CN1305101C - Micro-chamber four-electrode spectrum tube - Google Patents

Micro-chamber four-electrode spectrum tube Download PDF

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CN1305101C
CN1305101C CNB2004100651418A CN200410065141A CN1305101C CN 1305101 C CN1305101 C CN 1305101C CN B2004100651418 A CNB2004100651418 A CN B2004100651418A CN 200410065141 A CN200410065141 A CN 200410065141A CN 1305101 C CN1305101 C CN 1305101C
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electrode
vacuum
tube
ceramic
cavity
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CN1601691A (en
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张晓兵
毛福明
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Southeast University
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Southeast University
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Abstract

The present invention discloses a micro-cavity quadrupole mass spectrum tube which relates to a quadrupole mass spectrum tube carrying out residual gas analysis of electric vacuum devices such as a microwave device, a cathode ray tube (CRT), a field emission device, a light source, etc. and comprises a quadrupole mass analyzer, an ion source and an ion detector. The present invention is characterized in that a ceramic metallization quadrupole mass analyzer (1) is adopted, wherein a porcelain tube (1.2) serves as a vacuum casting and the inner cavity of the porcelain tube (1.2) is provided with four electrode masts (1.3) of the quadrupole mass analyzer; both end surfaces of the quadrupole mass analyzer (1) are provided with metalization conductive layers (1.5) to avoid charge accumulation; through a metalization hole (1.7) inside the porcelain tube (1.2), a metal electrode guide needle (1.6) is led out from the inner surface of a metalization conducting layer (1.5) or the four electrode masts (1.3) to the outside of the cavity of the vacuum porcelain tube (1.2); the porcelain tube (1.2) of the quadrupole mass analyzer (1) is connected with the vacuum cavities of the ion source (2) and the ion detector (3) in a mode of vacuum sealing connection between metal and ceramics.

