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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
cone
particulate
sampling
ionization
ion
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201711357993.8A
Other languages
Chinese (zh)
Other versions
CN108010829A (en
Inventor
刘本康
王利
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dalian Minzu University
Original Assignee
Dalian Nationalities University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dalian Nationalities University filed Critical Dalian Nationalities University
Priority to CN201711357993.8A priority Critical patent/CN108010829B/en
Publication of CN108010829A publication Critical patent/CN108010829A/en
Application granted granted Critical
Publication of CN108010829B publication Critical patent/CN108010829B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/04Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0409Sample holders or containers
    • H01J49/0418Sample 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 mass spectrometer of plumage brightness particulate in a kind of laser welding
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.
CN201711357993.8A 2017-11-14 2017-11-14 The mass spectrometer of plumage brightness particulate in a kind of laser welding Active CN108010829B (en)

Priority Applications (1)

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

Applications Claiming Priority (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

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
CN201711120072.XA Division CN107910241B (en) 2017-11-14 2017-11-14 Mass spectrum analysis device for plasma plume microparticle components in laser welding

Publications (2)

Publication Number Publication Date
CN108010829A CN108010829A (en) 2018-05-08
CN108010829B true CN108010829B (en) 2019-12-03

Family

ID=61843866

Family Applications (2)

Application Number Title Priority Date Filing Date
CN201711120072.XA Active CN107910241B (en) 2017-11-14 2017-11-14 Mass spectrum analysis device for plasma plume microparticle components in laser welding
CN201711357993.8A Active CN108010829B (en) 2017-11-14 2017-11-14 The mass spectrometer of plumage brightness particulate in a kind of laser welding

Family Applications Before (1)

Application Number Title Priority Date Filing Date
CN201711120072.XA Active CN107910241B (en) 2017-11-14 2017-11-14 Mass spectrum analysis device for plasma plume microparticle components in laser welding

Country Status (1)

Country Link
CN (2) CN107910241B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112133165A (en) * 2020-10-15 2020-12-25 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

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Also Published As

Publication number Publication date
CN108010829A (en) 2018-05-08
CN107910241A (en) 2018-04-13
CN107910241B (en) 2019-12-13

Similar Documents

Publication Publication Date Title
US9312111B2 (en) Apparatus and method for sub-micrometer elemental image analysis by mass spectrometry
Hattendorf et al. Peer reviewed: laser ablation-ICPMS
Pisonero et al. Critical revision of GD-MS, LA-ICP-MS and SIMS as inorganic mass spectrometric techniques for direct solid analysis
DE69936168T2 (en) Mehrfachprobeninlassmassenspektrometer
CN108010829B (en) The mass spectrometer of plumage brightness particulate in a kind of laser welding
CN108169092B (en) Online detection device and method for heavy metals and isotopes of atmospheric particulates
US20100181473A1 (en) Method and apparatus for the analysis of samples
Leach et al. Factors affecting the production of fast transient signals in single shot laser ablation inductively coupled plasma mass spectrometry
CN104392887A (en) Femtosecond laser post-ionization mass spectrum apparatus
Barnes et al. Use of a novel array detector for the direct analysis of solid samples by laser ablation inductively coupled plasma sector-field mass spectrometry
CZ306708B6 (en) A device for mass spectrometry
Wang et al. Simultaneous high sensitivity trace-element and isotopic analysis of gemstones using laser ablation inductively coupled plasma time-of-flight mass spectrometry
Stroh et al. Analysis of samples containing large amounts of dissolved solids using microsampling flow injection inductively coupled plasma mass spectrometry
Dorta et al. Determining isotope ratios using laser ablation sampling in air with MC-ICPMS
JP2008070122A (en) Mass analysis method and mass spectrometer
Ganeev et al. Mass spectrometric methods for the direct elemental and isotopic analysis of solid materials
le Roux Lithium isotope analysis of natural and synthetic glass by laser ablation MC-ICP-MS
Gundlach-Graham et al. Laser-ablation sampling for inductively coupled plasma distance-of-flight mass spectrometry
Fricker et al. Instrumentation, fundamentals, and application of laser ablation-inductively coupled plasma-mass spectrometry
Hirata In-situ precise isotopic analysis of tungsten using laser ablation multi-collector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS) with time resolved data acquisition
JP2021148679A (en) Imaging mass spectrometry system, and analysis method utilizing imaging mass spectrometry
He et al. A small high‐irradiance laser ionization time‐of‐flight mass spectrometer
Djurić et al. Measurement of light fragments in dissociative excitation of molecular ions: CD+
Hieftje et al. New developments and final frontiers in inductively coupled plasma spectrometry. Plenary lecture
CN107946167B (en) A kind of metal complex mass spectrometer

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant