion mass spectrometer a sample chamber having a first through hole for passing primary ions, a second through hole for passing secondary ions, and a third through hole for passing through the gas introduction conduit; Passing a gas sample through the third through hole to guide the gas sample to a surface of the metal plate, the gas sample forming the secondary ion under bombardment of the primary ion; the bow An electric field is formed between the pole and the metal plate to cause the secondary ions to fly away from the metal plate through the second through hole into the secondary ion mass spectrometer for mass analysis.
2. 如权利要求 1所述的系统, 其特征在于, 所述引出极接地电位, 所述二 次离子为负离子,所述金属板接负电压使得所述二次离子被推斥进入所述二次离 子质谱仪进行质量分析。  2. The system according to claim 1, wherein: the extraction pole is grounded, the secondary ion is a negative ion, and the metal plate is connected to a negative voltage such that the secondary ion is repulsed into the second Mass spectrometry was performed on a mass spectrometer.
3. 如权利要求 1或 2所述的系统, 其特征在于, 所述气体样品被引导至所 述金属板表面的一定区域,所述一次离子轰击该区域使得该区域附近的所述气体 样品离子化而生成所述二次离子。  3. The system according to claim 1 or 2, wherein the gas sample is directed to a certain area of the surface of the metal plate, the primary ion bombards the area such that the gas sample ions in the vicinity of the area The secondary ions are generated.
4. 如权利要求 1或 2所述的系统, 其特征在于, 所述引出极和所述金属板 之间保持一定距离,所述样品室处于真空状态;所述电场为均匀电场;所述距离 为 5毫米左右,所述金属板的表面光滑平整;所述金属板内不含所述气体样品所 包含的元素。  The system according to claim 1 or 2, wherein a distance is maintained between the extraction pole and the metal plate, the sample chamber is in a vacuum state; the electric field is a uniform electric field; The surface of the metal plate is smooth and flat about 5 mm; the metal plate does not contain elements contained in the gas sample.
5. 如权利要求 1或 2所述的系统, 其特征在于, 所述引出极上的第二通孔 位于所述引出极的中央形成中心孔,所述第一通孔和第三通孔对称分布在所述第 二通孔的两侧;所述弓 [出极的厚度约 2毫米,材质为包括无磁不锈钢的金属材质; 所述第一通孔、第二通孔、第三通孔直径约 2毫米;所述金属板的材质包括纯的 金或铟或钨金属材料。  The system according to claim 1 or 2, wherein the second through hole on the extraction pole is located at a center of the extraction pole to form a central hole, and the first through hole and the third through hole are symmetric Disposed on both sides of the second through hole; the bow [outer thickness is about 2 mm, and the material is made of a metal material including non-magnetic stainless steel; the first through hole, the second through hole, and the third through hole The diameter is about 2 mm; the material of the metal plate includes pure gold or indium or tungsten metal material.
6. 如权利要求 1或 2所述的系统, 其特征在于, 所述气体引入导管还包括 阀门,用于调节所述气体样品进入所述样品室的流量;所述气体引入导管选用金 属材质制成的细管, 该金属材质包括无磁不锈钢; 所述气体引入导管接地电位, 所述气体引入导管将所述气体样品从所述样品室外引入所述样品室内,所述气体 引入导管的末端与所述引出极齐平, 所述气体引入导管内径约 0.5毫米, 外径约 1毫米。 6. The system according to claim 1 or 2, wherein the gas introduction conduit further comprises a valve for regulating a flow rate of the gas sample into the sample chamber; the gas introduction conduit is made of a metal material. a thin tube, the metal material comprising a non-magnetic stainless steel; the gas introduction conduit ground potential, the gas introduction conduit introducing the gas sample from the sample chamber into the sample chamber, the end of the gas introduction conduit The extraction is extremely flush, and the gas introduction conduit has an inner diameter of about 0.5 mm and an outer diameter of about 1 mm.
