CN107910241B - Mass spectrum analysis device for plasma plume microparticle components in laser welding - Google Patents
Mass spectrum analysis device for plasma plume microparticle components in laser welding Download PDFInfo
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- CN107910241B CN107910241B CN201711120072.XA CN201711120072A CN107910241B CN 107910241 B CN107910241 B CN 107910241B CN 201711120072 A CN201711120072 A CN 201711120072A CN 107910241 B CN107910241 B CN 107910241B
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- ion
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- sampling
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- 238000003466 welding Methods 0.000 title claims abstract description 29
- 239000011859 microparticle Substances 0.000 title claims abstract description 24
- 238000001819 mass spectrum Methods 0.000 title description 3
- 238000005070 sampling Methods 0.000 claims abstract description 58
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 238000000605 extraction Methods 0.000 claims abstract description 20
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 230000001133 acceleration Effects 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 12
- 230000003595 spectral effect Effects 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 description 52
- 238000009434 installation Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001269 time-of-flight mass spectrometry Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000451 chemical ionisation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 210000003746 feather Anatomy 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000000752 ionisation method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0409—Sample holders or containers
- H01J49/0418—Sample holders or containers for laser desorption, e.g. matrix-assisted laser desorption/ionisation [MALDI] plates or surface enhanced laser desorption/ionisation [SELDI] plates
Landscapes
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Electron Tubes For Measurement (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a mass spectrometry device for plasma plume microparticle components in laser welding, and belongs to the technical field of mass spectrometry. Including corpuscle sample cell and vacuum chamber body system, corpuscle sample cell includes, sample awl, intercepting awl and the collimation awl of coaxial setting, sample awl, intercepting awl and collimation awl separate vacuum chamber system for sampling chamber in proper order, intercepting chamber and ionization sampling chamber, cooling system and mechanical vacuum pump are connected to the sampling chamber, vacuum pump group A is connected to the intercepting chamber, vacuum pump group B is connected to the ionization sampling chamber, and laser ionization device is located the outdoor side of ionization sampling, ionization sampling chamber inside is equipped with ion extraction system, mass analyzer and ion detector in proper order. The present application aims at the recognition and understanding of the spectral information of the plume generated in the laser welding process, and further accurately and deeply recognizes and judges the components of the micro-particles.
Description
Technical Field
The invention relates to a mass spectrometry device for micro-particle components, belonging to the technical field of mass spectrometry.
Background
The mass spectrometry technology is an important branch of the modern analysis technology field, and has important application in basic scientific research such as physics, chemistry, biotechnology or application frontier fields such as food quality detection, environmental monitoring and many aspects which are closely related to life. The working principle is simple, and the ions are mainly distinguished according to different charge-to-mass ratios of the ions and finally identified as corresponding components. The mass spectrometry can directly analyze ions through a mass analyzer, and neutral particles need to be ionized first and then analyzed by means of external ionization methods, such as electron bombardment, chemical ionization, laser ionization and the like.
High power lasers play a very important role in the modern manufacturing industry, and one of the most important branches is to use high power lasers for welding between homogeneous or heterogeneous materials, such as metals or alloys. Meanwhile, laser welding has been proven to have many advantages such as high precision, high quality, high efficiency, high flexibility, etc., and is increasingly widely used. In the laser welding process, due to the fact that huge energy acts on the material interface instantaneously, a plume consisting of different components is formed on the surface of the welding interface, and the main components of the plume comprise ions, electrons and neutral atoms or molecules. Since the existence of such a plume greatly suppresses the welding efficiency and affects the welding quality, it is necessary to understand the detailed information and state of the plume deeply and develop a reliable method for suppressing the plume, so that a fundamental method can be developed to suppress the generation of the plume and improve the welding quality. However, the current method for studying the characteristics of the plume is a spectral method, although the method can obtain information about some components in the plume and quantum states where the components are resolved. However, the detailed structure of the ions inside the plume cannot be accurately determined, which greatly limits the understanding of the overall characteristics of the plume.
