CN108010829B - The mass spectrometer of plumage brightness particulate in a kind of laser welding - Google Patents
The mass spectrometer of plumage brightness particulate in a kind of laser welding Download PDFInfo
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- CN108010829B CN108010829B CN201711357993.8A CN201711357993A CN108010829B CN 108010829 B CN108010829 B CN 108010829B CN 201711357993 A CN201711357993 A CN 201711357993A CN 108010829 B CN108010829 B CN 108010829B
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- 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
Abstract
This divisional application discloses a kind of mass spectrometer of plumage brightness particulate in laser welding, belongs to analytical technique of mass spectrum field.Including particulate sampling unit and vacuum cavity system, the particulate sampling unit includes, the sampling cone of coaxial arrangement, interception cone and collimation cone, the sampling cone, interception cone and collimation, which are bored, is successively divided into sampling room for vacuum cavity system, intercept room and ionization sampler chamber, sampling room's connection cooling system and oil-sealed rotary pump, the interception room connects vacuum pump group A, the ionization sampler chamber connects vacuum pump group B, laser ionization device is located on the outside of ionization sampler chamber, ion extraction system is successively arranged inside the ionization sampler chamber, mass analyzer and ion detector.This divisional application is directed in the understanding and understanding of the spectral information of the plumage brightness generated in laser beam welding, further the understanding and judgement accurate and deep to the ingredient of its particulate.
Description
The application is application number 201711120072X, 14 days November 2017 applying date, a kind of denomination of invention " Laser Welding
Connect the mass spectrometer of plasma plumage brightness particle subconstiuent " divisional application
Technical field
The present invention relates to a kind of mass spectrometers of particle subconstiuent, belong to analytical technique of mass spectrum field.
Background technique
An important branch of the mass-spectrometric technique as modern analytical technique field, in basic scientific research such as physics, chemistry, biology
Technology or application Disciplinary Frontiers such as food quality detection, environmental monitoring etc. have with closely bound up all various aspects of living
Important application.Its working principle is also relatively simple, it is main be exactly by ion according to its between each other different charge-mass ratio come into
Row is distinguished and finally assert its corresponding ingredient.Mass-spectrometric technique can directly analyze ion by mass analyzer,
And neutral particle is then needed by means of extraneous some Ionization modes, such as electron bombardment, chemi-ionization, laser ionization
Etc. means first ionized and analyzed again.
Superpower laser plays in modern manufacturing industry and its important role, and one of them very important point
Branch is exactly that the welding between homogeneities or dissimilar materials such as metal or alloy is carried out using superpower laser.Meanwhile laser
Welding had been proved to it already to be had many advantages, such as high-precision, high quality, high efficiency, high flexibility and is more widely answered
With.And in laser beam welding, since huge energy snap makes it can be in welding junction at material interface
Surface formed one have heterogeneity constitute plumage brightness, the main component of the plumage brightness include ion, electronics and neutral atom or
Person's molecule.And the presence of the plumage brightness can largely inhibit welding efficiency and influence the quality of welding, this is just needed
The detailed configuration information and state of the deep above-mentioned plumage brightness of understanding, and develop reliable plumage brightness suppressing method accordingly, thus
The method of essence can be developed to inhibit the generation of plumage brightness and improve welding quality.But it is used to study plumage brightness at present special
Property often using the method for spectrum, although some ingredients inside the available plumage brightness of this kind of method and its locating for
The information that quantum state is differentiated.But the detailed composition about the ion inside plumage brightness can not but accomplish accurately to judge, this is just
The very big understanding limited to plumage brightness overall permanence.
Therefore, how in understanding and understanding of the early period for the spectral information of the plumage brightness generated in laser beam welding,
The further understanding and judgement accurate and deep to the ingredient of its particulate are that be faced one of the field is urgently to be solved
Problem.
Summary of the invention
To solve defect of the existing technology, the object of the present invention is to provide plumage brightness particulates in a kind of laser welding
Mass spectrometer holds the detailed composition of plumage brightness particulate on the whole.
