CN105572216A - Novel flight time secondary ion mass spectrometer - Google Patents
Novel flight time secondary ion mass spectrometer Download PDFInfo
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- CN105572216A CN105572216A CN201511017099.7A CN201511017099A CN105572216A CN 105572216 A CN105572216 A CN 105572216A CN 201511017099 A CN201511017099 A CN 201511017099A CN 105572216 A CN105572216 A CN 105572216A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/64—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
Abstract
The invention discloses a novel flight time secondary ion mass spectrometer. The structure of the novel flight time secondary ion mass spectrometer comprises a sample carriage, a primary ion source, a femtosecond laser device, an ion extraction system, a flight time ion mass analyzer and a signal generator. The novel flight time secondary ion mass spectrometer is a sensitive and efficient surface analysis device, and the device allows qualitative and quantitative analysis results of material components to be rapidly and accurately obtained. A femtosecond laser strong field off-resonance ionization technology is adopted to detect neutral particles, and the laser power can be controlled to simultaneously generate univalent and multivalent ions of a same element to provide a natural internal standard source for mass scaling of elements to be analyzed, so the mass of the elements to be analyzed can be accurately determined.
Description
Technical field:
The present invention relates to secondary ion mass spectrum (SecondaryIonMassSpectrometry, SIMS) analysis field.More specifically, the present invention relates to the novel time of flight secondary ion massspectrometry of one introducing ionization technique after femtosecond laser, thus higher sensitivity and resolution can be obtained in analytic process.
Background technology:
Secondary ion mass spectrum technology the high energy ion beam focused on is injected the surface of solid sample, make it to produce corresponding plasma sputter (secondary ion), by carrying out the quality of above-mentioned plasma sputter analyzing the component information can known in this solid sample, the particularly important is the compositional information that the method can obtain trace element.Therefore, secondary ion mass spectrum all has important application in fields such as microelectronics, material science, geology and life sciences.But secondary ion mass spectrum technology also also exists many weak points, the sputtering yield between the low and different element ion composition of wherein secondary ion productive rate seriously makes secondary ion mass spectrum be restricted in quantitative test by matrix effect.Meanwhile, it is pointed out that in the sputtering main part produced with secondary ion simultaneously, the secondary neutral particle namely produced by ion beam sputtering, the ratio distribution of its composition but shows distribution proportion very consistent between composition corresponding to sample.Therefore, sputtered neutral product is analyzed and obtains its corresponding concentration information, then for the sample analysis of secondary ion mass spectrum realizes quantitative test lay a good foundation from qualitative.
In many ionization means, because the stable of laser ionization and ease for use make laser ionization mode once once be paid close attention to widely as the ionization means of sputtered neutral particle.But above-mentioned traditional laser ionization means are but because lower ionizing efficiency makes it be restricted in the rear ionization application of secondary ion mass spectrum.Even main manifestations for cannot surmount secondary ion mass spectrum from sensitivity in performance.And an important development direction thereafter how to realize secondary neutral particle effectively ionized to as sputtering main component.
For the mass analyzer that secondary ion mass spectrum adopts, wherein magnetic substance spectrum is eliminated gradually because of its complex structure and expensive cost, mainly adopt level Four bar mass spectrum in the equipment of current main flow, mainly consider that its structure is simple, cost is lower and the reason such as easy to operate.But for comparatively rare and some samples of trace, the employing of quality analysis means more efficiently just becomes and is even more important.This wherein, time of flight ion mass analyzer because of its higher quality analysis efficiency, wider mass measurement scope and become secondary ion mass spectrum quality analysis aspect development an important trend.