Therefore, how to accurately and deeply recognize and judge the components of the particles of the laser welding plume in the earlier recognition and understanding of the spectral information of the plume generated in the laser welding process is a problem to be solved urgently in the field.
Disclosure of Invention
In order to solve the problems of the prior art, an object of the present invention is to provide a mass spectrometer for analyzing the components of plasma plume microparticles in laser welding, which can grasp the detailed structure of the plume microparticles as a whole.
The technical scheme of the invention is as follows: the utility model provides a mass spectrometry device of plasma feather corpuscle composition in laser welding, includes corpuscle sampling unit and vacuum cavity system, corpuscle sampling unit includes, sample awl, intercepting awl and the collimation awl of coaxial setting, sample awl, intercepting awl and collimation awl are separated vacuum cavity system for sampling chamber in proper order, intercepting room and ionization sampling chamber, cooling system and mechanical vacuum pump are connected to the sampling chamber, vacuum pump package A is connected to the intercepting room, vacuum pump package B is connected to the ionization sampling chamber, and laser ionization device is located ionization sampling chamber outside, ionization sampling chamber inside is equipped with ion extraction system, mass analyzer and ion detector in proper order.
The cooling system is a liquid nitrogen cooling system or a low-temperature circulating water circulation cooling system and is used for cooling the sampling cone.
The size of the opening at the top of the sampling cone, the intercepting cone and the collimating cone is 0.1-1mm, the angle of the outer side of the cone body is 5-179 degrees, the angle of the inner side of the cone body is 5-178 degrees, and the material is stainless steel, copper or nickel.
The working vacuum degree of the sampling chamber is less than 1000Pa, and the pumping speed of the mechanical vacuum pump is more than 1L/s.
The laser ionization device is a nanosecond laser ionization device or a femtosecond laser ionization device.
The ion extraction system comprises an ion extraction electrode, an ion acceleration electrode, an ion focusing electrode and an ion deflection electrode, wherein the voltage applied by the ion extraction electrode and the ion acceleration is direct current high voltage or pulse high voltage, and the direct current high voltage is applied by the ion focusing electrode and the ion deflection electrode.
the opening and the extension direction of the mass analyzer are the same as the flying direction of the micro-particles.
The mass analyzer is a time-of-flight mass spectrometry ion mass analyzer or a quadrupole ion mass analyzer.
The cone top installation distance between the sampling cone and the intercepting cone is 1-20mm, and the cone top installation distance between the collimation cone and the intercepting cone is larger than 1 mm.
The working vacuum degree of the interception chamber is less than 1Pa, and the working vacuum degree of the ionization sampling chamber is less than 0.1 Pa.
The invention has the beneficial effects that: the method comprises the steps that pulse high voltage is applied to the interior of an ion extraction system, ions in the ion extraction system acquire kinetic energy and enter a subsequent field-free flight area, and the kinetic energy of the ions is consistent, the masses of the ions are different, and therefore the acquired speeds of the ions are different; after passing through the field-free flight region, the ions arrive at the ion detection system at different times, so that specific material components and corresponding concentration distribution information thereof can be determined according to specific time and ion count thereof. The present application aims at the recognition and understanding of the spectral information of the plume generated in the laser welding process, and further accurately and deeply recognizes and judges the components of the micro-particles.
Drawings
FIG. 1 is a schematic diagram of the present invention.
The reference numbers in the figures are as follows: 1. a sampling chamber; 1a, a sampling cone; 1b, a cooling system; 1c, a mechanical vacuum pump; 2. an intercepting chamber; 2a, intercepting a cone; 2b, a vacuum pump group A; 3. an ionization sampling chamber; 3a, a collimation cone; 3b, an ion extraction system; 3c, an ion detector; 3d, a vacuum pump group B; 3e, a mass analyzer; 4. a laser ionization device; 5. a sample to be analyzed; 6. and welding the workpiece by laser.
