US3423583A - Method of stabilization of thermionic sources and thermionic source obtained by application of said method or a like method - Google Patents
Method of stabilization of thermionic sources and thermionic source obtained by application of said method or a like method Download PDFInfo
- Publication number
- US3423583A US3423583A US442773A US3423583DA US3423583A US 3423583 A US3423583 A US 3423583A US 442773 A US442773 A US 442773A US 3423583D A US3423583D A US 3423583DA US 3423583 A US3423583 A US 3423583A
- Authority
- US
- United States
- Prior art keywords
- filament
- thermionic
- layer
- substance
- source
- 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.)
- Expired - Lifetime
Links
- 238000000034 method Methods 0.000 title description 11
- 230000006641 stabilisation Effects 0.000 title description 2
- 238000011105 stabilization Methods 0.000 title description 2
- 239000000126 substance Substances 0.000 description 23
- 238000010438 heat treatment Methods 0.000 description 11
- 238000004949 mass spectrometry Methods 0.000 description 10
- 238000001354 calcination Methods 0.000 description 8
- 239000003381 stabilizer Substances 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229910000480 nickel oxide Inorganic materials 0.000 description 5
- 230000000087 stabilizing effect Effects 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 4
- BDVMTRCCIQHRBL-UHFFFAOYSA-J phosphonato phosphate;titanium(4+) Chemical compound [Ti+4].[O-]P([O-])(=O)OP([O-])([O-])=O BDVMTRCCIQHRBL-UHFFFAOYSA-J 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000000151 deposition Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- -1 magnesium aluminate Chemical class 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000000155 isotopic effect Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical class [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical class [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical class [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical class [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052735 hafnium Chemical class 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical class [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical class [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H03—ELECTRONIC CIRCUITRY
- H03F—AMPLIFIERS
- H03F1/00—Details of amplifiers with only discharge tubes, only semiconductor devices or only unspecified devices as amplifying elements
- H03F1/52—Circuit arrangements for protecting such amplifiers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J27/00—Ion beam tubes
- H01J27/02—Ion sources; Ion guns
- H01J27/26—Ion sources; Ion guns using surface ionisation, e.g. field effect ion sources, thermionic ion sources
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
-
- H—ELECTRICITY
- H03—ELECTRONIC CIRCUITRY
- H03F—AMPLIFIERS
- H03F3/00—Amplifiers with only discharge tubes or only semiconductor devices as amplifying elements
- H03F3/04—Amplifiers with only discharge tubes or only semiconductor devices as amplifying elements with semiconductor devices only
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2913—Rod, strand, filament or fiber
- Y10T428/2933—Coated or with bond, impregnation or core
- Y10T428/294—Coated or with bond, impregnation or core including metal or compound thereof [excluding glass, ceramic and asbestos]
- Y10T428/2942—Plural coatings
- Y10T428/2949—Glass, ceramic or metal oxide in coating
Definitions
- the present invention is concerned with stabilized thermionic sources and their method of preparation.
- the thermionic sources according to the present invention are designed for use in mass spectrometry.
- the sources are prepared by coating a metallic heating filament with a layer of refractory substance possessing poor thermal conductivity.
- the coating preferably is carried out by depositing on the surface of the filament a layer of the refractory substance and calcining the structure thus obtained so as to adhere said layer to the filament.
- the resulting stabilized filament is then coated with a layer of a mixture comprising the product to be analyzed and the refractory substance.
- the filament is again calcined so as to produce an outer layer composed of the latter mixture. Titanium pyrophosphate, magnesium aluminate and nickel oxide have been found to be the preferable refractory substances.
- the invention has for its object a method of stabilization of a thermionic source which can be utilized in mass spectrometry and which makes it possible to obtain a constant thermionic emission.