Summary of the invention
The present invention's fact is in view of the above made, and its object is to provides a kind of novel time of flight secondary ion massspectrometry;
For achieving the above object, the technical solution adopted in the present invention is as described below:
A kind of novel time of flight secondary ion massspectrometry, its structure comprises sample carrier 1, primary ion source 2, femto-second laser 3, ion extraction system 4, time of flight ion mass analyzer 5 and the signal generator 6 that order is from left to right arranged;
Testing sample can be fixed among vacuum chamber by described sample analog bracket 1, and is realized the top to bottom, left and right, front and rear of testing sample and the adjustment of slight inclination angle by external control circuit;
Described primary ion source 2 can produce the focused ion beam that the positive ion of high-energy focusing, negative ion or negative ions coexist, and its beam spot diameter, is 20 nanometers to 200 micron, and energy is 5 keV to 50 keVs; Under described primary ion source 2 can be operated in continuous and pulse two kinds of mode of operations, and the ion beam pulses width produced time under pulse working mode was 5 nanoseconds nanosecond to 500;
It is 5-1000 hertz that described femto-second laser 3 can produce frequency, and single pulse energy is 0.5-30 millijoule, and pulse width is 8-500 femtosecond, and centre wavelength is in 800 nanometers, and spectral width is the femtosecond pulse of 30-70 nanometer;
On the offspring envelope that the femtosecond laser that described femto-second laser 3 produces produces focus on the sputtering of described primary ion source 2 after lens 3a after, and by carrying out to lens 3a the maximization that three-dimensional translating regulating and controlling realizes femtosecond laser ionizing efficiency;
Two plate electrodes that described ion extraction system 4 is arranged for parallel coaxial, two plate electrodes apply DC voltage according to certain ratio respectively; A plate electrode wherein near sample direction is plane electrode, and another plate electrode away from sample is tapered electrode, and tapered electrode is ground connection setting;
Described time of flight ion mass analyzer 5 can be orthoscopic or reflection time-of-flight mass, and resolution is 5000 to 25000 in the resolution that described primary ion source 2 works in the pulsing mode;
Described signal generator 6 is used for the relative delay of the ion detector controlling described primary ion source 2, femto-second laser 3 and time of flight ion mass analyzer 5, and the representative value of the relative delay between the primary ion source 2 that described signal generator 6 controls and femto-second laser 3 is a certain time delay between 2.5 microsecond to 10 microseconds of femto-second laser 3 after primary ion source 2 triggers.Thus realize maximum instrumental sensitivity.
Owing to adopting technique scheme, the novel time of flight secondary ion massspectrometry of one provided by the invention, compared with prior art has such beneficial effect:
Femtosecond laser and secondary ion mass spectrum combine by the present invention, for detecting the neutral particle composition that ion sputtering produces.Femtosecond laser has very high peak power, nearly all element can be realized ionization by simple venation flushing, to the full dimension analysis of components of target surface, realize the efficiency utilization of sputtering particle and then the sensitivity of instrument can be improved to a great extent, the improvement of the performance parameters such as follow-up resolution is had great importance.
Femtosecond laser and time of flight mass analyzer combine by the present invention, compare to traditional secondary ion massspectrum, can realize more efficient sputtering particle utilization ratio, and the ion produced in this process is more weak by the impact of sample matrices effect; Ion analysis efficiency can be increased substantially.Therefore, novel time of flight secondary ion massspectrometry provided by the present invention is the sensitiveer and efficient surface analysis apparatus of one, and this device can obtain rapidly result accurately on the qualitative and quantitative analysis of material composition.
The present invention adopts femtosecond laser high field off-resonance ionization technique to detect neutral particle, by the control to laser power, unit price state and the multivalent state ion of same element can be produced simultaneously, for element to be analyzed quality calibration provide natural in mark source, the quality of element to be analyzed can be determined exactly.
The present invention adopts femtosecond laser high field off-resonance ionization technique to detect neutral particle, basically identical to the ionizing efficiency of isotopic element, and therefore this technology has unique advantage in isotopic abundance analysis.
Accompanying drawing explanation
The principle schematic of Fig. 1 embodiment of the present invention;
Fig. 2 embodiment of the present invention tests the secondary neutral particle mass spectrum of the silver-colored sample obtained.
Wherein, in the device shown in Fig. 1,1-sample carrier; 2-primary ion source; 3-femto-second laser; 3a-lens; 4-ion extraction system; 5-time of flight ion mass analyzer; 6-signal generator.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail:
A kind of novel time of flight secondary ion massspectrometry, as shown in Figure 1, its structure comprises sample carrier 1, primary ion source 2, femto-second laser 3, ion extraction system 4, time of flight ion mass analyzer 5 and the signal generator 6 that order is from left to right arranged;
Testing sample can be fixed among vacuum chamber by described sample carrier 1, and is realized the top to bottom, left and right, front and rear of testing sample and the adjustment of slight inclination angle by external control circuit; Described sample carrier 1 the testing sample surface fixed for through metal coating process and conductive sample.
Described primary ion source 2 can produce the focused ion beam that the positive ion of high-energy focusing, negative ion or negative ions coexist, and its beam spot diameter, is 20 nanometers to 200 micron, and energy is 5 keV to 50 keVs; Under described primary ion source 2 can be operated in continuous and pulse two kinds of mode of operations, and the ion beam pulses width produced time under pulse working mode was 5 nanoseconds nanosecond to 500;
It is 5-1000 hertz that described femto-second laser 3 can produce frequency, and single pulse energy is 0.5-30 millijoule, and pulse width is 8-500 femtosecond, and centre wavelength is in 800 nanometers, and spectral width is the femtosecond pulse of 30-70 nanometer;
On the offspring envelope that the femtosecond laser that described femto-second laser 3 produces produces focus on the sputtering of described primary ion source 2 after lens 3a after, and by carrying out to lens 3a the maximization that three-dimensional translating regulating and controlling realizes femtosecond laser ionizing efficiency;
Two plate electrodes that described ion extraction system 4 is arranged for parallel coaxial, two plate electrodes apply DC voltage according to certain ratio respectively; A plate electrode wherein near sample direction is plane electrode, and another plate electrode away from sample is tapered electrode, and tapered electrode is ground connection setting;
Described time of flight ion mass analyzer 5 can be orthoscopic or reflection time-of-flight mass, and resolution is 5000 to 25000 in the resolution that described primary ion source 2 works in the pulsing mode;
Described signal generator 6 is used for the relative delay of the ion detector controlling described primary ion source 2, femto-second laser 3 and time of flight ion mass analyzer 5, the representative value of the relative delay between the primary ion source 2 that described signal generator 6 controls and femto-second laser 3 is a certain time delay between 2.5 microsecond to 10 microseconds of femto-second laser 3 after primary ion source 2 triggers, thus realizes maximum instrumental sensitivity.
Some characteristics that the present invention has and advantage will be described by specific embodiment below.The present invention is the time of flight secondary ion massspectrometry designed in the following manner.
As shown in Figure 1, the novel time of flight secondary ion massspectrometry of one of the present invention mainly comprises sample carrier 1, primary ion source 2, femto-second laser 3, ion extraction system 4, time of flight ion mass analyzer 5, signal generator 6.Wherein, the high-energy focusing ion beam mutation sample surfaces that primary ion source 2 exports, is ionized by the femto-second laser pulse that femto-second laser 3 produces carrying out with sample surfaces the secondary neutral particle composition sputtered in the process of colliding in the offspring of generation.Owing to adopting the neutral particle for occupying offspring overwhelming majority ratio to carry out rear ionization analysis here, primary ion source therefore can be avoided to a great extent to sputter the matrix effect of the secondary ion produced, improve the quantitative test ability of instrument.Meanwhile, adopt femto-second laser 3 to increase substantially the ionizing efficiency of secondary neutral particle as ionization source, and then have greatly improved for the lifting of instrument overall sensitivity.The time of flight ion mass analyzer wide in range in conjunction with high speed has done again further lifting to the analysis efficiency of secondary ion mass spectrum.
Embodiment 1
Ionizing efficiency test after the secondary neutral particle of fine silver target
The gain situation ionizing efficiency that femtosecond laser can produce after rear ionization means being compared to the secondary ion that simple primary ion source bombardment produces that the present embodiment purport is adopted in describing the present invention.O is adopted in the present embodiment
-ion gun is as primary ion source 2.Ionogenic electron gun diameter after focusing is about 5 microns, and energy is 15 keVs, and following experiments is carried out under ionogenic pulse mode.Frequency is 1000 hertz, and pulse width is 200 microseconds.This pulsed ionizing beam sputters the offspring of generation after injecting the sample surfaces of surface gold-plating, then carries out rear ionization via femtosecond laser.The frequency of the femtosecond laser that femto-second laser 3 is launched is 1 KHz, pulse width 35-45 femtosecond, energy 3.6 watts, the offspring envelope position produced in primary ions bombardment via the lens focus of 35 centimetres.Primary ion source 2 and the relative delay of femto-second laser 3 is regulated the neutral particle among offspring to be ionized by femtosecond laser thus realizes the lifting greatly to offspring ionizing efficiency by utilizing signal generator 6.As shown in Figure 2, that femtosecond laser carries out rear ionization relative to primary ion source ion beam mutation 4.6 microsecond, and apply positive 2000 DC voltage at sample surfaces, close sample one termination electrode of ion extraction system applies the flight time mass spectrum that positive 1800V DC voltage extracts.By carrying out area integral contrast to the mass spectra peak of initial ion and rear ionization ion, this ionization technique can make the signal intensity of secondary ion add more than 1000 times.
It will be appreciated by those skilled in the art that embodiment above provides purely in an illustrative manner, and some changes are possible.
