CN101374776A - Process for producing glass composition for lamp, glass composition for lamp, and lamp - Google Patents

Process for producing glass composition for lamp, glass composition for lamp, and lamp Download PDF

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Publication number
CN101374776A
CN101374776A CNA2007800035687A CN200780003568A CN101374776A CN 101374776 A CN101374776 A CN 101374776A CN A2007800035687 A CNA2007800035687 A CN A2007800035687A CN 200780003568 A CN200780003568 A CN 200780003568A CN 101374776 A CN101374776 A CN 101374776A
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lamp
glass composition
glass
manufacture method
composition
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元家淳志
仁熊泰郎
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Panasonic Holdings Corp
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Matsushita Electric Industrial Co Ltd
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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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J61/00—Gas-discharge or vapour-discharge lamps
    • H01J61/02—Details
    • H01J61/30—Vessels; Containers
    • H01J61/302—Vessels; Containers characterised by the material of the vessel
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/24—Manufacture or joining of vessels, leading-in conductors or bases
    • H01J9/245—Manufacture or joining of vessels, leading-in conductors or bases specially adapted for gas discharge tubes or lamps
    • H01J9/247—Manufacture or joining of vessels, leading-in conductors or bases specially adapted for gas discharge tubes or lamps specially adapted for gas-discharge lamps

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Glass Compositions (AREA)
  • Glass Melting And Manufacturing (AREA)
  • Vessels And Coating Films For Discharge Lamps (AREA)

Abstract

A process for producing a glass composition for lamps which includes a melting step in which a raw-material mixture containing an oxide of a given element and a hydroxide of the given element in an oxide/hydroxide proportion of from 1/3 to 1 by mole is melted and brought into a vitreous state. In the melting step, the raw-material mixture is heated so that the hydroxide undergoes a decomposition reaction to generate a gas comprising at least either of H2O and H2. Thus, a glass reduced in bubble inclusions can be produced without generating any harmful gas.

Description

The manufacture method of glass composition for lamp, glass composition for lamp and lamp
Technical field
The present invention relates to glass composition for lamp manufacture method, use the glass composition for lamp of this method manufacturing, the lamp that uses this glass composition for lamp to make.
Background technology
Usually, in as the back lighting of liquid crystal TV, PC, use luminescent lamp as light source with the permeation type liquid crystal display element of indicating meter etc.The luminescent lamp that back lighting is used has and the general illumination essentially identical structure of luminescent lamp, but the caliber of glass bulb (glass bulb) is littler, wall thickness is thinner.Therefore, in the luminescent lamp that such back lighting is used, use the hard glass (being designated hereinafter simply as " pyrex ") of the borosilicate acids of physical strength height, electrical insulating property excellence.
Yet if having bubble in the glass of glass bulb, the physical strength of this glass bulb reduces and apt to cause breakage.In the glass bulb of particularly little at caliber and wall thickness, it is very serious problem that such intensity reduces.Therefore, add arsenic or antimony in recent years in the glass as finings, thereby from glass, remove bubble (fining glass).
But above-mentioned arsenic or antimony are that environment is had dysgenic carrying capacity of environment material.Therefore, the glass that has added arsenic or antimony is unsuitable for recycling.In addition, add the glass of arsenic or antimony, should be noted that the operation in manufacturing works or waste treatment factory, also needed a lot of very big equipment to carry out the harmless treatment etc. of etching waste liquor.
In order to address this is that, a kind of manufacture method of glass is disclosed in the patent documentation 1, wherein add the SO that contains of significant quantity 3, Cl, F salt as finings.In this method, do not add the carrying capacity of environment material, can obtain the few glass of bubble.Known in addition, by in glass, adding NaNO 3Or KNO 3In nitrate, thereby can obtain clarifying effect.
Patent documentation 1: TOHKEMY 2004-284949 communique
Summary of the invention
But the manufacture method of patent documentation 1 can produce harmful gases such as sulfide-based gas or halogen gas in the glass melting operation.The generation of these obnoxious flavoures worsens the operating environment of making glass, so be unfavorable.