Detailed Description
The invention is further illustrated with reference to figure 1:
The utility model provides a mass spectrometry device of plasma plume microparticle composition in laser welding, includes microparticle sampling unit and vacuum cavity system, microparticle sampling unit includes, the sample awl 1a, intercepting awl 2a and the collimation awl 3a of coaxial setting, sample awl 1a, intercepting awl 2a and collimation awl 3a separate vacuum cavity system for sampling chamber 1 in proper order, intercepting chamber 2 and ionization sampling chamber 3, cooling system 1B and mechanical vacuum pump 1c are connected to sampling chamber 1, vacuum pump package A2B is connected to intercepting chamber 2, ionization sampling chamber 3 connects vacuum pump package B3d, and laser ionization device 4 is located the ionization sampling chamber 3 outside, ionization sampling chamber 3 inside is equipped with ion extraction system 3B, mass analyzer 3e and ion detector 3c in proper order.
The cooling system 1b is a liquid nitrogen cooling system or a low-temperature circulating water cooling system and is used for cooling the sampling cone 1 a.
The sizes of openings at the tops of the sampling cone 1a, the intercepting cone 2a and the collimating cone 3a are 0.1-1mm, the outer angle of the cone body is 5-179 degrees, the inner angle of the cone body is 5-178 degrees, and the sampling cone, the intercepting cone and the collimating cone are made of stainless steel, copper or nickel.
The working vacuum degree of the sampling chamber 1 is less than 1000Pa, and the pumping speed of the mechanical vacuum pump 1c is more than 1L/s.
The laser ionization device 4 is a nanosecond laser ionization device or a femtosecond laser ionization device.
The ion extraction system 3b includes an ion extraction electrode, an ion acceleration electrode, an ion focusing electrode, and an ion deflection electrode, wherein the voltage applied by the ion extraction electrode and the ion acceleration is a dc high voltage or a pulse high voltage, and the dc high voltage is applied by the ion focusing electrode and the ion deflection electrode.
The opening and the extending direction of the mass analyzer 3e are the same as the flying direction of the fine particles.
The mass analyser 3e is a time of flight mass spectrometry ion mass analyser or a quadrupole ion mass analyser.
The cone top installation distance between the sampling cone 1a and the intercepting cone 2a is 1-20mm, and the cone top installation distance between the collimating cone 3a and the intercepting cone 2a is larger than 1 mm.
The working vacuum degree of the interception chamber 2 is less than 1Pa, and the working vacuum degree of the ionization sampling chamber 3 is less than 0.1 Pa.
Examples
Based on liquid nitrogen cooling, femtosecond laser strong field ionization detection is used as a mass spectrum analysis device of the plume microparticles in the laser welding process by an ionization means. In the embodiment, the diameter of the opening of the sampling cone 1a is 0.5 mm, the cooling system in the sampling cone 1a is connected with the side wall of the sampling cone 1a through a copper wire, and the cooling system 1b is cooled by liquid nitrogen, so that the surface of the sampling cone 1a is not melted at high temperature when high-temperature plume sampling is carried out in the laser welding process. Meanwhile, the vacuum of the sampling chamber 1 is extracted by a vacuum pump with the extraction speed of 4L/s. The diameter of the opening of the skimmer cone 2a connected to the sampling chamber 1 was 0.3 mm, and an 8L/s mechanical pump was used as a backing pump, and a 1200L/s turbo molecular pump was additionally used for vacuum pumping. The vacuum degree which can be obtained in the vacuum can reach 6.0 multiplied by 10-2Pa. The opening of the collimating cone is 0.2 mm, and the ionization sampling chamber 3 is vacuumized by a 8L/s preceding stage mechanical pump combined with a 600L/s turbo molecular pump, thereby ensuring that the vacuum degree is maintained at 1.0 x 10-4Pa, and is beneficial to the subsequent mass spectrometry. After the sample 5 to be analyzed after