The technical scheme is that in a kind of laser welding plumage brightness particulate mass spectrometer, including particulate
Sampling unit and vacuum cavity system, the particulate sampling unit include sampling cone, interception cone and the standard of coaxial arrangement
Vacuum cavity system is successively divided into sampling room, intercepts room and ionization by right cone, the sampling cone, interception cone and collimation cone
Sampler chamber, sampling room's connection cooling system and oil-sealed rotary pump, the interception room connect vacuum pump group A, and the ionization is adopted
Specimen chamber connects vacuum pump group B, and laser ionization device is located at ionization sampler chamber outside, be successively arranged inside the ionization sampler chamber from
Sub- extraction system, mass analyzer and ion detector.
The cooling system is that liquid nitrogen cooling system or low temperature follow water ring cooling system, for cooling down sampling cone.
The vertex of a cone bore size of the sampling cone, interception cone and collimation cone is 0.1-1mm, on the outside of centrum angle be 5 °-
179 °, centrum inner angle is 5 ° -178 °, and material is stainless steel or copper or nickel.
The working vacuum degree of the sampling room is less than 1000Pa, and the pumping speed of oil-sealed rotary pump is greater than 1L/s.
The laser ionization device be nanosecond laser ionization device or femtosecond laser ionization device.
The ion extraction system includes that ion extraction electrode, ion acceleration electrode, ion focusing electrode and ion are inclined
Turn electrode, the voltage that the ion extraction electrode and ion acceleration apply is high direct voltage either high voltage pulse, the ion
What focusing electrode and ion deflecting electrode applied is high direct voltage.
The opening and extending direction of the mass analyzer are identical as the heading of particulate.
The mass analyzer is flight time mass spectrum mass of ion analyzer or quadrupole rod mass of ion analyzer.
Vertex of a cone mounting distance between the sampling cone and interception cone is 1-20mm, between the collimation cone and interception cone
Vertex of a cone mounting distance is greater than 1mm.
The vacuum degree of interception room work is less than 1Pa, and the vacuum degree of the ionization sampler chamber work is less than 0.1Pa.
The beneficial effects of the present invention are: the ion for keeping it internal obtains by applying high voltage pulse inside ion extraction system
Take kinetic energy and enter subsequent field-free flight region, due to the kinetic energy of ion therebetween is consistent and different therefore these ions of quality
Acquired speed is different;Ion detection system is reached at the time of a while difference after by field-free flight region, so as to
To determine specific material composition and its corresponding concentration distribution information with Ion Counting according to its specific time.The application needle
It is further accurate to the ingredient of its particulate in the understanding and understanding of the spectral information of the plumage brightness generated in laser beam welding
And deep understanding and judgement.
Detailed description of the invention
Fig. 1 is operation schematic diagram of the present invention.
Appended drawing reference is as follows in figure: 1, sampling room;1a, sampling cone;1b, cooling system;1c, oil-sealed rotary pump;2, it intercepts
Room;2a, interception cone;2b, vacuum pump group A;3, ionization sampler chamber;3a, collimation cone;3b, ion extraction system;3c, ion detection
Device;3d, vacuum pump group B;3e, mass analyzer;4, laser ionization device;5, sample to be analysed;6, laser welding workpiece.
Specific embodiment
1 the present invention will be further described with reference to the accompanying drawing:
The mass spectrometer of plumage brightness particulate in a kind of laser welding, including particulate sampling unit and vacuum cavity
System, the particulate sampling unit include sampling cone 1a, the interception cone 2a and collimation cone 3a of coaxial arrangement, the sampling
Vacuum cavity system is successively divided into sampling room 1 by cone 1a, interception cone 2a and collimation cone 3a, intercepts room 2 and ionization sampling
Room 3, the sampling room 1 connect cooling system 1b and oil-sealed rotary pump 1c, the connection of the interception room 2 vacuum pump group A2b, it is described from
Change sampler chamber 3 and connect vacuum pump group B3d, laser ionization device 4 is located on the outside of ionization sampler chamber 3, inside the ionization sampler chamber 3
It is successively arranged ion extraction system 3b, mass analyzer 3e and ion detector 3c.
The cooling system 1b is that liquid nitrogen cooling system or low temperature follow water ring cooling system, for cooling down sampling cone 1a.
