US3211826A - Quartz to metal seal - Google Patents

Quartz to metal seal Download PDF

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US3211826A
US3211826A US96128A US9612861A US3211826A US 3211826 A US3211826 A US 3211826A US 96128 A US96128 A US 96128A US 9612861 A US9612861 A US 9612861A US 3211826 A US3211826 A US 3211826A
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seal
lead
lead portion
quartz
parts
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US96128A
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Richard H Holcomb
Gene I Thomasson
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General Electric Co
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General Electric Co
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Priority to US96128A priority patent/US3211826A/en
Priority to ES0274377A priority patent/ES274377A1/en
Priority to GB6726/62A priority patent/GB946094A/en
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
    • C03C27/04—Joining glass to metal by means of an interlayer
    • C03C27/042—Joining glass to metal by means of an interlayer consisting of a combination of materials selected from glass, glass-ceramic or ceramic material with metals, metal oxides or metal salts
    • C03C27/044—Joining glass to metal by means of an interlayer consisting of a combination of materials selected from glass, glass-ceramic or ceramic material with metals, metal oxides or metal salts of glass, glass-ceramic or ceramic material only
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01K—ELECTRIC INCANDESCENT LAMPS
    • H01K1/00—Details
    • H01K1/38—Seals for leading-in conductors

Definitions

  • This invention relates generally to seals of metallic lead-in conductors in quartz or fused silica for electrical devices comprising a sealed envelope containing electric energy translation means to which electric current is supplied through the lead-in conductor.
  • quartz infrared lamps which comprise a tubular envelope of quartz having an incandescible fila-. ment of coiled tungsten wire extending longitudinally therethrough and connected at its ends to lead-in conductors which are hermetically sealed through compressed or pinched seal portions at the ends of the envelope.
  • the lead-in conductors are each generally composed of molybdenum wires having a very thin intermediate foliated or ribbon portion which is wetted to and hermetically sealed in the quartz seal portion. Molybdenum is preferred because of its high melting point whereby it can withstand the high temperatures required to fuse the quartz thereto.
  • seals are entirely satisfactory so long as the seal temperature does not exceed about 350 C. At higher temperatures, the seal fails much more rapidly due to oxidation of the molybdenum. For example, at temperatures not exceeding 350 C. the seal lasts for several thousand hours whereas at a temperature of about 400 C. the average life drops to a few hundred hours. There has been a need for seals which will remain hermetically tight at elevated temperatures.
  • quartz to metal seals of increased life at elevated temperatures More particularly, it is an object to provide a seal structure having a life which may be up to eight hundred times that of the prior art molybdenum-quartz seal in the temperature range of about 500 to 800 C. Such temperatures are encountered in the case of very highly loaded lamps, and even in the case of lamps not so highly loaded but employed in an environment where such temperatures are reached.
  • FIGURE 1 is an elevation of a quartz infrared lamp embodying seals in accordance with the invention
  • FIGURE 2 is a fragmentary elevation of one end of a lamp illustrating a step in the manufacture of the seal
  • FIGURE 3 is a fragmentary longitudinal cross section, on an enlarged scale, showing the completed seal
  • FIGURE 4 is a transverse cross section of the completed seal
  • FIGURE 5 is a transverse cross section of a modified form of seal.
  • the lamp illustrated therein may be, for example, of the quartz infrared lamp type disclosed and claimed in Patent 2,864,025 Foote et al. which is assigned to the same assignee as the 3,211,826 Patented Oct. 12, 1965 present invention.
  • the lamp comprises an elongated tubular envelope 1 consisting essentially of fused silica, preferably either clear crystal quartz or translucent sand quartz.
  • a helically coiled tungsten filament 2 extends axially the length of the envelope 1 and is suitably connected at its ends to lead in conductors 3 which are sealed through flattened press or pinch seal portions 4 at the ends of the envelope.
  • the elongated filament 2 is supported from the envelope wall at spaced points along its length by suitable support members 5, preferably tantalum discs of the type described and claimed in Patent 2,813,993 Fridrich which is assigned to the same assignee as the present invention.
  • the envelope 1 is preferably filled with an inert gas at substantial pressure, for example argon at nearly atmospheric pressure.
  • the actual hermetic seal between the quartz seal portion 4 and the lead-in conductor 3 is at an extremely thin intermediate ribbon or foliated portion 6, preferably of molybdenum.
  • the intermediate foliated portion 6 may be composed of a separate piece of molybdenum foil welded at opposite ends to the ends of respective inner and outer lead portions 7 and 8, or the said foliated portion 6 may be formed as an integral part of a molybdenum inner lead portion 7 by flattening a part of the inner lead portion to a thickness of from .0005 to .001 inch by longitudinal rolling, as disclosed and claimed in Patent 2,667,595 Noel et al. which is assigned to the assignee of the present invention.
  • the outer lead portion 8 is made of molybdenum, either as a separate piece welded to the intermediate foil portion 6 or as an integral part of the intermediate foil portion 6 and inner lead portion 7, a long life in excess of about 5,000 hours is obtained so long as the seal temperature does not rise above about 350 C.
  • the seal may fail in three ways which are, in general, characteristic of the temperature range.
  • the molybdenum lead is slowly oxidized progressively along the length of the seal until it leaks and air is admitted to the interior of the envelope 1 which causes the filament 2 to vaporize and blacken the bulb and eventually fail by burning through at some point.
  • the lamp may continue to burn for several hundred hours after the leak has started so that the useful life depends upon the degree of blackening that can be tolerated in a particular application.
  • seal life is materially increased by a combination of an outer lead 8 of material which resists oxidation at elevated temperatures above about 350 C., and a low melting glass 10 (FIGURE 3) filling the space or spaces 9 between the quartz and the part of the outer lead surrounded thereby.
  • a low melting glass 10 FOGURE 3
  • Particularly good results are obtained with the combination of a platinum outer lead 8 and a filling of a lead borate glass composition.
  • the lead borate glass is heavily loaded with fluorides, and still further improved results are obtained by the addition of thallium oxide to the glass composition.
  • FIGURE 2 A preferred method of introducing the glass composition into the cavities 9 (which may have a width of the order of a thousandth of an inch), is illustrated in FIGURE 2.
  • a small ring or bead 11 of the low melting glass is slipped over the end of the outer lead 8 and onto the upper end of the quartz seal portion 4.