- the method in accordance with the invention consists in depositing on a metallic filament which serves as a heating source a layer of substance which is capable of providing as a result of heating a uniform layer having a smooth surface, in effecting the slow calcination of the filament which is coated with said substance until there is formed a layer which effectively adheres to the filament, in charging the aggregate thus obtained with a mixture consisting of said substance and of the product to be analyzed by mass spectrometry and in calcining the aggregate.
- the thermionic source as thus prepared can be employed for the purpose of performing an analysis by mass spectrometry; said source consists of a heating filament which is coated with a layer of stabilizing substance which is in turn coated with a layer of a mixture of the stabilizing substance and of the substance to be analyzed.
- the stabilizer must be refractory and have poor thermal conductivity in order to withstand without melting the high temperatures to which the filament is brought at the time of heating.
- the stabilizer must be such that, after it has been applied on the filament and after said filament has been heated, said stabilizer is present in a uniform layer having a smooth surface.
- the stabilizing substance thus prepared is essentially intended for temperature stabilizatron.
- Titanium pyrophosphate TiP O- Magnesium aluminate (MgAl O Nickel oxide (NiO).
- salts are also suitable for the practical application of the invention. It is merely necessary to ensure that such salts meet the following conditions: they must be refractory, they must have poor thermal conductivity and they must provide, once they have been applied on the filament and heated, a uniform layer having a smooth surface.
- salts of calcium, strontium, barium, zirconium, thorium and hafnium can be mentioned by way of example the salts of calcium, strontium, barium, zirconium, thorium and hafnium.
- the metallic heating filament consists of a metal which has a high melting point and which can advantageously be platinum, rhenium or tungsten.
- the stabilizer is prepared in the form of gel and is deposited on the filament by means of a platinum spatula; the aggregate is then subjected to a first calcining treatment by sending an electric current through the filament, thus increasing its temperature by Joule effect.
- the heating must be performed with care in such a manner as to ensure that the layer of stabilizing substance effectively adheres to the filament after calcination.
- the filament which is thus covered with stabilizer is then charged with a layer of stabilizing substance which is mixed with the product to be analyzed.
- the quantities employed must be small since it would prove undesirable to overcharge the filament.
- the calcination is then performed under the same conditions as before.
- the filament appears in the form of a thin layer of stabilizer which adheres to the metal in a perfect manner and the thickness of which can vary between 0.2 and 1 mm. but is preferably equal to 0.5 mm. Under the microscope, the surface of said layer is of uniform appearance although not glass-like.
- the source then remains stable throughout the analysis (this latter can last several hours) without any appreciable decrease in.the ion current.
- a thermionic source in accordance with the invention has the great advantage, in particular when performing an analysis by mass spectrometry, in that the product to be analyzed can be utilized in solid form, thus requiring only a minimum number of manipulations. Moreover, a source of this kind makes it possible to perform isotopic analyses of long duration without any fluctuations which are higher than those produced by a gas source.
- a method for producing a stabilized thermionic source designed for use in mass spectrometry which method comprises the steps of:
- a method according to claim 1 wherein said substance is selected from the group consisting of titanium pyrophosphate, magnesium aluminate and nickel oxide.
- a thermionic source designed for use in mass spectrometery which comprises a heating filament composed of a conductive substance having a high melting point coated with a uniform layer of a refractory substance having poor thermal conductivity and additionally coated with a layer comprising a mixture of the product to be analyzed by mass spectrometry and said refractory substance.
- a thermionic source according to claim 3 wherein said refractory substance is selected from the group consisting of titanium pyrophosphate, magnesium aluminate and nickel oxide.