The vertex of a cone bore size of the sampling cone 1a, interception cone 2a and collimation cone 3a are 0.1-1mm, angle on the outside of centrum
It is 5 ° -179 °, centrum inner angle is 5 ° -178 °, and material is stainless steel or copper or nickel.
The working vacuum degree of the sampling room 1 is less than 1000Pa, and the pumping speed of oil-sealed rotary pump 1c is greater than 1L/s.
The laser ionization device 4 be nanosecond laser ionization device or femtosecond laser ionization device.
The ion extraction system 3b includes ion extraction electrode, ion acceleration electrode, ion focusing electrode and ion
Deflecting electrode, the voltage that the ion extraction electrode and ion acceleration apply are high direct voltage either high voltage pulse, it is described from
What sub- focusing electrode and ion deflecting electrode applied is high direct voltage.
The opening and extending direction of the mass analyzer 3e is identical as the heading of particulate.
The mass analyzer 3e is flight time mass spectrum mass of ion analyzer or quadrupole rod mass of ion analyzer.
Vertex of a cone mounting distance between the sampling cone 1a and interception cone 2a is 1-20mm, and the collimation cone 3a and interception are bored
Vertex of a cone mounting distance between 2a is greater than 1mm.
The vacuum degree that the interception room 2 works is less than 1Pa, and the vacuum degree that the ionization sampler chamber 3 works is less than 0.1Pa.
Embodiment
Cooling based on liquid nitrogen, femtosecond laser high field ionization detection is as plumage brightness particulate in ionization means laser beam welding
Mass spectrometer.The opening diameter of sampling cone 1a is 0.5 millimeter in the present embodiment, and sampling cone 1a inner cooling system passes through
The side wall of one copper bar line and sampling cone 1a is connected together, and cooling system 1b then uses liquid nitrogen to be cooled down, therefore this
In may insure the surface of sampling cone 1a when carrying out the sampling of laser beam welding high temperature plumage brightness not by high temperature melt.With
The vacuum of this while sampling room 1 then uses the extraction of the vacuum pump progress vacuum of a 4L/s pumping speed.What is be connected with sampling room 1 cuts
The opening diameter for taking cone 2a is 0.3 millimeter, makees fore pump using the mechanical pump of a 8L/s, and in addition adds a 1200L/s's
The extraction of turbomolecular pump progress vacuum.The vacuum degree that can be obtained in this grade of vacuum can achieve 6.0 × 10-2Pa.Collimation
The aperture of cone is 0.2 millimeter, ionization sampler chamber 3 by the turbomolecular pump of the prime mechanical pump combination 600L/s of a 8L/s into
The extraction of row vacuum, to guarantee that its vacuum degree maintains 1.0 × 10-4Within Pa, and it is conducive to subsequent mass spectral analysis.In quilt
After the ionization of femtosecond laser high field, ion component will enter sample to be analysed 5 after sampling via ion extraction system 3b
The field-free flight region of ionization sampler chamber 3.By applying high voltage pulse inside ion extraction system 3b, the ion for keeping it internal is obtained
Take kinetic energy and enter subsequent field-free flight region, since the kinetic energy of ion therebetween is consistent and quality is different, these from
Speed acquired in son is different.By ion detector 3c can be reached in different at the time of after field-free flight region, thus
Specific material composition and its corresponding concentration distribution information can be determined according to its specific time with Ion Counting.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications, these improvements and modifications can also be made
Also it should be regarded as protection scope of the present invention.
Claims (9)
1. the mass spectrometer of plumage brightness particulate in a kind of laser welding, which is characterized in that including particulate sampling unit with
And vacuum cavity system, the particulate sampling unit include, sampling cone (1a), interception cone (2a) and the collimation of coaxial arrangement
It bores (3a), cooling system (1b) is connected together by the side wall of a copper bar line and sampling cone (1a), the sampling cone
(1a), interception cone (2a) and collimation cone (3a) vacuum cavity system is successively divided into sampling room (1), intercept room (2) and
Ionization sampler chamber (3), sampling room (1) connection cooling system (1b) and oil-sealed rotary pump (1c), interception room (2) connection
Vacuum pump group A (2b), the ionization sampler chamber (3) connect vacuum pump group B (3d), and laser ionization device (4) is located at ionization sampling
On the outside of room (3), be successively arranged inside the ionization sampler chamber (3) ion extraction system (3b), mass analyzer (3e) and from
Sub- detector (3c);The working vacuum degree of the sampling room (1) is less than 1000Pa, and the vacuum degree of interception room (2) work is small
It is less than 0.1Pa in the vacuum degree of 1Pa, ionization sampler chamber (3) work.