  • Heat is then applied to the surface of the press or pinch seal 4, preferably by a small oxyhydrogen flame applied locally to the area enclosing the outer lead 8, to cause the bead 11 to melt and be drawn into the capillary spaces or passages 9 (FIGURE 3).
  • the low melting glass filling 10 serves as a liquid seal to prevent ingress of atmospheric oxygen to the molybdenum foil 6 through the spaces 9. At lower temperatures the glass 10 begins to harden and then cracks when the seal has become cool.
  • a composition, in parts by weight, of low melting lead borate glass which has given good results is as follows:
  • the amount of F1 is the total equivalent F: contributed by all fluorides in batch.
  • the glass head 11 may have a weight of about 3 mg. While the glass composition listed above has given the best results, some improvement may also be obtained with a simple lead borate, although it is preferred to improve the chemical and physical properties of the lead borate by the addition of the other ingredients in the above composition.
  • the composition may be varied somewhat by employing the ingredients, in part by Weight of a calculated analysis, in the following ranges:
  • the SiO increases the chemical durability.
  • the addition of Ca F (flu orspar) and ZnF provides a means of introducing F to the batch, in addition to that provided by the fluorides of lead, potassium, sodium and lithium, and the CaO and ZnO thus formed increase the chemical durability of the resulting glass.
  • the K 0, Na O, Li O and F contribute to a lowering of the softening point and melt viscosity.
  • the F is especially effective in this respect.
  • the thallic-oxide addition is particularly effective and unique in that it reduces the viscosity of the melt and broadens the temperature range of low viscosity.
  • FIG. 5 there is illustrated a modified form of seal wherein the tubular quartz seal portion 4' is evacuated and collapsed upon the lead-in conductor in accordance with a Well-known technique, instead of being pressed flat as in FIG. 4.
  • the opening or cavity 9 around the platinum outer lead 8 completely encircles the lead and is filled with the low melting glass 10'.
  • a seal for electrical devices comprising a member of fused silica and a lead-in conductor sealed in and extending through said member, said conductor including an intermediate foliated lead portion of molybdenum hermetically sealed Within said member and subject to oxidation at elevated temperatures above about 350 C., and an outer lead portion of platinum connected to and extending from said intermediate lead portion through said silica member to the exterior thereof with a slight space between the silica member and the part of said outer lead portion enclosed thereby, and a filling in said space of low melting lead borate glass which is molten at elevated temperatures above about 350 C.
  • a seal for electrical devices comprising a member of fused silica and a lead-in conductor sealed in and extending through said member, said conductor including an intermediate foliated lead portion of molybdenum hermetically sealed within said member and subject to oxidation at elevated temperatures above about 350 C., and an outer lead portion of platinum connected to and extending from said intermediate lead portion through said silica member to the exterior thereof with a slight space between the silica member and the part of said outer lead portion enclosed thereby, and a filling in said space of low melting lead borate glass which is molten at elevated temperatures above about 350 C.
  • said lead borate glass containing, by weight, approximately 2-5 parts SiO 70- parts PbO 12-15 parts B 0 1-5 parts T1 0 l-2 parts ZnO, .25-1 parts CaO, .25-1 parts K 0, 0.5 parts Na O, 0.5 parts U 0 and 1-4 parts F 3.
  • a seal for electrical devices comprising a member of fused silica and a lead-in conductor sealed in and extending through said member, said conductor including an intermediate foliated lead portion of molybdenum hermetically sealed within said member and subject to oxidation at elevated temperatures above about 350 C., and an outer lead portion of platinum connected to and extend ing from said intermediate lead portion through said silica member to the exterior thereof with a slight space between the silica member and the part of said outer lead portion enclosed thereby, and a filling in said space of low melting lead borate glass which is molten at elevated temperatures above about 350 C.
  • said lead borate glass containing, by weight, approximately 3.26 parts SiO 75.5 parts PbO, 13.6 parts B 0 1.34 parts ZnO, .62 parts K 0, .22 parts Na O, .29 parts Li O, .32 parts CaO, 1.92 parts T1 0 and 2.97 parts F 4.
  • a seal for electrical devices comprising a member of fused silica and a lead-in conductor sealed in and extending through said member, said conductor including an intermediate foliated lead portion of molybdenum hermetically sealed within said member and subject to oxidation at elevated temperatures above about 350 C., and an outer lead portion of platinum connected to and extending from said intermediate lead portion through said silica member to the exterior thereof with a slight space between the silica member and the part of said outer lead portion enclosed thereby, and a filling in said space of low melting lead borate glass which is molten at elevated temperatures above about 35 0 C.
  • said lead borate glass comprising by Weight, 65-85 parts PbO, 20 parts B 0 and about 1-4 parts of equivalent fluorine added as fluoride of at least one of the elements lead, zinc, potassium, sodium, lithium and calcium.
  • a seal for electrical devices comprising a member of fused silica and a lead-in conductor sealed in and extending through said member, said conductor including an intermediate foliated lead portion of molybdenum hermetically sealed Within said member and subject to oxidation at elevated temperatures above about 350 C., and an outer lead portion of platinum connected to and extending from said intermediate lead portion through said silica member to the exterior thereof with a slight space between the silica member and the part of said outer lead portion enclosed thereby, and a filling in said space of low melting lead borate glass which is molten at elevated temperatures above about 350 C. forming a liquid seal preventing ingress of atmospheric oxygen to said molybdenum intermediate lead portion, said lead borate glass comprising, by Weight, 6585 parts PbO, 10-20 parts B 0 and about 1-5 parts thallic oxide.
  • a seal for electrical devices comprising a member of fused silica and a lead-in conductor sealed in and extending through said member, said conductor including an intermediate foliated lead portion of molybdenum hermetically sealed within said member and subject to oxidation at elevated tempertaures above about 350 C., and an outer lead portion of platinum connected to and extending from said intermediate lead portion through said silica member to the exterior thereof with a slight space between the silica member and the part of said outer lead portion enclosed thereby, and a filling in said space of low melting lead borate glass which is molten at elevated temperatures above about 350 C.
  • said lead borate glass comprising by weight, 65-85 parts PbO, 1020 parts B 0 about 15 parts thallic oxide, and about 1-4 parts of equivalent fluorine added as fluoride of at least one of the elements lead, zinc, potassium, sodium, lithium and calcium.

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Description

Oct. 12, 1965 R. H. HOLCOMB ETAL 3,211,826
QUARTZ TO METAL SEAL Filed March 16, 1961 p 3 i Tiigll; 8 9 4 P/aT/hum "Lam/2776127279 H ouler lead lelaaaraie 4 Y 6 3 l0 3 7 5 Molybdenum fa/Z.
Fig. 5.
Invewlrovs:
Richard H. Holcomb, Gene 1. Thomasson,
United States Patent 3,211,826 QUARTZ T0 METAL SEAL Richard H. Holcomb, Cleveland, and Gene I. Thomasson,
Wicklitfe, Ohio, assignors to General Electric Company, a corporation of New York Filed Mar. 16, 1961, Ser. No. 96,128 6 Claims. (Cl. 17450.64)
This invention relates generally to seals of metallic lead-in conductors in quartz or fused silica for electrical devices comprising a sealed envelope containing electric energy translation means to which electric current is supplied through the lead-in conductor.
As a matter of convenience, and not by way of limitation, the invention will be referred to especially in connection with quartz infrared lamps which comprise a tubular envelope of quartz having an incandescible fila-. ment of coiled tungsten wire extending longitudinally therethrough and connected at its ends to lead-in conductors which are hermetically sealed through compressed or pinched seal portions at the ends of the envelope. The lead-in conductors are each generally composed of molybdenum wires having a very thin intermediate foliated or ribbon portion which is wetted to and hermetically sealed in the quartz seal portion. Molybdenum is preferred because of its high melting point whereby it can withstand the high temperatures required to fuse the quartz thereto.
Such seals are entirely satisfactory so long as the seal temperature does not exceed about 350 C. At higher temperatures, the seal fails much more rapidly due to oxidation of the molybdenum. For example, at temperatures not exceeding 350 C. the seal lasts for several thousand hours whereas at a temperature of about 400 C. the average life drops to a few hundred hours. There has been a need for seals which will remain hermetically tight at elevated temperatures.
Many attempts have been made to achieve that objective, including the application of various types of oxidation resistant coatings to the molybdenum leads. Various metals and combinations of metals which have been proposed for this purpose have relatively low melting points so that they melt during formation of the seal. Furthermore, in some cases such coatings prevent the formation of a hermetic seal.
Accordingly, it is an object of the invention to provide quartz to metal seals of increased life at elevated temperatures. More particularly, it is an object to provide a seal structure having a life which may be up to eight hundred times that of the prior art molybdenum-quartz seal in the temperature range of about 500 to 800 C. Such temperatures are encountered in the case of very highly loaded lamps, and even in the case of lamps not so highly loaded but employed in an environment where such temperatures are reached.
The invention will better be understood by reference to the following detailed description taken in conjunction with the drawing wherein:
FIGURE 1 is an elevation of a quartz infrared lamp embodying seals in accordance with the invention;
FIGURE 2 is a fragmentary elevation of one end of a lamp illustrating a step in the manufacture of the seal;
FIGURE 3 is a fragmentary longitudinal cross section, on an enlarged scale, showing the completed seal;
FIGURE 4 is a transverse cross section of the completed seal; and
FIGURE 5 is a transverse cross section of a modified form of seal.
Referring to FIGURE 1 of the drawing, the lamp illustrated therein may be, for example, of the quartz infrared lamp type disclosed and claimed in Patent 2,864,025 Foote et al. which is assigned to the same assignee as the 3,211,826 Patented Oct. 12, 1965 present invention. The lamp comprises an elongated tubular envelope 1 consisting essentially of fused silica, preferably either clear crystal quartz or translucent sand quartz. A helically coiled tungsten filament 2 extends axially the length of the envelope 1 and is suitably connected at its ends to lead in conductors 3 which are sealed through flattened press or pinch seal portions 4 at the ends of the envelope. The elongated filament 2 is supported from the envelope wall at spaced points along its length by suitable support members 5, preferably tantalum discs of the type described and claimed in Patent 2,813,993 Fridrich which is assigned to the same assignee as the present invention. The envelope 1 is preferably filled with an inert gas at substantial pressure, for example argon at nearly atmospheric pressure.
The actual hermetic seal between the quartz seal portion 4 and the lead-in conductor 3 is at an extremely thin intermediate ribbon or foliated portion 6, preferably of molybdenum. The intermediate foliated portion 6 may be composed of a separate piece of molybdenum foil welded at opposite ends to the ends of respective inner and outer lead portions 7 and 8, or the said foliated portion 6 may be formed as an integral part of a molybdenum inner lead portion 7 by flattening a part of the inner lead portion to a thickness of from .0005 to .001 inch by longitudinal rolling, as disclosed and claimed in Patent 2,667,595 Noel et al. which is assigned to the assignee of the present invention.
When the outer lead portion 8 is made of molybdenum, either as a separate piece welded to the intermediate foil portion 6 or as an integral part of the intermediate foil portion 6 and inner lead portion 7, a long life in excess of about 5,000 hours is obtained so long as the seal temperature does not rise above about 350 C. At elevated temperatures the seal may fail in three ways which are, in general, characteristic of the temperature range. At temperatures above about 350 C. and below about 450 C., the molybdenum lead is slowly oxidized progressively along the length of the seal until it leaks and air is admitted to the interior of the envelope 1 which causes the filament 2 to vaporize and blacken the bulb and eventually fail by burning through at some point. The lamp may continue to burn for several hundred hours after the leak has started so that the useful life depends upon the degree of blackening that can be tolerated in a particular application.