being sampled is ionized by the femtosecond laser strong field, the ion components enter the field-free flight area of the ionization sampling chamber 3 through the ion extraction system 3 b. The ions in the ion extraction system 3b acquire kinetic energy and enter a subsequent field-free flight region by applying a pulse high voltage to the inside of the ion extraction system, and the ions have the same kinetic energy and different masses therebetween, so that the ions are separatedThe acquired speeds are different. After passing through the field-free flight region, the ions arrive at the ion detector 3c at different times, so that the specific material composition and its corresponding concentration profile information can be determined from its specific time and ion count.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (9)
1. The utility model provides a mass spectrometry device of plasma plume microparticle composition in laser welding which characterized in that, includes microparticle sampling unit and vacuum cavity system, microparticle sampling unit includes, and coaxial setting's sample awl (1 a), intercepting awl (2 a) and collimation awl (3 a), sample awl (1 a), intercepting awl (2 a) and collimation awl (3 a) are separated vacuum cavity system for sampling chamber (1) in proper order, intercepting chamber (2) and ionization sampling chamber (3), cooling system (1B) and mechanical vacuum pump (1 c) are connected in sampling chamber (1), vacuum pump group A (2B) is connected in intercepting chamber (2), ionization sampling chamber (3) are connected vacuum pump group B (3 d), and laser ionization device (4) are located ionization sampling chamber (3) outside, ionization sampling chamber (3) inside is equipped with ion extraction system (3B) in proper order, The mass analyzer (3 e) and the ion detector (3 c), the working vacuum degree of the sampling chamber (1) is less than 1000Pa, the working vacuum degree of the intercepting chamber (2) is less than 1Pa, and the working vacuum degree of the ionization sampling chamber (3) is less than 0.1 Pa.
2. The apparatus for mass spectrometry of plasma plume microparticle composition in laser welding according to claim 1, wherein the cooling system (1 b) is a liquid nitrogen cooling system or a low temperature circulating water cooling system for cooling the sampling cone (1 a).
3. The apparatus for mass spectrometry of the components of plasma plume microparticles in laser welding according to claim 1, wherein the size of the opening at the top of the sampling cone (1 a), the intercepting cone (2 a) and the collimating cone (3 a) is 0.1-1mm, the angle of the outside of the cone is 5-179 degrees, the angle of the inside of the cone is 5-178 degrees, and the material is stainless steel or copper or nickel.
4. The apparatus for mass spectrometry of the components of plasma plumes in laser welding according to claim 1, wherein the pumping speed of the mechanical vacuum pump (1 c) is greater than 1L/s.
5. The mass spectrometer for plasma plume microparticle composition in laser welding according to claim 1, wherein the laser ionizer (4) is a nanosecond laser ionizer or a femtosecond laser ionizer.
6. The apparatus for mass spectrometry of the components of plasma plumes and microparticles in laser welding according to claim 1, wherein the ion extraction system (3 b) includes an ion extraction electrode, an ion acceleration electrode, an ion focusing electrode, and an ion deflection electrode, the voltages applied to the ion extraction electrode and the ion acceleration are dc high voltage or pulsed high voltage, and the dc high voltage is applied to the ion focusing electrode and the ion deflection electrode.
7. The mass spectrometer for plasma plume microparticle components in laser welding according to claim 1, wherein the opening of the mass analyzer (3 e) extends in the same direction as the flight direction of the microparticles.
8. The apparatus for mass spectrometry of plasma plume microparticle composition in laser welding according to claim 1, wherein the mass analyzer (3 e) is a time-of-flight mass spectrometer ion mass analyzer or a quadrupole ion mass analyzer.
