CN112573831A - Glass bead for fixing filament of incandescent lamp and preparation process thereof - Google Patents

Glass bead for fixing filament of incandescent lamp and preparation process thereof Download PDF

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Publication number
CN112573831A
CN112573831A CN202011444456.9A CN202011444456A CN112573831A CN 112573831 A CN112573831 A CN 112573831A CN 202011444456 A CN202011444456 A CN 202011444456A CN 112573831 A CN112573831 A CN 112573831A
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Prior art keywords
glass
filament
fixing
incandescent lamp
glue
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CN202011444456.9A
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Chinese (zh)
Inventor
何纪生
缪锡根
朱元海
潘华路
缪波
申亮
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Ganzhou China Ceramics Technology Co ltd
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Ganzhou China Ceramics Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C12/00Powdered glass; Bead compositions
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/06Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/06Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • C03B19/063Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction by hot-pressing powders
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/076Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/11Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen
    • C03C3/112Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine
    • C03C3/115Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine containing boron
    • C03C3/118Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine containing boron containing aluminium

Abstract

The invention discloses a glass bead for fixing an incandescent lamp filament and a preparation process thereof, belonging to the field of incandescent lamp materials, wherein the glass bead for fixing the incandescent lamp filament and the preparation process thereof comprise the following steps: step 1 obtaining a glass frit: weighing materials, mixing the materials by a ball mill, putting the materials into a crucible for melting, and pouring molten glass into deionized water; step 2, obtaining a glass preform: and (2) drying the glass fragments obtained in the step (1), crushing the glass fragments by a ball mill, using organic matters as a binder, preparing glass powder into slurry, granulating by a spray granulator, pressing into a glass tube blank by a mould, slowly heating by a glue discharging furnace, discharging glue, and sintering to form a glass preform. The invention discloses a glass bead for fixing filament of incandescent lamp and its preparation process, which adopts a new glass formulation without toxic components to obtain glass powder, and prepares glass granulated powder by adding glue, and then prepares the glass bead or glass tube suitable for fixing filament by pressing blank and removing glue.