In addition, the situation of interpolation nitrate also can produce harmful nitrose gas (NO x), thereby the operating environment of making glass is worsened, so be unfavorable.
The manufacture method that the purpose of this invention is to provide a kind of glass composition for lamp wherein, does not produce deleterious gas, and can make the few glass of entrapped air pockets.In addition, another object of the present invention provides and does not produce the few glass composition for lamp of bubble that deleterious gas can be made, and the lamp that forms with this glass composition for lamp, be difficult to breakage.
In order to achieve the above object, the manufacture method of the glass composition for lamp of an embodiment of the invention is characterised in that,
Comprise with the raw mix fusion being the fusion operation of vitreousness, described raw mix has been for having added the mixture of the oxyhydroxide of the oxide compound of element-specific and described element-specific with the mol ratio of oxide/hydroxide=1/3～1,
In above-mentioned fusion operation, heating above-mentioned raw materials mixture, so that above-mentioned oxyhydroxide generation decomposition reaction, thereby comprise H from above-mentioned oxyhydroxide generation 2O or H 2At least a gas.
The glass composition for lamp of the glass composition for lamp of an embodiment of the invention for making by the manufacture method of above-mentioned glass composition for lamp is characterized in that, when test portion thickness is 2mm, at wavelength zone 3620cm -1Near the mnm. of infrared rays transmitance is 3.0～4.5%.
The lamp of an embodiment of the invention is characterised in that to possess the glass bulb that forms with above-mentioned glass composition for lamp.
The manufacture method of glass composition for lamp of the present invention has following effect, and the oxyhydroxide generation from element-specific in the fusion operation comprises H 2O or H 2At least a gas, thereby do not produce obnoxious flavour and can make the few glass of bubble.Below this effect is elaborated.
The inventor etc. have repeated various researchs, found that, the part of the oxide compound by the element-specific of will add in the raw mix is replaced as the oxyhydroxide of above-mentioned element-specific, thereby making the fusion of above-mentioned raw materials mixture is in the fusion operation of vitreousness, produce gas from above-mentioned oxyhydroxide, utilize the bubble in this gas removal glass melting liquid, and obtain clarifying effect.The gas that produces from above-mentioned oxyhydroxide is the gas that produces the decomposition reaction of above-mentioned oxyhydroxide, thereby comprises H 2O or H 2In at least a.Under 500～1000 ℃ of the temperature ranges of vitrifying reaction beginning, the decomposition reaction of above-mentioned oxyhydroxide takes place, thereby obtain clarifying effect.
So the bubble that exists in the glass is the CO that is produced when raw mix is melt into vitreousness 2From glass melting liquid, do not eliminate and remaining bubble Deng gas.CO particularly 2Bubble be minor diameter, buoyancy is little and be difficult to float from glass melting liquid, thereby does not eliminate from glass melting liquid and remain in the glass easily.
In order to remove the bubble of this minor diameter, in the manufacture method of lantern pane of the present invention, produce from the oxyhydroxide of element-specific and to comprise H 2O or H 2Gas.This comprises H 2O or H 2The diameter of bubble of gas compare CO 2Diameter in bubble is big, thereby buoyancy is bigger, removes from glass melting liquid easily, is difficult to remain in the glass.Thereby, comprise H 2O or H 2The bubble of gas, from glass melting liquid, carried CO during come-up secretly 2In bubble, therefore comprise CO 2Deng the bubble of minor diameter also can from glass, remove.
But, comprise H if in glass melting liquid, produce 2O or H 2Gas, have in the glass problem of residual moisture easily so.If the moisture remaining quantity is many in the glass, the gasification of this moisture causes foaming again (boiling again) easily when then heating, if with such glass manufacturing lamp, is then partly caused at superheated by burner etc. during hot-work and foams and become the reason of slow gas leakage or crackle.