Claims (1)
1. a novel time of flight secondary ion massspectrometry, it is characterized in that: a kind of novel time of flight secondary ion massspectrometry, its structure comprises sample carrier (1), primary ion source (2), femto-second laser (3), ion extraction system (4), time of flight ion mass analyzer (5) and the signal generator (6) that order is from left to right arranged;
Testing sample can be fixed among vacuum chamber by described sample carrier (1), and is realized the top to bottom, left and right, front and rear of testing sample and the adjustment of slight inclination angle by external control circuit;
Described primary ion source (2) can produce the focused ion beam that the positive ion of high-energy focusing, negative ion or negative ions coexist, and its beam spot diameter, is 20 nanometers to 200 micron, and energy is 5 keV to 50 keVs; Under described primary ion source (2) can be operated in continuous and pulse two kinds of mode of operations, and the ion beam pulses width produced time under pulse working mode was 5 nanoseconds nanosecond to 500;
It is 5-1000 hertz that described femto-second laser (3) can produce frequency, and single pulse energy is 0.5-30 millijoule, and pulse width is 8-500 femtosecond, and centre wavelength is in 800 nanometers, and spectral width is the femtosecond pulse of 30-70 nanometer;
On the offspring envelope that the femtosecond laser that described femto-second laser (3) produces produces focus on described primary ion source (2) sputtering after lens (3a) after, and by carrying out to condenser lens (3a) maximization that three-dimensional translating regulating and controlling realizes femtosecond laser ionizing efficiency;
Two plate electrodes that described ion extraction system (4) is arranged for parallel coaxial, two plate electrodes apply DC voltage according to certain ratio respectively; A plate electrode wherein near sample direction is plane electrode, and another plate electrode away from sample is tapered electrode, and tapered electrode is ground connection setting;
Described time of flight ion mass analyzer (5) can be orthoscopic or reflection time-of-flight mass, and resolution is 5000 to 25000 in described primary ion source (2) work resolution in the pulsing mode;
Described signal generator (6) is used for the relative delay of the ion detector controlling described primary ion source (2), femto-second laser (3) and time of flight ion mass analyzer (5), the representative value of the relative delay between the primary ion source (2) that described signal generator (6) controls and femto-second laser (3) be femto-second laser (3) be positioned at primary ion source (2) trigger after 2.5 microsecond to 10 microseconds between a certain time delay.
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Cited By (8)
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| CN107219214A (en) * | 2017-07-26 | 2017-09-29 | 大连理工大学 | A kind of spectrum combines the quantitative analysis device of element in mass spectrographic unknown sample |
| CN108169092A (en) * | 2018-03-19 | 2018-06-15 | 南京信息工程大学 | Atmospheric particulates heavy metal and its isotope on-line water flushing devices and methods therefor |
| CN112526585A (en) * | 2020-11-02 | 2021-03-19 | 中国科学院国家空间科学中心 | Detector and detection method for in-situ measurement of track neutral gas particle velocity |
| CN112986303A (en) * | 2021-02-07 | 2021-06-18 | 中国建筑材料科学研究总院有限公司 | Method for detecting secondary electron emission yield on surface of ion-induced material |
| CN113640368A (en) * | 2020-04-27 | 2021-11-12 | 株式会社岛津制作所 | Method for analyzing structure of organic compound |
| CN113678227A (en) * | 2018-06-18 | 2021-11-19 | 富鲁达加拿大公司 | High resolution imaging apparatus and method |
| CN115295395A (en) * | 2022-07-11 | 2022-11-04 | 中国科学院上海技术物理研究所 | Ionization source based on LIBS and SLRI |
| CN115295393A (en) * | 2022-07-11 | 2022-11-04 | 中国科学院上海技术物理研究所 | Laser ionization method for isotope mass spectrometry detection |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107219214A (en) * | 2017-07-26 | 2017-09-29 | 大连理工大学 | A kind of spectrum combines the quantitative analysis device of element in mass spectrographic unknown sample |
| CN107219214B (en) * | 2017-07-26 | 2023-10-27 | 大连理工大学 | Quantitative analysis device for elements in unknown sample by spectrum combination with mass spectrum |
| CN108169092A (en) * | 2018-03-19 | 2018-06-15 | 南京信息工程大学 | Atmospheric particulates heavy metal and its isotope on-line water flushing devices and methods therefor |
| CN108169092B (en) * | 2018-03-19 | 2023-10-27 | 南京信息工程大学 | Online detection device and method for heavy metals and isotopes of atmospheric particulates |
| CN113678227A (en) * | 2018-06-18 | 2021-11-19 | 富鲁达加拿大公司 | High resolution imaging apparatus and method |
| CN113640368A (en) * | 2020-04-27 | 2021-11-12 | 株式会社岛津制作所 | Method for analyzing structure of organic compound |
| CN112526585A (en) * | 2020-11-02 | 2021-03-19 | 中国科学院国家空间科学中心 | Detector and detection method for in-situ measurement of track neutral gas particle velocity |
| CN112986303A (en) * | 2021-02-07 | 2021-06-18 | 中国建筑材料科学研究总院有限公司 | Method for detecting secondary electron emission yield on surface of ion-induced material |
| CN115295395A (en) * | 2022-07-11 | 2022-11-04 | 中国科学院上海技术物理研究所 | Ionization source based on LIBS and SLRI |
| CN115295393A (en) * | 2022-07-11 | 2022-11-04 | 中国科学院上海技术物理研究所 | Laser ionization method for isotope mass spectrometry detection |
| CN115295395B (en) * | 2022-07-11 | 2024-03-22 | 中国科学院上海技术物理研究所 | Ionization source based on LIBS and SLRI |
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Application publication date: 20160511 |