In the temperature range of about 450 C. to 640 C. failure of the seal is abrupt. It will be understood that because of the difference in coefiicient of expansion of the quartz and the relatively heavy outer lead portion 8, there is a slight space or passage between the quartz and the part of the outer lead portion 3 enclosed therein (as illustrated at 9 in FIGURE 4) through which atmospheric air can reach the outer end of the foil portion 6. In this temperature range, the oxide builds up at the end of the foil 6 before it can penetrate the seal, and cracks the quartz where it contacts the lead. The crack progresses to the exterior of the quartz whereupon the exposed foil oxidizes rapidly and fuses, usually cracking off a dishshaped piece of quartz. The hermetic seal remains intact but electrical continuity is broken. At temperatures above about 640 C., molybdenum oxidizes so rapidly that the outer lead portion 8 simply disintegrates, leaving the seal intact.
In accordance with the present invention, seal life is materially increased by a combination of an outer lead 8 of material which resists oxidation at elevated temperatures above about 350 C., and a low melting glass 10 (FIGURE 3) filling the space or spaces 9 between the quartz and the part of the outer lead surrounded thereby. Particularly good results are obtained with the combination of a platinum outer lead 8 and a filling of a lead borate glass composition. For improved results, the lead borate glass is heavily loaded with fluorides, and still further improved results are obtained by the addition of thallium oxide to the glass composition.
A preferred method of introducing the glass composition into the cavities 9 (which may have a width of the order of a thousandth of an inch), is illustrated in FIGURE 2. With the otherwise completed lamp in an upright position, a small ring or bead 11 of the low melting glass is slipped over the end of the outer lead 8 and onto the upper end of the quartz seal portion 4. Heat is then applied to the surface of the press or pinch seal 4, preferably by a small oxyhydrogen flame applied locally to the area enclosing the outer lead 8, to cause the bead 11 to melt and be drawn into the capillary spaces or passages 9 (FIGURE 3). During operation of the lamp, With the seal portions 4 at elevated temperatures, the low melting glass filling 10 serves as a liquid seal to prevent ingress of atmospheric oxygen to the molybdenum foil 6 through the spaces 9. At lower temperatures the glass 10 begins to harden and then cracks when the seal has become cool.
A composition, in parts by weight, of low melting lead borate glass which has given good results is as follows:
The amount of F1 is the total equivalent F: contributed by all fluorides in batch.
Lamps having seals of the type described, including platinum outer leads and a filling glass 10 of the composition stated above, and operated under conditions such that the seal temperature was above 700 C., had an average life of about 800 hours. This is in contrast to as little as one hour life of lamps with outer leads 8 of molybdenum, and fifty hours with outer leads 8 of platinum but no filling glass 10. It will be understood that it is not feasible to make the entire lead-in conductor 3 of platinum because the foliated portion, required for formation of a hermetic seal to quartz, would melt at the sealing temperature. The outer lead portion 8 of platinum does not melt because it conducts away the heat sufficiently rapidly on account of its relatively large size, which may be a wire of 30 mil diameter, for example. It is preferred that only sufficient of the low melting glass be used to fill the cavity 9; in the case of a 30 mil outer lead 8 the glass head 11 may have a weight of about 3 mg. While the glass composition listed above has given the best results, some improvement may also be obtained with a simple lead borate, although it is preferred to improve the chemical and physical properties of the lead borate by the addition of the other ingredients in the above composition. The composition may be varied somewhat by employing the ingredients, in part by Weight of a calculated analysis, in the following ranges:
The SiO increases the chemical durability. The addition of Ca F (flu orspar) and ZnF provides a means of introducing F to the batch, in addition to that provided by the fluorides of lead, potassium, sodium and lithium, and the CaO and ZnO thus formed increase the chemical durability of the resulting glass. The K 0, Na O, Li O and F contribute to a lowering of the softening point and melt viscosity. The F is especially effective in this respect. The thallic-oxide addition is particularly effective and unique in that it reduces the viscosity of the melt and broadens the temperature range of low viscosity.
The most significant physical properties of these glasses are very low softening point (about 320 C. for the preferred composition), melt viscosity and melt surface tension. Contributing largely to those three properties, especially the last two, are the large number of fluoride additions and the thallic-oxide addition.
In FIG. 5 there is illustrated a modified form of seal wherein the tubular quartz seal portion 4' is evacuated and collapsed upon the lead-in conductor in accordance with a Well-known technique, instead of being pressed flat as in FIG. 4. In this case the opening or cavity 9 around the platinum outer lead 8 completely encircles the lead and is filled with the low melting glass 10'.
What we claim as new and desire to secure by Letters Patent of the United States is:
1. A seal for electrical devices comprising a member of fused silica and a lead-in conductor sealed in and extending through said member, said conductor including an intermediate foliated lead portion of molybdenum hermetically sealed Within said member and subject to oxidation at elevated temperatures above about 350 C., and an outer lead portion of platinum connected to and extending from said intermediate lead portion through said silica member to the exterior thereof with a slight space between the silica member and the part of said outer lead portion enclosed thereby, and a filling in said space of low melting lead borate glass which is molten at elevated temperatures above about 350 C. forming a liquid seal preventing ingress of atmospheric oxygen to said molybdenum intermediate lead portion, said lead borate glass comprising, by weight, 65-85 parts PbO and 10-20 parts B 0 2. A seal for electrical devices comprising a member of fused silica and a lead-in conductor sealed in and extending through said member, said conductor including an intermediate foliated lead portion of molybdenum hermetically sealed within said member and subject to oxidation at elevated temperatures above about 350 C., and an outer lead portion of platinum connected to and extending from said intermediate lead portion through said silica member to the exterior thereof with a slight space between the silica member and the part of said outer lead portion enclosed thereby, and a filling in said space of low melting lead borate glass which is molten at elevated temperatures above about 350 C. forming a liquid seal preventing ingress of atmospheric oxygen to said molybdenum intermediate lead portion, said lead borate glass containing, by weight, approximately 2-5 parts SiO 70- parts PbO 12-15 parts B 0 1-5 parts T1 0 l-2 parts ZnO, .25-1 parts CaO, .25-1 parts K 0, 0.5 parts Na O, 0.5 parts U 0 and 1-4 parts F 3. A seal for electrical devices comprising a member of fused silica and a lead-in conductor sealed in and extending through said member, said conductor including an intermediate foliated lead portion of molybdenum hermetically sealed within said member and subject to oxidation at elevated temperatures above about 350 C., and an outer lead portion of platinum connected to and extend ing from said intermediate lead portion through said silica member to the exterior thereof with a slight space between the silica member and the part of said outer lead portion enclosed thereby, and a filling in said space of low melting lead borate glass which is molten at elevated temperatures above about 350 C. forming a liquid seal preventing ingress of atmospheric oxygen to said molybdenum intermediate lead portion, said lead borate glass containing, by weight, approximately 3.26 parts SiO 75.5 parts PbO, 13.6 parts B 0 1.34 parts ZnO, .62 parts K 0, .22 parts Na O, .29 parts Li O, .32 parts CaO, 1.92 parts T1 0 and 2.97 parts F 4. A seal for electrical devices comprising a member of fused silica and a lead-in conductor sealed in and extending through said member, said conductor including an intermediate foliated lead portion of molybdenum hermetically sealed within said member and subject to oxidation at elevated temperatures above about 350 C., and an outer lead portion of platinum connected to and extending from said intermediate lead portion through said silica member to the exterior thereof with a slight space between the silica member and the part of said outer lead portion enclosed thereby, and a filling in said space of low melting lead borate glass which is molten at elevated temperatures above about 35 0 C. forming a liquid seal preventing ingress of atmospheric oxygen to said molybdenum intermediate lead portion, said lead borate glass comprising by Weight, 65-85 parts PbO, 20 parts B 0 and about 1-4 parts of equivalent fluorine added as fluoride of at least one of the elements lead, zinc, potassium, sodium, lithium and calcium.
5. A seal for electrical devices comprising a member of fused silica and a lead-in conductor sealed in and extending through said member, said conductor including an intermediate foliated lead portion of molybdenum hermetically sealed Within said member and subject to oxidation at elevated temperatures above about 350 C., and an outer lead portion of platinum connected to and extending from said intermediate lead portion through said silica member to the exterior thereof with a slight space between the silica member and the part of said outer lead portion enclosed thereby, and a filling in said space of low melting lead borate glass which is molten at elevated temperatures above about 350 C. forming a liquid seal preventing ingress of atmospheric oxygen to said molybdenum intermediate lead portion, said lead borate glass comprising, by Weight, 6585 parts PbO, 10-20 parts B 0 and about 1-5 parts thallic oxide.
6. A seal for electrical devices comprising a member of fused silica and a lead-in conductor sealed in and extending through said member, said conductor including an intermediate foliated lead portion of molybdenum hermetically sealed within said member and subject to oxidation at elevated tempertaures above about 350 C., and an outer lead portion of platinum connected to and extending from said intermediate lead portion through said silica member to the exterior thereof with a slight space between the silica member and the part of said outer lead portion enclosed thereby, and a filling in said space of low melting lead borate glass which is molten at elevated temperatures above about 350 C. forming a liquid seal preventing ingress of atmospheric oxygen to said molybdenum intermediate lead portion, said lead borate glass comprising by weight, 65-85 parts PbO, 1020 parts B 0 about 15 parts thallic oxide, and about 1-4 parts of equivalent fluorine added as fluoride of at least one of the elements lead, zinc, potassium, sodium, lithium and calcium.
References Cited by the Examiner UNITED STATES PATENTS 2,114,869 4/38 Bol et al 49-92.5 XR 2,177,685 10/39 Bol et al 49-92.5 XR 2,242,774 5/41 Brumley 49-92.5 XR 2,305,901 12/42 Scharfnagel 49-92.5 XR 2,508,354 5/50 Brinson 49-92.5 2,583,388 1/52 Nelson et al. 49-92.5 2,716,584 8/55 Retzer 49-81 2,739,901 3/56 Herold et a1. 106-53 2,803,926 8/57 Ekkers 49-92.5 XR 2,876,120 3/59 Machlan 49-77 2,951,167 8/60 Kegg et al 161-196 3,012,167 12/61 Poole 49-92.5 XR 3,030,541 4/62 Hanlet 252-3016 FOREIGN PATENTS 1,125,534 9/47 Australia.
520,486 6/53 Belgium.
799,097 7/58 Great Britain.
OTHER REFERENCES I.B.M. Technical Disclosure Bulletin, vol. 3, No. 5, October 1960, 2 pp.
Ceramic Age, May 1949, pp. 260-265, Invitation to Glass Technology, by Alexis G. Pincus.
Handbook of Glass Manufacture, by Fay Tooley, vol. II, published by Ogden Publishing Co., West 42nd Street, New York 36, N.Y., pp. 187 to 219.
ALEXANDER WYMAN, Primary Examiner. EARL M. BERGERT, ARTHUR P. KENT, Examiners.

Claims (1)

1. A SEAL FOR ELECTRICAL DEVICES COMPRISING A MEMBER OF FUSED SILICA AND A LEAD-IN CONDUCTOR SEALED IN AND EXTENDING THROUGH SAID MEMBER, SAID CONDUCTOR INCLUDING AN INTERMEDIATE FOLIATED LEAD PORTION OF MOLYBDENUM HERMETICALLY SEALED WITHIN SAID MEMBER AND SUBJECT TO OXIDATION AT ELEVATED TEMPERATURES ABOVE ABOUT 350*C., AND AN OUTER LEAD PORTION OF PLATINUM CONNECTED TO AND EXTENDING FROM SAID INTERMEDIATE LEAD PORTION THROUGH SAID SILICA MEMBER TO THE EXTERIOR THEREOF WITH A SLIGHT SPACE BETWEEN THE SILICA MEMBER AND THE PART OF SAID OUTER LEAD PORTION ENCLOSED THEREBY, AND A FILLING IN SAID SPACE OF LOW MELTING
US96128A 1961-03-16 1961-03-16 Quartz to metal seal Expired - Lifetime US3211826A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
FR1317782D FR1317782A (en) 1961-03-16
US96128A US3211826A (en) 1961-03-16 1961-03-16 Quartz to metal seal
ES0274377A ES274377A1 (en) 1961-03-16 1962-02-07 Quartz to metal seal
GB6726/62A GB946094A (en) 1961-03-16 1962-02-21 Improvements in quartz to metal seals

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US96128A US3211826A (en) 1961-03-16 1961-03-16 Quartz to metal seal

Publications (1)

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US3211826A true US3211826A (en) 1965-10-12

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Country Status (4)

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US (1) US3211826A (en)
ES (1) ES274377A1 (en)
FR (1) FR1317782A (en)
GB (1) GB946094A (en)

Cited By (31)

* Cited by examiner, † Cited by third party
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US3408212A (en) * 1965-06-04 1968-10-29 Fairchild Camera Instr Co Low melting oxide glass
US3420683A (en) * 1962-12-17 1969-01-07 Nippon Electric Co Low melting glass
US3425817A (en) * 1964-09-16 1969-02-04 Nippon Electric Co Low melting point devitrified glass and method
US3442993A (en) * 1962-12-17 1969-05-06 Nippon Electric Co Vitreous material for use in semiconductor devices
US3455708A (en) * 1964-03-18 1969-07-15 Physical Sciences Corp Ceramic material
US3515929A (en) * 1968-01-24 1970-06-02 Westinghouse Electric Corp Short arc lamp seal
US3515420A (en) * 1968-09-26 1970-06-02 Gen Electric Quartz to metal seal for electrical devices
US3668391A (en) * 1970-08-19 1972-06-06 Sylvania Electric Prod Tungsten halogen lamp having improved seal of molybdenum aluminide
US3742117A (en) * 1972-05-11 1973-06-26 Gen Electric Oxidation-resistant seal
US3753026A (en) * 1969-12-13 1973-08-14 Philips Corp Quartz lamp seal
US3776764A (en) * 1969-08-25 1973-12-04 Nippon Electric Glass Co METHOD FOR SEALING GLASS, METAL OR CERAMICS WITH MIXTURE OF PbO GLASS AND {62 -EUCRYPTITE CONTAINING GLASS
US3899708A (en) * 1974-04-10 1975-08-12 Gte Sylvania Inc Noise free incandescent lamp
US3991337A (en) * 1974-05-17 1976-11-09 U.S. Philips Corporation Electric lamp
US4254300A (en) * 1978-11-29 1981-03-03 U.S. Philips Corporation Electric lamp
US4273585A (en) * 1980-04-21 1981-06-16 Exxon Research & Engineering Co. Sealing glass
US4492814A (en) * 1984-01-04 1985-01-08 Gte Products Corporation Solder glass and electrical device employing same
US4493944A (en) * 1984-01-04 1985-01-15 Gte Products Corporation Solder glass and electrical device employing same
US4521641A (en) * 1984-01-04 1985-06-04 Gte Products Corporation Solder glass and electrical device employing the same
US4539509A (en) * 1982-12-17 1985-09-03 General Electric Company Quartz to metal seal
EP0245734A2 (en) * 1986-05-12 1987-11-19 Patent-Treuhand-Gesellschaft für elektrische Glühlampen mbH Electric lamp
US4746977A (en) * 1987-03-12 1988-05-24 Remote Technology Corporation Remotely operated steerable vehicle with improved arrangement for remote steering
EP0492189A2 (en) * 1990-12-25 1992-07-01 Ushiodenki Kabushiki Kaisha Electric lamp with foil seal construction and method for its manufacture
EP0615279A1 (en) * 1993-03-08 1994-09-14 Koninklijke Philips Electronics N.V. Electric lamp
EP0818805A2 (en) * 1996-07-12 1998-01-14 Koito Manufacturing Co., Ltd Discharge lamp ARC tube and method of producing the same
US5847510A (en) * 1996-08-21 1998-12-08 Patent-Treuhand-Gesellschaft Fuer Elektrische Gluehlampen Mbh High pressure discharge bulb
WO2009056163A1 (en) * 2007-10-29 2009-05-07 Osram Gesellschaft mit beschränkter Haftung Electric lamp having a light bulb and method for producing an electric lamp
US20100021147A1 (en) * 2008-07-28 2010-01-28 Ushio Denki Kabushiki Kaisha Filament lamp
US20180035721A1 (en) * 2013-03-15 2018-02-08 Healthier Choices Management Corp Electronic cigarette
US20180049466A1 (en) * 2013-03-15 2018-02-22 Healthier Choices Management Corp Electronic cigarette
US20190274355A1 (en) * 2018-03-09 2019-09-12 Healthier Choices Management Corp Electronic cigarette
US11064732B2 (en) * 2013-03-15 2021-07-20 Healthier Choices Management Corp. Electronic vaporizer cartridge with encased heat source

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US2242774A (en) * 1938-10-12 1941-05-20 Westinghouse Electric & Mfg Co Seal for discharge lamps
US2305901A (en) * 1940-01-13 1942-12-22 Scharfnagel Rudolf Electron tube
US2508354A (en) * 1944-10-21 1950-05-23 Bendix Aviat Corp Spark plug or the like
US2583388A (en) * 1947-05-01 1952-01-22 Gen Electric Conducting seal for high-pressure lamps
US2716584A (en) * 1953-12-16 1955-08-30 Westinghouse Electric Corp Double hermetic seal for gaseous discharge lamps
US2739901A (en) * 1952-07-14 1956-03-27 Paul G Herold Ruthenium containing glasses and stains
US2803926A (en) * 1954-05-15 1957-08-27 Patelhold Patentverwertung Method of sealing electrode lead-in conductors to the wall of electric discharge tube and electrode collar produced thereby
GB799097A (en) * 1954-05-15 1958-07-30 Patelhold Patentverwertung Improvements in sealing conductors through glass-walled electron discharge devices
US2876120A (en) * 1954-12-03 1959-03-03 Owens Corning Fiberglass Corp Glass composition
US2951167A (en) * 1958-06-26 1960-08-30 Kimble Glass Co Support means for mounting color-control element in glass portion of cathode-ray tube envelope
US3012167A (en) * 1959-07-14 1961-12-05 Gen Electric Co Ltd Envelopes for electrical devices
US3030541A (en) * 1955-12-30 1962-04-17 Electronique & Automatisme Sa Electroluminescent compositions

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US2177685A (en) * 1934-10-17 1939-10-31 Gen Electric Composition of matter
US2114869A (en) * 1935-08-31 1938-04-19 Gen Electric Quartz-to-metal seal
US2242774A (en) * 1938-10-12 1941-05-20 Westinghouse Electric & Mfg Co Seal for discharge lamps
US2305901A (en) * 1940-01-13 1942-12-22 Scharfnagel Rudolf Electron tube
US2508354A (en) * 1944-10-21 1950-05-23 Bendix Aviat Corp Spark plug or the like
US2583388A (en) * 1947-05-01 1952-01-22 Gen Electric Conducting seal for high-pressure lamps
US2739901A (en) * 1952-07-14 1956-03-27 Paul G Herold Ruthenium containing glasses and stains
US2716584A (en) * 1953-12-16 1955-08-30 Westinghouse Electric Corp Double hermetic seal for gaseous discharge lamps
US2803926A (en) * 1954-05-15 1957-08-27 Patelhold Patentverwertung Method of sealing electrode lead-in conductors to the wall of electric discharge tube and electrode collar produced thereby
GB799097A (en) * 1954-05-15 1958-07-30 Patelhold Patentverwertung Improvements in sealing conductors through glass-walled electron discharge devices
US2876120A (en) * 1954-12-03 1959-03-03 Owens Corning Fiberglass Corp Glass composition
US3030541A (en) * 1955-12-30 1962-04-17 Electronique & Automatisme Sa Electroluminescent compositions
US2951167A (en) * 1958-06-26 1960-08-30 Kimble Glass Co Support means for mounting color-control element in glass portion of cathode-ray tube envelope
US3012167A (en) * 1959-07-14 1961-12-05 Gen Electric Co Ltd Envelopes for electrical devices

Cited By (41)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3420683A (en) * 1962-12-17 1969-01-07 Nippon Electric Co Low melting glass
US3442993A (en) * 1962-12-17 1969-05-06 Nippon Electric Co Vitreous material for use in semiconductor devices
US3455708A (en) * 1964-03-18 1969-07-15 Physical Sciences Corp Ceramic material
US3425817A (en) * 1964-09-16 1969-02-04 Nippon Electric Co Low melting point devitrified glass and method
US3408212A (en) * 1965-06-04 1968-10-29 Fairchild Camera Instr Co Low melting oxide glass
US3515929A (en) * 1968-01-24 1970-06-02 Westinghouse Electric Corp Short arc lamp seal
US3515420A (en) * 1968-09-26 1970-06-02 Gen Electric Quartz to metal seal for electrical devices
US3776764A (en) * 1969-08-25 1973-12-04 Nippon Electric Glass Co METHOD FOR SEALING GLASS, METAL OR CERAMICS WITH MIXTURE OF PbO GLASS AND {62 -EUCRYPTITE CONTAINING GLASS
US3753026A (en) * 1969-12-13 1973-08-14 Philips Corp Quartz lamp seal
US3668391A (en) * 1970-08-19 1972-06-06 Sylvania Electric Prod Tungsten halogen lamp having improved seal of molybdenum aluminide
US3742117A (en) * 1972-05-11 1973-06-26 Gen Electric Oxidation-resistant seal
US3899708A (en) * 1974-04-10 1975-08-12 Gte Sylvania Inc Noise free incandescent lamp
US3991337A (en) * 1974-05-17 1976-11-09 U.S. Philips Corporation Electric lamp
US4254300A (en) * 1978-11-29 1981-03-03 U.S. Philips Corporation Electric lamp
US4273585A (en) * 1980-04-21 1981-06-16 Exxon Research & Engineering Co. Sealing glass
US4539509A (en) * 1982-12-17 1985-09-03 General Electric Company Quartz to metal seal
US4492814A (en) * 1984-01-04 1985-01-08 Gte Products Corporation Solder glass and electrical device employing same
US4493944A (en) * 1984-01-04 1985-01-15 Gte Products Corporation Solder glass and electrical device employing same
US4521641A (en) * 1984-01-04 1985-06-04 Gte Products Corporation Solder glass and electrical device employing the same
EP0245734A2 (en) * 1986-05-12 1987-11-19 Patent-Treuhand-Gesellschaft für elektrische Glühlampen mbH Electric lamp
EP0245734A3 (en) * 1986-05-12 1989-11-02 Patent-Treuhand-Gesellschaft Fur Elektrische Gluhlampen Mbh Electric lamp
US4766346A (en) * 1986-05-12 1988-08-23 Patent Treuhand Gesellschaft fur elektrische Glulampen mbH Lamp with low-toxicity, molybdenum-compatible sealing glass
US4746977A (en) * 1987-03-12 1988-05-24 Remote Technology Corporation Remotely operated steerable vehicle with improved arrangement for remote steering
EP0492189A2 (en) * 1990-12-25 1992-07-01 Ushiodenki Kabushiki Kaisha Electric lamp with foil seal construction and method for its manufacture
EP0492189A3 (en) * 1990-12-25 1992-12-02 Ushiodenki Kabushiki Kaisha Electric lamp with foil seal construction and method for its manufacture
US5310374A (en) * 1990-12-25 1994-05-10 Ushiodenki Kabushiki Kaisha Electric lamp with foil seal construction and method of producing the same
EP0615279A1 (en) * 1993-03-08 1994-09-14 Koninklijke Philips Electronics N.V. Electric lamp
US5993279A (en) * 1996-07-12 1999-11-30 Koito Manufacturing Co., Ltd. Discharge lamp arc tube and method of producing the same
EP0818805A3 (en) * 1996-07-12 1998-03-25 Koito Manufacturing Co., Ltd Discharge lamp ARC tube and method of producing the same
US5877590A (en) * 1996-07-12 1999-03-02 Koito Manufacturing Co., Ltd. Discharge lamp arc tube and method of producing the same
EP0818805A2 (en) * 1996-07-12 1998-01-14 Koito Manufacturing Co., Ltd Discharge lamp ARC tube and method of producing the same
US5847510A (en) * 1996-08-21 1998-12-08 Patent-Treuhand-Gesellschaft Fuer Elektrische Gluehlampen Mbh High pressure discharge bulb
WO2009056163A1 (en) * 2007-10-29 2009-05-07 Osram Gesellschaft mit beschränkter Haftung Electric lamp having a light bulb and method for producing an electric lamp
US8488953B2 (en) * 2008-07-28 2013-07-16 Ushio Denki Kabushiki Kaisha Filament lamp
US20100021147A1 (en) * 2008-07-28 2010-01-28 Ushio Denki Kabushiki Kaisha Filament lamp
US20180035721A1 (en) * 2013-03-15 2018-02-08 Healthier Choices Management Corp Electronic cigarette
US20180049466A1 (en) * 2013-03-15 2018-02-22 Healthier Choices Management Corp Electronic cigarette
US20190075847A1 (en) * 2013-03-15 2019-03-14 Healthier Choices Management Corp. Electronic cigarette
US20200221763A1 (en) * 2013-03-15 2020-07-16 Healthier Choices Management Corp Electronic cigarette
US11064732B2 (en) * 2013-03-15 2021-07-20 Healthier Choices Management Corp. Electronic vaporizer cartridge with encased heat source
US20190274355A1 (en) * 2018-03-09 2019-09-12 Healthier Choices Management Corp Electronic cigarette

Also Published As

Publication number Publication date
GB946094A (en) 1964-01-08
FR1317782A (en) 1963-05-08
ES274377A1 (en) 1962-06-16

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