For this problem, discoveries such as the inventor are defined in by the ratio of mixture with oxide compound and oxyhydroxide in 1/3～1 the scope, thereby can obtain sufficient clarifying effect, are not easy to cause foaming more simultaneously.
Above-mentioned ratio of mixture comprises H greater than under 1 the situation 2O or H 2The generation of gas few, thereby clarifying effect is insufficient.On the other hand, above-mentioned ratio of mixture causes foaming more easily less than under 1/3 the situation during hot-work, use and be not suitable for lamp.
In addition,, can consider boron (B), aluminium (Al) and calcium (Ca) etc., mean that at this moment the oxyhydroxide of above-mentioned element-specific is respectively H as element-specific 3BO 3, Al (OH) 3And Ca (OH) 2
In addition, in the oxyhydroxide of the present invention, comprise that not only the oxyhydroxide of narrow sense promptly has the compound of hydroxyl, comprise that also generalized oxyhydroxide promptly has the compound of protium and oxygen element.For example, not only comprise Al (OH) 3And Ca (OH) 2Etc. the oxyhydroxide of narrow sense, also comprise as H 3BO 3(can souvenir be B (OH) also 3) generalized oxyhydroxide.
The manufacture method of glass composition for lamp of the present invention, above-mentioned oxide compound and oxyhydroxide are added in the above-mentioned raw materials mixture, so that the content of the above-mentioned element-specific in the glass composition for lamp, count under the situation of 8～17mol% with the oxide compound conversion, the stopping property that can obtain meltbility and lead-in wire is good, and is difficult to take place the glass composition for lamp of phase-splitting.
The manufacture method of glass composition for lamp of the present invention, above-mentioned oxyhydroxide is added in the above-mentioned raw materials mixture, so that the content of the above-mentioned element-specific in the glass composition for lamp, convert with oxide compound and to count under the situation of 5～10.5mol%, can obtain that bubble is few, be difficult to cause the glass composition for lamp of foaming again during hot-work.
The manufacture method of glass composition for lamp of the present invention, glass composition for lamp are that pyrex, element-specific are under the situation of boron, and clarifying effect is remarkable especially.For example, the oxyhydroxide of boron is H 3BO 3, in 300～800 ℃ broad temperature range, comprise H by the decomposition reaction generation 2O or H 2At least a gas, thereby in the fusion operation, carry out temperature treatment easily.H 3BO 3Decomposition reaction (formula 1) described as follows and (formula 2) expression.
2H 3B 3→ 3H 2O+B 2O 3(formula 1)
2H 3BO 3→ 3/2O 2+ 3H 2+ B 2O 2(formula 2)
In addition, by using cheap H 3BO 3, also have the effect of making glass with low cost, even and add a large amount of H 3BO 3Glass can be not painted yet effect.
In addition, the pyrex among the present invention is the glass of Young's modulus or Vickers hardness height and physical strength excellence, particularly, is meant in oxide compound and converts, and contains B 2O 3The glass of 6～20mol%.
Thermal expansivity (the α of glass composition for lamp of the present invention 30/380) be 34 * 10 -7/ K～43 * 10 -7During/K, perhaps be 43 * 10 -7/ K～55 * 10 -7During/K, bring into play following effect.
In general, with in the lamp, use can tolerate the lead-in wire by the pyritous tungsten system or the Kovar alloy system of discharge generation in back lighting.Therefore, for the reliability of the gas-tight seal that improves lead-in wire, preferably make the thermal expansivity of glass composition for lamp approach the thermal expansivity of tungsten or Kovar alloy.
Thermal expansivity (α 30/380) be 34 * 10 -7/ K～43 * 10 -7During/K, with the thermal expansivity of tungsten making line be equal extent, chemical durability is also high, therefore the reliability height of the gas-tight seal of lead-in wire.
Thermal expansivity (α 30/380) be 43 * 10 -7/ K～55 * 10 -7During/K, with the thermal expansivity of Kovar alloy making line be equal extent, chemical durability is also high, therefore the reliability height of the gas-tight seal of lead-in wire.
Light fixture of the present invention is equipped with the glass bulb that is formed by above-mentioned glass composition for lamp.Therefore, bubble is few in the glass of glass bulb, and lamp is not easy breakage.
Description of drawings
Fig. 1 illustrates the composition and the characteristic of the glass composition that an embodiment of the invention relate to.
Fig. 2 is the synoptic diagram that the major portion structure of the cold-cathode fluorescence lamp that an embodiment of the invention relate to is shown.
Fig. 3 illustrates the composition and the characteristic of the glass composition that comparative example relates to.
Fig. 4 illustrates glass composition that an embodiment of the invention relate at 2800cm -1～3800cm -1Infrared rays transmitance in the scope.
Fig. 5 illustrates glass composition that an embodiment of the invention relate at 3600cm -1～3800cm -1Infrared rays transmitance in the scope.
Nomenclature
1 lamp
Embodiment
Manufacture method and lamp based on the glass composition for lamp in the description of drawings embodiments of the present invention, glass composition for lamp.
(explanation of glass composition for lamp)
The composition of the glass composition in the present embodiment is shown in the embodiment among Fig. 1 1～5.In addition, " % " expression " mol% " among Fig. 1.
The composition of glass composition of the present invention is not limited to the composition shown in the embodiment 1～5, but in order to ensure the characteristic as glass composition for lamp, preferably converts in oxide compound and be essentially SiO 2: 55～75mol%, Al 2O 3: 1～10mol%, B 2O 3+ H 3BO 3: 8～17mol%, Li 2O+Na 2O+K 2O:0～12mol%, Li 2O:0～5mol%, Na 2O:0～8mol%, K 2O:0～12mol%, MgO:0.5～5mol%, CaO:0.5～10mol%, SrO:0～8mol%, BaO:0～10mol%, CeO 2: 0.01～2mol%, Fe 2O 3: 0～0.2mol%, SnO:0.01～5mol%.
In addition, in the present embodiment, boron (B) contained in the glass composition comprises, add boron in the raw mix to as the oxide compound of boron, and add boron in the raw mix to as the oxyhydroxide of boron, but in order to distinguish them, for the boron that adds as oxide compound, souvenir is " B 2O 3"; For the boron that adds as oxyhydroxide, souvenir is " H 3BO 3".They are all the same in Fig. 1 and Fig. 3 described later.
Therefore, be recited as B in above-mentioned 2O 3+ H 3BO 3: the meaning of 8～17mol% is meant, in the glass composition, and the total amount of boron that adds as oxide compound and the boron that adds as oxyhydroxide, the value that converts with oxide compound is 8～17mol%.
What glass composition for lamp of the present invention was stipulated as described above the reasons are as follows.
SiO 2For forming the composition of glass skeleton, its content is preferably the scope of 55～75mol%.If be less than 55mol%, then thermal expansivity becomes too high, and chemical durability also worsens.On the other hand, if more than 75mol%, then thermal expansivity became low, shaped the difficulty that becomes.
Al 2O 3Be for the purpose of the weathering resistance that improves glass and increased devitrification resistance and the composition that adds, its content is preferably the scope of 1～10mol%.If be less than 1mol%, then be difficult to obtain above-mentioned effect.On the other hand, if more than 10mol%, then glass melting deterioration.Its content is preferably 2～7mol% especially.
B 2O 3It is the essential composition of the present embodiment that adds in order to improve glass melting, regulate the coefficient of expansion and to regulate the purpose of viscosity.
H 3BO 3It is the essential composition of the present embodiment that adds in order to improve glass melting, regulate the coefficient of expansion, regulate viscosity and to promote the purpose of clarifying effect.
B 2O 3+ H 3BO 3Be preferably the scope of 8～17mol%.If B 2O 3+ H 3BO 3Be less than 8mol%, then glass melting deterioration, the viscosity and the coefficient of expansion rise and make the sealing of lead-in wire become difficult simultaneously.On the other hand, if more than 17mol%, cause that then the glass phase-splitting makes the making of glass become difficult.Total content is preferably 10～16mol% especially.
With B 2O 3/ H 3BO 3=1/3～1 mol ratio is added B 2O 3And H 3BO 3If above-mentioned mol ratio is less than 1/3, then luminescent lamp causes foaming again by burner in overheated portion when hot-work, becomes the reason of slow gas leakage or crackle.In addition, if above-mentioned mol ratio greater than 1, then the clarifying effect of glass becomes insufficient.
Li 2O, Na 2O and K 2The alkalimetal oxide of O adds for the viscosity that reduces glass, the purpose that improves melt processable.Its content is preferably the scope of 0～10mol%.If more than 10mol%, then the thermal expansivity of glass becomes excessive.In addition because the stripping from glass easily of alkali composition, if thereby use this glass to make luminescent lamp, then the reaction of glass and fluor or mercury reduces the optical throughput of luminescent lamp.The content of each composition is preferably Li 2O:0～5mol%, Na 2O:0～8mol%, K 2O:0～12mol%.
The alkaline earth metal oxide of MgO and CaO adds for the purpose that improves electrical insulating property and chemical durability.The content of MgO is preferably the scope of 0.5～5mol%; The content of CaO is preferably 0.5～10mol%.When MgO is less than 0.5mol% or CaO when being less than 0.5mol%, the situation that existence can not achieve the above object.On the other hand, as MgO during more than 5mol% or CaO during more than 10mol%, the tendency of glass devitrification increases.
The purpose of the glass bulb processibility when SrO and BaO make in order to improve glass melting and luminescent lamp is added.The content of SrO is preferably 0～8mol%; The content of BaO is preferably 0～10mol%.As SrO during more than 8mol% or BaO during more than 10mol%, the easy devitrification of glass.
CeO 2For the purpose that effectively absorbs ultraviolet ray and suppress solarization (solarization) is added.Its content is preferably the scope of 0.01～2mol%.If be less than 0.01mol%, then can not achieve the above object; If more than 2mol%, then cause the devitrification of glass, be difficult to make the luminescent lamp of light flux with expectation.Its content is preferably the scope of 0.01～1mol% especially.
Fe 2O 3For the purpose that obtains the ultraviolet radiation absorption effect is added.Its content is preferably the scope of 0～0.2mol%.If more than 0.2mol%, then the transmitance of visible region reduces, thereby the reduction of the optical throughput of luminescent lamp, so be not preferred.
SnO adds from the purpose that 4+ is changed to 3+ in order to promote Ce ionic valence mumber.Its content is preferably the scope of 0.01～5mol%.If be less than 0.01mol%, then can not obtain above-mentioned effect; If more than 5mol%, then exist the physical strength of glass to reduce, problem such as yield rate reduction in the pipe stretching process of Glass tubing.Be preferably the scope of 0.1～3mol% especially.
In addition, glass of the present invention, the content of its each composition in the limit that does not break away from above-mentioned compositing range, can also contain other composition as long as in above-mentioned scope in fact.As other composition, for example can enumerate: ZrO 2, ZnO, P 2O 5, TiO 2, WO 3Deng.
Up to now, CeO 2As a kind of finings by known, if but heavy addition then can not obtain clarifying effect.But, if in order to obtain clarifying effect heavy addition, then produce the problem of glass coloring.Therefore, in fact only add CeO as finings 2Be to be difficult to make colourless and glass that entrapped air pockets is few.
In addition, SnO 2As a kind of finings also by known, but and CeO 2The same, if heavy addition then can not obtain clarifying effect.But, if in order to obtain clarifying effect heavy addition, then produce the problem of glass devitrification.Therefore, in fact only add SnO as finings 2Be to be difficult to make the few glass of no devitrification and entrapped air pockets.
(explanation of the manufacture method of glass composition for lamp)
In the manufacture method of the glass composition for lamp of present embodiment, at first the multiple frit of allotment obtains raw mix in the scope of the composition of glass composition for lamp of the present invention.Then, raw mix is put in the glass-melting furnace, in atmospheric atmosphere, 1500～1600 ℃ of following fusions 5～8 hours and obtain glass melting liquid.At this moment, do not stir or processing such as foaming.Then, glass melting liquid is configured as tubulose, cuts off the size that is processed into regulation again, make the lantern pane pipe by pipe stretching methods such as Danner methods.In addition, this Glass tubing is carried out hot-work make glass bulb, make various lamps.
In addition, be not limited to frit is deployed into the program of putting into behind the raw mix in the glass-melting furnace, it is also conceivable that staggers the time a part of frit and other frit puts in the glass-melting furnace allotment raw mix in glass-melting furnace (dissolving still).
(explanation of lamp)
An embodiment as lamp of the present invention describes straight tubular cold-cathode fluorescence lamp based on accompanying drawing.Fig. 2 is the synoptic diagram that the major portion structure of the cold-cathode fluorescence lamp in the present embodiment is shown.The structure of this cold-cathode fluorescence lamp 1 is based on the structure of the cold-cathode fluorescence lamp of prior art basically.
The glass bulb 2 of cold-cathode fluorescence lamp 1 is formed by the glass composition for lamp of above-mentioned present embodiment, and its external diameter is about that 4.0mm, internal diameter are about 3.0mm, total length is about 730mm.In addition, the external diameter of glass bulb 2, internal diameter and total length are not subjected to above-mentioned qualification, because the glass bulb 2 of cold-cathode fluorescence lamp 1 usefulness is contemplated to be tubule footpath and thin-walled, therefore preferred external diameter is 1.8 (internal diameter is 1.4)～6.0 (internal diameter is 5.0) mm.
The both ends of glass bulb 2 use pearl glass (bead glass) 3 to carry out gas-tight seal respectively.In addition, at the both ends of glass bulb 2, the lead-in wire 4 of the about 0.8mm of diameter that is made by tungsten metal or Kovar alloy is hermetically sealed in the mode that connects pearl glass 3.In addition, the electrode 5 of cup-shaped is installed on the end of each lead-in wire glass bulb 2 private side of 4, this electrode 5 make by nickel or niobium and in surface coated the evaporation of electron material.
On the inner face of glass bulb 2, form coated with rare earth class fluor (Y 2O 3: Eu 3+, LaPO 4: Ce 3+, Tb 3+, BaMg 2Al 16O 27: Eu 2+, Mn 2+) and the luminescent coating 6 that obtains, described rare earth class fluor mixed glow, the fluor of green light and blue light-emitting.In addition, rare gas (not shown) such as the mercury (not shown) of 0.8～2.5mg and xenon have been enclosed in the inside of glass bulb 2.
More than, specifically understand straight tube shape cold-cathode fluorescence lamp 1 of the present invention based on embodiment, but content of the present invention is not limited to above-mentioned embodiment.
(explanation of experiment)
Make the glass composition for lamp of present embodiment shown in Figure 1 and the glass composition for lamp of comparative example shown in Figure 3, and estimate, their characteristic relatively.
The following making of each glass composition: the raw mix that will get with the allotment of the composition in scheming takes by weighing 17g and puts in the platinum crucible, 1500 ℃ of following heating and meltings are 3 hours in electric furnace, in electric furnace, take out then, the crucible bottom surface contacted with cold water carry out chilling, glass and crucible are being peeled off at the interface, thereby made.
Thermal expansivity (α 30/380) and glass transition point, it is the columned test portion that each glass composition is configured as diameter 5.0mm, length 15mm, (Rigaku makes reusable heat sizing device, model: the average coefficient of linear expansion that TAS300 TMA8140C) is determined at 30～380 ℃ temperature range.
The bubble number is to use the number of bubbles of being confirmed among the 120mm2 of Section Central portion, the thickness of slab 3mm of processes pixel computed in software glass composition.Only the bubble more than the diameter 30 μ m is counted bubble.
During the bubble number was measured, glass composition was cut into the 120mm of Section Central portion 2(vertical 10mm * horizontal 12mm), thickness of slab 3mm, mirror polish is carried out to #400, #800, #1000, #1500, #2000 number in the two sides of interim ground abrading glass then, makes glass sample.Then, use the number of bubbles of confirming in this glass sample of processes pixel computed in software.Only the bubble more than the diameter 30 μ m is counted bubble.
Entrapped air pockets judges that number of bubbles is judged to be " * " when surpassing 350; Number of bubbles is 350 and is judged to be " zero " when following.This is because if surpass 350 glass composition making lamp with number of bubbles, confirm then to cause that significant yield rate reduces.
Foaming again during hot-work is, when the hot-work glass composition, the situation that superheat section is produced the bubble more than the diameter 30 μ m foams and is judged to be " * " as existing, and the situation of not having foaming again is not judged to be " zero ".
The infrared rays transmitance is to use FT-IR (the system FTIR-8200 of Shimadzu Scisakusho Ltd), for the glass composition of the test portion thickness 2mm that the two sides is carried out mirror ultrafinish, at wavelength 2800～3800cm -1Scope in measure.The situation of estimating real glass bulb is, handles 3 hours under the temperature of glass bulb softening temperature+20 ℃, makes glass bulb softening, makes the sheet glass of thickness of slab 2mm.Then, the square of indulging 15mm * horizontal 15mm is cut in this sheet glass processing, obtains the evaluation sample of vertical 15mm * horizontal 15mm * thick 2mm.Grind interimly this evaluation with the two sides of sample to #400, #800, #1000, #1500, #2000 number, carry out mirror polish.
Measurement result as shown in Figure 4.The purpose of measuring the infrared rays transmitance is to estimate remaining amount of moisture in the glass composition.Remaining moisture is by H in the glass composition 3BO 3Decomposition reaction the time produce its part molten existence in the glass composition.If the molten amount of moisture of depositing is more in the glass composition, then when the hot-work glass composition, the molten moisture of depositing gasifies and causes foaming again.
Amount of moisture in the glass composition can pass through 3620cm -1The mnm. of the infrared rays transmitance of vicinity is promptly at 3620cm -1The OH that the vicinity is confirmed -1The size of absorption peak confirm.Particularly, 3620cm -1The mnm. of the infrared rays transmitance of vicinity is more little, represents that then amount of moisture remaining in the glass composition is many more.Among Fig. 5 at wavelength 3600cm -1～3800cm -1Scope in the measurement result of infrared rays transmitance is done to amplify expression so that confirm 3620cm easily -1Near the mnm. of infrared rays transmitance.
In the comparative example 1～5,3620cm -1Near infrared rays transmitance is 7.8～8.0% high value.This is because do not add H 3BO 3, the moisture remaining quantity in the glass composition is less.But, in the comparative example 1～5 owing to do not add H 3BO 3, thereby the clarifying effect that can not obtain expecting, and remaining in the glass composition a large amount of bubbles are arranged.So being unsuitable for lamp uses.
In the comparative example 6 and 7, because H 3BO 3Addition more, so the moisture remaining quantity in the glass composition is more, 3620cm -1Near infrared rays transmitance is 2%.If the moisture remaining quantity like this in the glass composition is more, then when hot-work, cause foaming again, use so be unsuitable for lamp.
In the comparative example 8, added B 2O 3And H 3BO 3Both.But, B 2O 3/ H 3BO 3Ratio of mixture less than 1/3, so the moisture remaining quantity in the glass composition is more, 3620cm -1Near infrared rays transmitance is 2%.If the moisture remaining quantity like this in the glass composition is more, then when hot-work, cause foaming again, use so be unsuitable for lamp.
In the comparative example 9, added B 2O 3And H 3BO 3Both.But, B 2O 3/ H 3BO 3Ratio of mixture greater than 1, so clarifying effect is insufficient, remaining a large amount of bubble in the glass composition is unsuitable for lamp and uses.