2. the mass spectrometer of plumage brightness particulate in laser welding according to claim 1, which is characterized in that described cold
But system (1b) is that liquid nitrogen cooling system or low temperature follow water ring cooling system, for cooling down sampling cone (1a).
3. the mass spectrometer of plumage brightness particulate in laser welding according to claim 1, which is characterized in that described to take
The vertex of a cone bore size that sample bores (1a), interception cone (2a) and collimation cone (3a) is 0.1-1mm, on the outside of centrum angle be 5 °-
179 °, centrum inner angle is 5 ° -178 °, and material is stainless steel or copper or nickel.
4. the mass spectrometer of plumage brightness particulate in laser welding according to claim 1, which is characterized in that the machine
The pumping speed of tool vacuum pump (1c) is greater than 1L/s.
5. the mass spectrometer of plumage brightness particulate in laser welding according to claim 1, which is characterized in that described to swash
Photo-ionisation device (4) be nanosecond laser ionization device or femtosecond laser ionization device.
6. the mass spectrometer of plumage brightness particulate in laser welding according to claim 1, which is characterized in that it is described from
Sub- extraction system (3b) includes ion extraction electrode, ion acceleration electrode, ion focusing electrode and ion deflecting electrode, institute
Stating the voltage that ion extraction electrode and ion acceleration apply is high direct voltage either high voltage pulse, the ion focusing electrode with
And the application of ion deflecting electrode is high direct voltage.
7. the mass spectrometer of plumage brightness particulate in laser welding according to claim 1, which is characterized in that the matter
The extending direction of the opening of contents analyzer (3e) is identical as the heading of particulate.
8. the mass spectrometer of plumage brightness particulate in laser welding according to claim 1, which is characterized in that the matter
Contents analyzer (3e) is flight time mass spectrum mass of ion analyzer or quadrupole rod mass of ion analyzer.
9. the mass spectrometer of plumage brightness particulate in laser welding according to claim 1, which is characterized in that described to take
It is 1-20mm that sample, which bores the vertex of a cone mounting distance between (1a) and interception cone (2a), between the collimation cone (3a) and interception cone (2a)
Vertex of a cone mounting distance be greater than 1mm.
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CN201711357993.8A 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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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 |
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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 |
CN105122422A (en) * | 2013-04-19 | 2015-12-02 | 株式会社岛津制作所 | Mass spectroscopy device |
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 |
CN107068534A (en) * | 2011-12-12 | 2017-08-18 | 塞莫费雪科学(不来梅)有限公司 | Mass spectrometer vacuum interface method and equipment |
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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 |
US10493559B2 (en) * | 2008-07-09 | 2019-12-03 | Fei Company | Method and apparatus for laser machining |
CN102176045B (en) * | 2011-01-20 | 2013-03-13 | 大连理工大学 | Measurement method for spatial distribution of deuterium or tritium detained on surface of first Tokamak wall |
KR20150052898A (en) * | 2013-11-06 | 2015-05-15 | 연세대학교 산학협력단 | Sample plate using MALDI-TOF mass spectrometer and manufacturing method of the sample plate |
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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CN107068534A (en) * | 2011-12-12 | 2017-08-18 | 塞莫费雪科学(不来梅)有限公司 | Mass spectrometer vacuum interface method and equipment |
CN105122422A (en) * | 2013-04-19 | 2015-12-02 | 株式会社岛津制作所 | Mass spectroscopy device |
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 |
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CN107910241A (en) | 2018-04-13 |
CN107910241B (en) | 2019-12-13 |
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