7. 如权利要求 1或 2所述的系统, 其特征在于, 所述一次离子包括铯离子 或镓离子; 所述气体样品为无强烈腐蚀性的气体, 包括氧气, 氮气或二氧化碳; 所述二次离子质谱仪包括磁式质谱仪、飞行时间质谱仪或四极杆质谱仪;所述二 次离子进入所述二次离子质谱仪的电场和 /或磁场进行质量分析。 7. The system according to claim 1 or 2, wherein the primary ions comprise helium ions or gallium ions; the gas sample is a non-corrosive gas, including oxygen, nitrogen or carbon dioxide; The secondary ion mass spectrometer comprises a magnetic mass spectrometer, a time-of-flight mass spectrometer or a quadrupole mass spectrometer; the secondary ions enter an electric field and/or a magnetic field of the secondary ion mass spectrometer for mass analysis.
8. 一种使用二次离子质谱仪分析气体样品的方法, 包括采用引出极、 金属 板和气体引入导管;所述弓 [出极和所述金属板位于所述二次离子质谱仪的样品室 内,所述引出极上设有用于通过一次离子的第一通孔、用于通过二次离子的第二 通孔、以及用于穿过所述气体引入导管的第三通孔,其特征在于,包括以下步骤: 步骤 1, 将所述气体引入导管穿过所述第三通孔, 使用所述气体引入导管将 所述气体样品引导至所述金属板的表面;  8. A method of analyzing a gas sample using a secondary ion mass spectrometer, comprising: using an extraction pole, a metal plate, and a gas introduction conduit; the bow [outlet and the metal plate are located in a sample chamber of the secondary ion mass spectrometer a first through hole for passing ions, a second through hole for passing secondary ions, and a third through hole for passing through the gas introduction duct, wherein the extraction pole is provided, The method includes the following steps: Step 1: passing the gas introduction conduit through the third through hole, and guiding the gas sample to a surface of the metal plate using the gas introduction conduit;
步骤 2,采用所述一次离子对引导至所述金属板表面的所述气体样品进行轰 击, 形成所述二次离子;  Step 2, using the primary ion pair to bombard the gas sample guided to the surface of the metal plate to form the secondary ion;
步骤 3, 在所述引出极和所述金属板之间形成电场, 使所述二次离子通过所 述第二通孔飞离所述金属板进入所述二次离子质谱仪进行质量分析。  Step 3, an electric field is formed between the extraction pole and the metal plate, and the secondary ions are passed through the metal plate through the second through hole to enter the secondary ion mass spectrometer for mass analysis.
9. 如权利要求 8所述的方法, 其特征在于, 步骤 3具体包括: 将所述引出 极接地电位,将所述金属板接负电压使得所述二次离子被推斥进入所述二次离子 质谱仪进行质量分析,其中所述二次离子为负离子;步骤 1具体包括:将所述气 体样品被引导至所述金属板表面的一定区域;步骤 2具体包括:使用所述一次离 子轰击该区域使得该区域附近的所述气体样品离子化而生成所述二次离子。  9. The method according to claim 8, wherein the step 3 comprises: grounding the extraction pole to a ground potential, and connecting the metal plate to a negative voltage such that the secondary ion is repulsed into the second Mass spectrometer performs mass analysis, wherein the secondary ion is a negative ion; step 1 specifically includes: directing the gas sample to a certain area of the surface of the metal plate; step 2 specifically includes: bombarding the primary ion using the primary ion The region ionizes the gas sample in the vicinity of the region to generate the secondary ions.
10. 如权利要求 8或 9所述的方法, 其特征在于, 步骤 1之前还包括将所述 样品室抽真空;步骤 3中所述引出极和所述金属板之间保持一定距离,所述电场 为均匀电场;所述距离为 5毫米左右,所述金属板的表面光滑平整;所述金属板 内不含所述气体样品所包含的元素。  10. The method according to claim 8 or 9, wherein the step 1 further comprises: evacuating the sample chamber; and maintaining a distance between the extraction pole and the metal plate in step 3, The electric field is a uniform electric field; the distance is about 5 mm, and the surface of the metal plate is smooth and flat; the metal plate does not contain elements contained in the gas sample.
PCT/CN2013/089380 2013-12-13 2013-12-13 System and method for analyzing gas sample using secondary ion mass spectrometer WO2015085577A1 (en)

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