Description

Micro-chamber four-electrode spectrum tube
Technical field
The present invention relates to electron tubes such as microwave device, cathode ray tube (CRT), feds, light source are carried out the four-electrode spectrum tube of rga, it has also solved the difficult problem of electron tubes such as volume is little, vacuum degree is high microwave tube, Field Emission Display residual gas nondestructive analysis in exhaust process and product export advance line pipe except the function with traditional four-electrode spectrum tube.
Background technology
The residual gas of electron tube inside is one of principal element that influences the electron tube performance, and residual gas often adopts the way of mass spectral analysis to the influence of component failure in the electron tube in order to analyze.Directly put into the method that the mass spectral analysis vacuum system breaks up and carry out the sample analysis except that the small electrical vacuum device can adopt, generally be to make a call to a hole of not running through in advance on the glass bulb of electron tube or metal-back, the pipeline with hole and mass spectrometry system is connected then.After vacuum system reaches the certain vacuum degree, with boring device this hole is broken up, make the interior gas of pipe enter the vacuum analytical system by the hole.In this analytical system, generally adopt quadrupole mass spectrometer to carry out the analysis of residual gas.Analyze vacuum system and be made up of sampler and pipeline, analysis room, four-electrode spectrum tube, vacuum unit etc. usually, four-electrode spectrum tube generally is made up of ion source, mass analyzer and ion detector three parts.Four-electrode spectrum tube is placed in the vacuum cavity now, and all contact conductors focus on the stem stem flange and guide to outside the vacuum cavity.For guaranteeing the gap and the vacuum exhaust performance of contact conductor, the volume of spectrum tube will arrive several thousand milliliters at hundreds of, and the surface area of vacuum chamber internal electrode is also bigger.Because devices such as microwave tube, Field Emission Display plate, its internal volume is very little, great majority only have several milliliters to tens milliliters, big pipe also only has the hundreds of milliliter, vacuum degree is than higher in face and the pipe, particularly microwave tube can reach the level of ultra high vacuum, therefore the residual air capacity in the pipe is very little, adopt this traditional four-electrode spectrum tube and sampling vacuum system to analyze, pressure after residual gas to be analyzed expands can reduce significantly, and the background gas of spectrum tube and vacuum analytical system can produce very big interference to analysis precision simultaneously.
Summary of the invention
Technical problem: the purpose of this invention is to provide a kind of micro-chamber four-electrode spectrum tube that the four-electrode spectrum tube vacuum cavity of stock size is dwindled hundreds of times.
Technical scheme: in order to realize above purpose, the long-pending four-electrode spectrum tube of microbody of the present invention is with each assembly of traditional four-electrode spectrum tube, applied metal-ceramic vacuum sealing technology, the earthenware of shell and the synthetic special shape of quadrupole rod, make quadrupole rod hyperboloid shape in the porcelain tube, be coated with metal film or the sheet metal electrode that performs an analysis, contact conductor directly passes the porcelain bar, ion detector, the vacuum cavity of parts such as ion source also carries out miniaturized, internal cavity is a vacuum, space for the electronic and ionic proper motion, thereby dwindled the cavity space of conventional structure spectrum tube and the surface area of the interior electrode of vacuum greatly, satisfied microwave tube, the rga of the vacuum device of little discharge quantity such as feds.
Micro-chamber four-electrode spectrum tube of the present invention specifically comprises four-electrode quality analyzer, ion source, ion detector, adopt the ceramic metallization four-electrode quality analyzer, wherein, porcelain tube is as vacuum casting, the porcelain tube inner chamber is provided with four utmost point bars of four-electrode quality analyzer, both ends of the surface at four-electrode quality analyzer also are provided with the metallization conductive layer to avoid the electric charge accumulation, metal electrode draws pin and is drawn out to outside the vacuum porcelain tube cavity by the plated-through hole the porcelain tube from metallization conductive layer or four utmost point bar inner surfaces, and the vacuum seal that is connected to metal-ceramic between the vacuum cavity of the porcelain tube of four-electrode quality analyzer and ion source and ion detector is connected;
The internal holes of the porcelain tube in the ceramic metallization four-electrode quality analyzer is hyperboloid type hole, and the inner surface in hyperboloid type hole is made the electrode of four utmost point bars of metallization, is the space between adjacent two electrodes.
Ionogenic shell is a vacuum cavity, it can be metal, it also can be pottery, outer face or side at this vacuum cavity are provided with passage or the vacuum joint access flange that analytical gas enters, for the metal vacuum cavity, electrode is drawn out to the spectrum tube outside by the contact conductor that is produced on the stem stem flange; For the ceramic vacuum cavity, electrode is installed or directly is coated on the internal face of porcelain tube vacuum cavity,
Ion source can adopt the vacuum pan seal structure, promptly in this ion source, with ceramic ring at interval as the medium between the electrode slice, between first electrode slice, second electrode slice and the ceramic ring and the vacuum seal of the end face ceramic segment of first electrode slice and four-electrode quality analyzer employing vacuum pan seal structure, this part is a joint face with the left side of porcelain tube, the order that is linked in sequence is: first electrode slice, ceramic ring, second electrode slice, ceramic ring, the cathode filament electrode, ceramic ring, inlet flange.
The cathode filament electrode is drawn by the Cyclometalated hole of porcelain.
The ion detector that described ion detector is made up of electron multiplier, the flange and contact conductor, the vacuum cavity that provide electrode to draw are formed; The right side of porcelain tube adopts the vacuum seal of metal-ceramic to be connected in its vacuum cavity and the four-electrode quality analyzer, and the electrode of ion detector is drawn out to the spectrum tube outside by the contact conductor that is produced on the stem stem flange.
Form ion detector by Faraday cup in the described ion detector, this ion detector directly with the sealing-in mutually of four-electrode quality analyzer earthenware.
Metallized four utmost point bars of described four-electrode quality analyzer inner surface adopt ceramic metallization, vacuum coating, the method that belongs to diaphragm of gilding makes four electrodes of ceramic surface have conductivity, keep electric insulation between four electrodes.
Beneficial effect: use the volume that this structure can be dwindled the four-electrode spectrum tube vacuum cavity, reduced the discharge quantity of electrode surface simultaneously, reduced the interference of background gas, improved the reliability of measurement data.
The present invention adopts metal-ceramic sealing technology and spectrum tube structure, has made the spectrum tube of microcavity body, satisfies the rga requirement of little residual air capacity vacuum devices such as microwave tube.This microcavity body spectrum tube can be used with the traditional vacuum analytical system, also can be used as an individual components exhaust together of devices such as microwave tube, after the pipe sealed-off, the finished product device is carried out gas analysis in direct or certain time limit, spectrum tube sealed-off from the device, finish the nondestructive analysis of device at last.
Description of drawings
Fig. 1 is in the ceramic metallization micro-chamber four-electrode mass analyzer of the present invention, the cross section structure schematic diagram of porcelain tube 1.2.
Fig. 2 is the end face structure schematic diagram of ceramic metallization four-electrode quality analyzer of the present invention.
Fig. 3 is the structural representation that ceramic metallization four-electrode quality analyzer electrode of the present invention is drawn from end face.
Fig. 4 is the structural representation that ceramic metallization four-electrode quality analyzer electrode of the present invention is drawn from the spectrum tube inner surface electrode.
Fig. 5 is the structural representation of micro-chamber four-electrode spectrum tube of the present invention.
Fig. 6 is the structural representation of Faraday cup ion detector micro-chamber four-electrode spectrum tube.
Fig. 7 adopts the disk seal technology to draw the micro-chamber four-electrode spectrum tube structural representation of ion source electrode.
Embodiment
All electrodes of the spectrum tube of traditional quadrupole mass spectrometer and lead-in wire all are placed in the vacuum cavity fully, cause cavity volume very big, the surface area of vacuum chamber internal electrode is also very big, the rga that be not suitable for being applied to small sizes such as microwave tube and Field Emission Display, hangs down the vacuum device of discharge quantity.
The present invention proposes a kind of micro-chamber four-electrode spectrum tube structure and manufacturing technology that reduces spectrum tube vacuum cavity volume, can reduce hundreds of times of the volumes of spectrum tube cavity effectively, make its be fit to the rga of small size such as microwave tube, low discharge quantity vacuum device, also can substitute traditional four-electrode spectrum tube simultaneously.
Scheme proposed by the invention is made the long-pending four-electrode quality analyzer 1 of microbody, this spectrum tube is made of the vacuum porcelain tube 1.2 that inside has hyperboloid type hole 1.1, the inner surface in the hyperboloid type hole in the porcelain tube 1.2 adopts ceramic metallization method or vacuum coating or the method that belongs to diaphragm of gilding is made metallization quadrupole rod electrode 1.3, between two electrodes, be provided with space 1.4, do not make metallic electrode and make between the adjacent electrode and insulate, make metallization end face electrode 1.5 to avoid the electric charge accumulation yet in the both ends of the surface of spectrum tube; The mode that electrode connecting line is drawn to vacuum cavity from metallized end face changes metal electrode into and draws pin 1.6, be drawn out to outside the vacuum ceramic cavity 1.2 by the plated-through hole the vacuum ceramic 1.7 from metallization end face electrode 1.5 or from four-electrode spectrum tube inner surface electrode 1.3, metal electrode draws the method that adopts the metallization slurry to fill sintering between pin 1.6 and the plated-through hole 1.7 and realizes vacuum seal, and the advantage of Fig. 3 lead-in wire is the precision that the local deformation of electrode contact surface can not influence quadrupole field.
The diameter of the metal vacuum cavity 2.7 at ion source position 2 can be narrowed down to the size suitable with ionogenic diameter, the cavity aperture of vacuum cavity 2.7 and mass analyzer connecting portion is narrowed down to the size suitable with metallized ceramic micro-chamber four-electrode mass analyzer 1, directly to carry out the sealing-in of metal-ceramic with mass analyzer vacuum porcelain tube 1.2, electrode directly is drawn out to the outside by contact conductor 2.9, at the vacuum joint access flange 2.10 of ion source one end retention analysis gas admission passage, as shown in Figure 5.Adopt vacuum seal to be connected between vacuum cavity 2.7 and the electrode stem stem flange 2.8.
The diameter of the ceramic vacuum cavity 2.7 at ion source position 2 can be narrowed down to the size suitable with ionogenic diameter, vacuum cavity 2.7 and mass analyzer connecting portion adopt becket respectively with ceramic vacuum cavity 2.7, and mass analyzer vacuum porcelain tube 1.2 carries out the sealing-in of metal-ceramic, electrode is installed or directly is coated on the internal face of porcelain tube vacuum cavity 2.7, is drawn out to the outside by the plated-through hole that is produced on the porcelain tube vacuum cavity.
If adopt the ion detector of electron multiplier, then the diameter of the vacuum cavity 3.2 of ion detector 3 is by the kind and the size decision of electron multiplier, but narrow down to the size suitable in cavity aperture with metallized ceramic micro-chamber four-electrode mass analyzer 1 with the mass analyzer connecting portion, adopt the sealing technology of metal-ceramic to carry out vacuum seal with ceramic segment with cermet four-electrode quality analyzer end face, the electrode of ion detector is drawn out to the spectrum tube outside by the contact conductor 3.4 that is produced on the stem stem flange 3.3, as shown in Figure 5.
If adopt the ion detector 3 of faraday cylinder collector, then Faraday cup 3.1 directly adopts the sealing technology sealing-in mutually of metal-ceramic with the analyzer earthenware, as shown in Figure 6.
Fig. 7 is a kind of metal dish sealed-off component schematic diagram.Vacuum seal between metal electrode such as first electrode slice 2.4, second electrode slice 2.3 and the ceramic ring 2.5 adopts the vacuum pan encapsulation technique to make, and the lead-out wire 2.2 of filament 2.1 electrodes and plated-through hole 2.6 sealing-in are mutually drawn.Sample gas is introduced by feeder connection flange or metal tube 2.10.Ion source shown in Figure 7 with compare with the scheme of Fig. 5, do not have ion source contact conductor occupation space, the vacuum cavity volume is further reduced, but the vacuum seal of Fig. 5 mode lead-out wire is fairly simple.
During work, inlet flange 2.10 is connected to the mass spectral analysis vacuum system, spectrum tube of the present invention is vacuumized, after reaching the vacuum degree that meets test request, open is supporting spectrum tube power supply of the present invention and the shell that breaks up sample to be analyzed, the mass signal of collected specimens gas reaches analysis purpose.
Because four-electrode spectrum tube of the present invention dwindles hundred times more than than the cavity volume of traditional four-electrode spectrum tube, with The time spectrum tube can high-temperature baking resistant, therefore except the function with traditional four-electrode spectrum tube, can also be as one Independently annex after the device sealed-off, is opened mass spectrograph with analyzed vacuum device exhaust as required at any time. Owing to do not have attached sampling vacuum system, can obtain real gas mass spectrogram, after to be analyzed the finishing, again matter The sealed-off from the device of spectrum pipe is got off, thereby finishes the nondestructive analysis of vacuum device, and this is major advantage of the present invention.

Claims (8)

1. micro-chamber four-electrode spectrum tube, comprise four-electrode quality analyzer, ion source, ion detector, it is characterized in that: adopt ceramic metallization four-electrode quality analyzer (1), wherein, porcelain tube (1.2) is as vacuum casting, porcelain tube (1.2) surface of internal cavity is covered with four utmost point bars (1.3) of four-electrode quality analyzer, both ends of the surface at four-electrode quality analyzer (1) also are provided with metallization conductive layer (1.5) to avoid the electric charge accumulation, metal electrode draws pin (1.6) and is drawn out to outside vacuum porcelain tube (1.2) cavity by the plated-through hole (1.7) the porcelain tube (1.2) from metallization conductive layer (1.5) or four utmost point bars (1.3) inner surface, and the vacuum seal that is connected to metal-ceramic between the vacuum cavity of the porcelain tube (1.2) of four-electrode quality analyzer (1) and ion source (2) and ion detector (3) is connected.
2. micro-chamber four-electrode spectrum tube according to claim 1, it is characterized in that: the internal holes of the porcelain tube (1.2) in the ceramic metallization four-electrode quality analyzer (1) is hyperboloid type hole (1.1), the inner surface in hyperboloid type hole (1.1) is made the electrode of four utmost point bars of metallization (1.3), is space (1.4) between adjacent two electrodes.
3. micro-chamber four-electrode spectrum tube according to claim 1, it is characterized in that: the shell of ion source (2) is metal vacuum cavity (2.7), outer face or side at this vacuum cavity (2.7) are provided with passage or the vacuum joint access flange (2.10) that analytical gas enters, and electrode is drawn out to the spectrum tube outside by the contact conductor (2.9) that is produced on stem stem flange (2.8).
4. micro-chamber four-electrode spectrum tube according to claim 1, it is characterized in that: the shell of ion source (2) is ceramic vacuum cavity (2.7), outer face or side at this vacuum cavity (2.7) are provided with passage or the vacuum joint access flange (2.10) that analytical gas enters, be connected with becket between the porcelain tube (1.2) of ion source ceramic vacuum cavity (2.7) and four-electrode quality analyzer (1) as transition, adopt the metal-ceramic Sealing Technology to carry out sealing-in, at this moment electrode is installed or directly is coated on the internal face of ceramic vacuum cavity (2.7), is drawn out to the outside by the plated-through hole that is produced on the ceramic vacuum cavity.
5. micro-chamber four-electrode spectrum tube according to claim 1, it is characterized in that: ion source (2) adopts the vacuum pan seal structure, promptly in this ion source (2), with ceramic ring (2.5) at interval as the medium between the electrode slice, first electrode slice (2.4), between second electrode slice (2.3) and the ceramic ring (2.5) and the vacuum seal of the end face ceramic segment of first electrode slice (2.4) and four-electrode quality analyzer (1) adopt the vacuum pan seal structure, this part is a joint face with the left side of porcelain tube (1.2), the order that is linked in sequence is: first electrode slice (2.4), ceramic ring (2.5), second electrode slice (2.3), ceramic ring (2.5), cathode filament electrode (2.2), ceramic ring (2.5), inlet flange (2.10), cathode filament electrode (2.2) is drawn by the Cyclometalated hole of porcelain (2.6).
6. micro-chamber four-electrode spectrum tube according to claim 1 is characterized in that: the ion detector (3.1) that described ion detector (3) is made up of electron multiplier, the flange (3.3) and contact conductor (3.4), the vacuum cavity (3.2) that provide electrode to draw are formed; The right side of porcelain tube (1.2) adopts the vacuum seal of metal-ceramic to be connected in its vacuum cavity (3.2) and the four-electrode quality analyzer, and the electrode of ion detector is drawn out to the spectrum tube outside by the contact conductor (3.4) that is produced on the stem stem flange (3.3).
7. micro-chamber four-electrode spectrum tube according to claim 1 is characterized in that forming ion detector (3.1) by Faraday cup in the described ion detector (3), this ion detector (3.1) directly with four-electrode quality analyzer earthenware (1.2) sealing-in mutually.
8. micro-chamber four-electrode spectrum tube according to claim 1 and 2, it is characterized in that described four-electrode quality analyzer (1) metallized four utmost point bars of inner surface (1.3) adopt metallization slurry coating back sintering, vacuum coating, the method that belongs to diaphragm of gilding to make four electrodes of ceramic surface have conductivity, keep electric insulation between four electrodes.
CNB2004100651418A 2004-10-27 2004-10-27 Micro-chamber four-electrode spectrum tube Active CN1305101C (en)

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CN100454020C (en) * 2005-10-19 2009-01-21 广州禾信自动化***有限公司 Gas-phase molecular ion reactor based on radio-frequency quard-polar rod, its realization and use
CN100454477C (en) * 2005-12-16 2009-01-21 广州禾信自动化***有限公司 Single-particle aerosol online ionization source and realization method thereof
CN101144794B (en) * 2007-10-29 2010-11-24 钢铁研究总院 Impulse melting mass spectrometry analysis method for element
CN103187218B (en) * 2012-10-19 2015-08-19 北京北分瑞利分析仪器(集团)有限责任公司 Hyperboloid quadrupole rod and processing method thereof and quadrupole mass spectrometer
US9508534B2 (en) * 2014-11-07 2016-11-29 Thermo Finnigan Llc Systems and methods for calibrating gain in an electron multiplier
CN108519427B (en) * 2018-04-13 2020-02-21 哈尔滨工业大学(威海) Mass analysis method and mass spectrometer suitable for high-pressure environment
CN110400732A (en) * 2019-07-18 2019-11-01 苏州微木智能***有限公司 A kind of electrode moulding method, migration tube and ionic migration spectrometer

Citations (4)

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Publication number Priority date Publication date Assignee Title
US3940616A (en) * 1972-01-13 1976-02-24 Geoffrey William Ball Mass spectrometers
CN1100808A (en) * 1993-05-11 1995-03-29 Mks仪器有限公司 Quadrupole mass spectrometer
JPH1125904A (en) * 1997-06-30 1999-01-29 Shimadzu Corp Quadrupole mass spectrometer
CN2751434Y (en) * 2004-10-27 2006-01-11 东南大学 Micro-cavity quadrupole mass spectrum tube

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3940616A (en) * 1972-01-13 1976-02-24 Geoffrey William Ball Mass spectrometers
CN1100808A (en) * 1993-05-11 1995-03-29 Mks仪器有限公司 Quadrupole mass spectrometer
JPH1125904A (en) * 1997-06-30 1999-01-29 Shimadzu Corp Quadrupole mass spectrometer
CN2751434Y (en) * 2004-10-27 2006-01-11 东南大学 Micro-cavity quadrupole mass spectrum tube

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