Among the embodiment 1～3, the ratio of mixture of the scope with 1/3～1 is added B 2O 3And H 3BO 3Therefore, the bubble in clarifying effect height and the glass composition is few.In addition, 3620cm -1Near the infrared rays transmitance be 3.0～4.5% scope, the moisture remaining quantity in the glass composition is few and be difficult to cause foaming again when hot-work.So being suitable for lamp uses.
Industrial usability
The manufacture method of glass composition for lamp of the present invention, glass composition for lamp and lamp are passable In all lamps, be extensive use of. Be specially adapted to liquid crystal TV, PC display, car Carry the back lighting that requires the permeation type liquid crystal display element of high-grade demonstration with liquid crystal panel etc. Cold-cathode fluorescence lamp etc. In addition, the manufacture method of glass composition for lamp of the present invention, lamp Do not add in fact the carrying capacity of environment materials such as arsenic, antimony, lead with glass composition and lamp, therefore yet Meet the society need of earth environment protection.

Claims (14)

1. the manufacture method of glass composition for lamp is characterized in that,
Comprise with the raw mix fusion being the fusion operation of vitreousness, described raw mix has been for having added the mixture of the oxyhydroxide of the oxide compound of element-specific and described element-specific with the mol ratio of oxide/hydroxide=1/3～1,
In described fusion operation, heat described raw mix, so that described oxyhydroxide generation decomposition reaction, thereby comprise H from described oxyhydroxide generation 2O or H 2At least a gas.
2. the manufacture method of the described glass composition for lamp of claim 1, it is characterized in that, described oxide compound and oxyhydroxide are added in the described raw mix, count 8～17mol% so that the content of the described element-specific in the glass composition for lamp converts with oxide compound.
3. the manufacture method of the described glass composition for lamp of claim 2, it is characterized in that, described oxyhydroxide is added in the described raw mix, count 5～10.5mol% so that the content of the described element-specific in the glass composition for lamp converts with oxide compound.
4. the manufacture method of the described glass composition for lamp of claim 3 is characterized in that, described glass composition for lamp is a pyrex, and described element-specific is a boron.
5. the manufacture method of the described glass composition for lamp of claim 1, it is characterized in that, described oxyhydroxide is added in the described raw mix, count 5～10.5mol% so that the content of the described element-specific in the glass composition for lamp converts with oxide compound.
6. the manufacture method of the described glass composition for lamp of claim 1 is characterized in that, described glass composition for lamp is a pyrex, and described element-specific is a boron.
7. glass composition for lamp, it is that manufacture method by the described glass composition for lamp of claim 1 makes, wherein,
When test portion thickness is 2mm, at wavelength region may 3620cm -1Near the mnm. of infrared rays transmitance is 3.0～4.5%.
8. the described glass composition for lamp of claim 7 is characterized in that, the thermal expansivity (α under 30～380 ℃ 30/380) be 34 * 10 -7/ K～43 * 10 -7/ K.
9. the described glass composition for lamp of claim 7 is characterized in that, the thermal expansivity (α under 30～380 ℃ 30/380) be 43 * 10 -7/ K～55 * 10 -7/ K.
10. glass composition for lamp, it is that manufacture method by the described glass composition for lamp of claim 4 makes, wherein,
When test portion thickness is 2mm, at wavelength region may 3620cm -1Near the mnm. of infrared rays transmitance is 3.0～4.5%.
11. the described glass composition for lamp of claim 10 is characterized in that, the thermal expansivity (α under 30～380 ℃ 30/380) be 34 * 10 -7/ K～43 * 10 -7/ K.
12. the described glass composition for lamp of claim 10 is characterized in that, the thermal expansivity (α under 30～380 ℃ 30/380) be 43 * 10 -7/ K～55 * 10 -7/ K.
13. lamp is characterized in that, possesses the glass bulb that is formed by the described glass composition for lamp of claim 7.
14. lamp is characterized in that, possesses the glass bulb that is formed by the described glass composition for lamp of claim 10.
CNA2007800035687A 2006-01-30 2007-01-24 Process for producing glass composition for lamp, glass composition for lamp, and lamp Pending CN101374776A (en)

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