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Analytical Chemistry (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR968985A FR1398135A (fr) | 1964-03-27 | 1964-03-27 | Procédé de stabilisation de sources thermoioniques et source thermoionique conforme à celles obtenues par application dudit procédé ou d'un procédé analogue |
Publications (1)
Publication Number | Publication Date |
---|---|
US3423583A true US3423583A (en) | 1969-01-21 |
Family
ID=8826561
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US442773A Expired - Lifetime US3423583A (en) | 1964-03-27 | 1965-03-25 | Method of stabilization of thermionic sources and thermionic source obtained by application of said method or a like method |
Country Status (9)
Country | Link |
---|---|
US (1) | US3423583A (en]) |
BE (1) | BE661230A (en]) |
CH (1) | CH432054A (en]) |
DE (1) | DE1297899B (en]) |
FR (1) | FR1398135A (en]) |
GB (1) | GB1088268A (en]) |
IL (1) | IL23192A (en]) |
LU (1) | LU48259A1 (en]) |
NL (1) | NL6503985A (en]) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2019213130A3 (en) * | 2018-04-30 | 2019-12-19 | Leidos, Inc. | An improved low-power mass interrogation system and assay for determining vitamin d levels |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9091151B2 (en) | 2009-11-19 | 2015-07-28 | Halliburton Energy Services, Inc. | Downhole optical radiometry tool |
US8885163B2 (en) | 2009-12-23 | 2014-11-11 | Halliburton Energy Services, Inc. | Interferometry-based downhole analysis tool |
BR112012027653A2 (pt) | 2010-06-01 | 2016-08-16 | Halliburton Energy Services Inc | método e sistema para medir propriedades de formação |
CA2781331A1 (en) * | 2010-06-16 | 2011-12-22 | Halliburton Energy Services, Inc. | Downhole sources having enhanced ir emission |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2710354A (en) * | 1952-08-28 | 1955-06-07 | Mark G Inghram | Ion source |
US2756341A (en) * | 1954-02-15 | 1956-07-24 | Gen Electric | Multiple cartridge source for mass spectrometer |
US3195004A (en) * | 1960-08-19 | 1965-07-13 | Rca Corp | Cathode heater for electron discharge devices |
-
1964
- 1964-03-27 FR FR968985A patent/FR1398135A/fr not_active Expired
-
1965
- 1965-03-15 CH CH357365A patent/CH432054A/fr unknown
- 1965-03-17 DE DEC35339A patent/DE1297899B/de active Pending
- 1965-03-17 BE BE661230A patent/BE661230A/xx unknown
- 1965-03-19 GB GB11756/65A patent/GB1088268A/en not_active Expired
- 1965-03-22 IL IL23192A patent/IL23192A/en unknown
- 1965-03-25 US US442773A patent/US3423583A/en not_active Expired - Lifetime
- 1965-03-25 LU LU48259A patent/LU48259A1/xx unknown
- 1965-03-29 NL NL6503985A patent/NL6503985A/xx unknown
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2710354A (en) * | 1952-08-28 | 1955-06-07 | Mark G Inghram | Ion source |
US2756341A (en) * | 1954-02-15 | 1956-07-24 | Gen Electric | Multiple cartridge source for mass spectrometer |
US3195004A (en) * | 1960-08-19 | 1965-07-13 | Rca Corp | Cathode heater for electron discharge devices |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2019213130A3 (en) * | 2018-04-30 | 2019-12-19 | Leidos, Inc. | An improved low-power mass interrogation system and assay for determining vitamin d levels |
US11227754B2 (en) | 2018-04-30 | 2022-01-18 | Leidos, Inc. | Low-power mass interrogation system and assay for determining vitamin D levels |
US11967495B2 (en) | 2018-04-30 | 2024-04-23 | Leidos, Inc. | Low-power mass interrogation system and assay for determining Vitamin D levels |
US12261032B2 (en) | 2018-04-30 | 2025-03-25 | Leidos, Inc. | Low-power mass interrogation system and assay for determining vitamin D levels |
Also Published As
Publication number | Publication date |
---|---|
LU48259A1 (en]) | 1965-05-25 |
FR1398135A (fr) | 1965-05-07 |
BE661230A (en]) | 1965-07-16 |
NL6503985A (en]) | 1965-09-28 |
GB1088268A (en) | 1967-10-25 |
IL23192A (en) | 1968-07-25 |
CH432054A (fr) | 1967-03-15 |
DE1297899B (de) | 1969-06-19 |
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