9. The apparatus for mass spectrometry of plasma plume microparticle composition in laser welding according to claim 1, wherein the distance between the sampling cone (1 a) and the skimmer cone (2 a) is 1-20mm, and the distance between the collimating cone (3 a) and the skimmer cone (2 a) is greater than 1 mm.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711357993.8A CN108010829B (en) | 2017-11-14 | 2017-11-14 | The mass spectrometer of plumage brightness particulate in a kind of laser welding |
| CN201711120072.XA CN107910241B (en) | 2017-11-14 | 2017-11-14 | Mass spectrum analysis device for plasma plume microparticle components in laser welding |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711120072.XA CN107910241B (en) | 2017-11-14 | 2017-11-14 | Mass spectrum analysis device for plasma plume microparticle components in laser welding |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711357993.8A Division CN108010829B (en) | 2017-11-14 | 2017-11-14 | The mass spectrometer of plumage brightness particulate in a kind of laser welding |
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| Publication Number | Publication Date |
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| CN107910241A CN107910241A (en) | 2018-04-13 |
| CN107910241B true CN107910241B (en) | 2019-12-13 |
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| CN201711120072.XA Expired - Fee Related CN107910241B (en) | 2017-11-14 | 2017-11-14 | Mass spectrum analysis device for plasma plume microparticle components in laser welding |
| CN201711357993.8A Expired - Fee Related CN108010829B (en) | 2017-11-14 | 2017-11-14 | The mass spectrometer of plumage brightness particulate in a kind of laser welding |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201711357993.8A Expired - Fee Related CN108010829B (en) | 2017-11-14 | 2017-11-14 | The mass spectrometer of plumage brightness particulate in a kind of laser welding |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112133165B (en) * | 2020-10-15 | 2024-06-25 | 大连理工大学 | Linear plasma experimental device |
| CN112557488A (en) * | 2020-12-09 | 2021-03-26 | 上海交通大学 | Integrated molecular beam sampling interface |
| CN114005570B (en) * | 2021-10-12 | 2024-04-30 | 浙江大学 | Apparatus and method for selective capture release of charge in vacuum |
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| CN102149509A (en) * | 2008-07-09 | 2011-08-10 | Fei公司 | Method and apparatus for laser machining |
| CN102176045A (en) * | 2011-01-20 | 2011-09-07 | 大连理工大学 | Measurement method for spatial distribution of deuterium or tritium detained on surface of first Tokamak wall |
| CN204464235U (en) * | 2014-12-31 | 2015-07-08 | 聚光科技(杭州)股份有限公司 | A kind of icp ms of adjustable vacuum pressure |
| CN105762055A (en) * | 2014-12-17 | 2016-07-13 | 中国科学院大连化学物理研究所 | Mass spectrum device for research of plasma-micromolecule system reaction |
| CN104637773B (en) * | 2015-02-16 | 2017-03-01 | 江苏天瑞仪器股份有限公司 | Mass spectrograph one-level vacuum structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US8067730B2 (en) * | 2007-07-20 | 2011-11-29 | The George Washington University | Laser ablation electrospray ionization (LAESI) for atmospheric pressure, In vivo, and imaging mass spectrometry |
| GB2498173C (en) * | 2011-12-12 | 2018-06-27 | Thermo Fisher Scient Bremen Gmbh | Mass spectrometer vacuum interface method and apparatus |
| EP2988316B1 (en) * | 2013-04-19 | 2020-10-14 | Shimadzu Corporation | Mass spectrometer |
| KR20150052898A (en) * | 2013-11-06 | 2015-05-15 | 연세대학교 산학협력단 | Sample plate using MALDI-TOF mass spectrometer and manufacturing method of the sample plate |
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2017
- 2017-11-14 CN CN201711120072.XA patent/CN107910241B/en not_active Expired - Fee Related
- 2017-11-14 CN CN201711357993.8A patent/CN108010829B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102149509A (en) * | 2008-07-09 | 2011-08-10 | Fei公司 | Method and apparatus for laser machining |
| CN102176045A (en) * | 2011-01-20 | 2011-09-07 | 大连理工大学 | Measurement method for spatial distribution of deuterium or tritium detained on surface of first Tokamak wall |
| CN105762055A (en) * | 2014-12-17 | 2016-07-13 | 中国科学院大连化学物理研究所 | Mass spectrum device for research of plasma-micromolecule system reaction |
| CN204464235U (en) * | 2014-12-31 | 2015-07-08 | 聚光科技(杭州)股份有限公司 | A kind of icp ms of adjustable vacuum pressure |
| CN104637773B (en) * | 2015-02-16 | 2017-03-01 | 江苏天瑞仪器股份有限公司 | Mass spectrograph one-level vacuum structure |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107910241A (en) | 2018-04-13 |
| CN108010829B (en) | 2019-12-03 |
| CN108010829A (en) | 2018-05-08 |
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