Description

Glass bead for fixing filament of incandescent lamp and preparation process thereof
Technical Field
The invention relates to the field of incandescent lamp packaging materials, in particular to glass beads for fixing an incandescent lamp filament and a preparation process thereof.
Background
The automobile lamp (such as a high beam) is of the incandescent lamp (figure 1) type, the LED lamp type and the like. The incandescent lamp has high power and high temperature, and its main components are filament (generally tungsten filament) and electrode leads (made of Dumet wire) at two ends of the tungsten filament. Dumet wire is made up of iron-nickel alloy wire (nickel content 43.0 +/-0.5%) as core wire, electrolytic copper as coating and borate (Na)2B4O7) Is coated. The coefficient of thermal expansion of Dumet wire is (8-10) x10-6V. C. In order to secure the two dumet wire leads and prevent the short circuit problem caused by softening, bending or twisting of the two dumet wire leads, it is necessary to secure the two dumet wires with high temperature resistant glass, as shown in fig. 2. The requirement for the filament fixing glass is that its thermal expansion coefficient matches that of Dumet wire, e.g. the deviation is 0.5x10-6The glass transition temperature is higher than 595 ℃ and 615 ℃ and the glass softening point is higher than 650 ℃ within/° C, and most importantly, the high-temperature resistivity of the glass is high, for example, the insulation resistivity of the glass is not less than 10 under the condition of the temperature of more than 470 DEG C8Ohm.
The existing filament glass is barium silicate-based glass imported from Germany, the real formula of the glass is not disclosed, but toxic V can be confirmed to be contained in the glass2O5Component, great harm, high cost of imported glass and long supply time.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to solve the technical problem of providing a glass bead for fixing an incandescent lamp filament and a preparation process thereof, researching and developing a novel glass formula of non-toxic components, obtaining glass powder, preparing the glass powder into glass granulation powder by adding glue, and then preparing the glass bead or glass tube suitable for fixing and packaging the filament by a compacting and glue discharging process.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a glass bead for fixing filament of an incandescent lamp, which comprises the following glass components in percentage by mass: (46-54)% SiO2、(20-25)%BaO、(0.2-4.0)%SrO、(1.5-4.0)%MgO、 (1.0-4.0)%CaO、(0-4.0)%Bi2O3、(2.0-7.0)%B2O3、(1.0-3.0)%Na2O、 (2.0-6.0)%K 20、(1.5-4.5)%Al2O3、(0.5-1.0)%Cr2O3、(0.2-1.5)%MnO2、 (0.2-1.0)%Co2O3、(0.17-0.80)%Fe2O3、(0-1.0)%CaF2And (0-1.0)% CeO2
The invention provides a preparation process of glass beads for fixing filament of incandescent lamp, which comprises the following steps:
step 1-obtaining glass fragments: weighing required materials, mixing the materials through a ball mill, putting the mixture after ball milling and uniform mixing into a ceramic crucible, melting and preserving heat of the mixture, and pouring molten glass liquid into deionized water to obtain glass fragments;
step 2-obtaining a glass preform: and (2) drying the glass fragments obtained in the step (1), crushing the glass fragments by a ball mill, preparing glass powder into slurry by using an organic binder such as polyvinyl alcohol (PVA), granulating by using a spray granulator, pressing the glass powder into a glass tube blank by using a mould, slowly heating and removing the glue by using a glue removing furnace, and finally sintering to form a glass preform.
Preferably, the glass melting temperature in the step 1 is 1450-1500 ℃, and the heat preservation time is 80-120 min.
Preferably, in step 2, the median diameter particle size D50 of the ground glass pieces after ball milling is between 15 μm and 35 μm.
Preferably, the mass fraction of the binder polyvinyl alcohol (PVA) used in step 2 is between (2-4)%.
Preferably, in step 2, the spray granulator is used for granulating and then pressing the granules into a glass tube blank through a die, and the required pressure is between 20MPa and 100 MPa.
Preferably, in the step 2, the sintering temperature required by the glass tube blank sintered after the temperature is slowly raised and the glue is discharged through the glue discharging furnace is between 680 and 720 ℃.
Preferably, in step 2, the temperature needs to be slowly raised to the required sintering temperature, and the heating process is as follows:
room temperature (warming up with 120 min) → 250 ℃ (holding 30min) → 250 ℃ (warming up with 150 min) → 400 ℃ (holding 30min) → 400 ℃ (warming up with 30min) → 450 ℃ (holding 30min) → 450 ℃ (warming up with 90 min) → 700 ℃ (holding 10min) → 700 ℃ (power off) → furnace cooling.
The invention has the beneficial effects that:
the prepared glass tube meets the basic performance requirements of the incandescent lamp on fixing glass and the operability requirements of the filament fixing and sealing process, obtains the satisfactory effects of filament electric insulation fixing and lamp tube airtight packaging, can replace foreign similar products, and overcomes the defect of toxic components in foreign similar glass.
Drawings
FIG. 1 is a schematic view of a filament and fusion sealed glass beads;
FIG. 2 is a physical diagram of a glass bead or glass tube for filament mounting and encapsulation;
FIG. 3 is a schematic diagram showing the shape and size of a glass bead or glass tube for filament fixing and sealing;
FIG. 4 is a thermal expansion curve of a filament fixing glass bead of an incandescent lamp according to an embodiment of the present invention;
table 1 shows the dimensional data of the glass beads or glass tubes for filament fixing and sealing;
table 2 shows the batch calculations for the glass formulations of example 1;
table 3 is a comparison table of different formulations used to make different glasses;
table 4 shows a comparison of the properties of the glasses obtained with the different formulations.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
Table 1: dimensional data of glass beads or glass tubes for filament mounting and encapsulation
(Code) Description of the invention Data of
A Outer diameter OD 7.05-7.95mm
B Outer diameter ID 5.25-5.75mm
C Length of 1.7+/-0.15mm
W Weight (D) 100+/-mg/pcs
Table 2: batch calculation for glass formulation of example 1
Figure RE-GDA0002955474520000041
Figure RE-GDA0002955474520000051
As shown in fig. 1 to 4 and tables 1 to 4, the content (mass fraction) and composition (component) of a glass bead for fixing a filament of an incandescent lamp provided in this series of examples were: (46-54)% SiO2、(20-25)%BaO、(0.2-4.0)%SrO、(1.5-4.0)%MgO、(1.0-4.0)% CaO、(0-0.5)%V2O5、(0-4.0)%Bi2O3、(2.0-7.0)%B2O3、(1.0-3.0)% Na2O、(2.0-6.0)%K 20、(1.5-4.5)%Al2O3、(0.5-1.0)%Cr2O3、 (0.2-1.5)%MnO2、(0.2-1.0)%Co2O3、(0.17-0.80)%Fe2O3、 (0-1.0)%CaF2And (0-1.0)% CeO2
The preparation process of the glass bead for fixing the filament of the incandescent lamp provided by the series of embodiments is based on the glass bead for fixing the filament of the incandescent lamp, and further comprises the following steps of:
step 1-obtaining glass fragments: weighing required materials, mixing the materials by a ball mill in a dry method or a wet method, putting the mixture after ball milling and mixing into a ceramic crucible, melting and preserving heat of the mixture, and pouring molten glass into deionized water to obtain glass fragments;
step 2-obtaining a glass preform: and (2) drying the glass fragments obtained in the step (1), crushing (dry grinding or wet grinding) the dried glass fragments by using a ball mill, preparing glass powder into water-based (or organic-based) slurry by using polyvinyl alcohol (PVA) as a water-soluble binder or polyvinyl butyral (PVB) as an organic solvent-based binder, granulating by using a spray granulator, pressing the slurry into a glass tube blank by using a die, slowly heating and discharging glue by using a glue discharging furnace, and finally sintering to form a glass preform.
Further, the glass melting temperature in the step 1 is 1450-1500 ℃, and the heat preservation time is 80-120 min.
Further, in step 2, the median diameter particle size D50 of the glass cullet after being pulverized by the ball mill is between 15 μm and 35 μm.
Further, the binder polyvinyl alcohol (PVA) or polyvinyl butyral (PVB) used in step 2 is present in a mass fraction of between (2-4)%.
Further, in step 2, the spray granulator is used for granulating and then is pressed into a glass tube blank through a die, and the required pressure is 20MPa-100 MPa.
Further, in the step 2, the sintering temperature required by the glass tube blank sintered after the temperature is slowly raised and the glue is discharged through the glue discharging furnace is between 680 and 720 ℃.
Further, in step 2, the temperature needs to be slowly raised to the required sintering temperature, and the heating process is as follows:
room temperature (warming up with 120 min) → 250 ℃ (holding 30min) → 250 ℃ (warming up with 150 min) → 400 ℃ (holding 30min) → 400 ℃ (warming up with 30min) → 450 ℃ (holding 30min) → 450 ℃ (warming up with 90 min) → 700 ℃ (holding 10min) → 700 ℃ (power off) → furnace cooling.
Table 3: comparison table for different formulas for making different glasses
Component (c) is Example 1 Example 2 Example 3 Example 4 Comparative example 1 Comparative example 2 Comparative example 3
SiO2 46 49.00 48.50 52.00 55.00 50.20 41
BaO 22.2 20 21.92 25 21.7 18.5 16.56
SrO 1.5 4 2.00 0.2 2 0.2
MgO 1.5 2.50 2.50 4.00 2.50 2.90 11.14
CaO 3.2 4 3.70 1 0.7 4.8 13
V2O5 5 0 4.00 3.67 0.00 6.40
Bi2 O 3 1 4.00 0.00 0.5
B2O3 6 5.5 7.00 2 7.5 1.7 2
Na2O 1.5 0.90 3.00 1.00 1.50 1.00 0.5
K2O 2.3 2.7 2.00 6 1.7 5.2 2.5
Al2O3 4.5 3.00 1.50 3.50 3.00 5.70 1.95
Cr2O3 1 0.50 0.50 0.57 0.50 0.50 1.5
MnO2 1.5 1.40 1.40 0.20 1.40 1.40 1.5
Co2O3 1 0.20 0.20 0.20 0.20 0.20 0.4
Fe2O3 0.8 0.80 0.28 0.17 0.80 0.80 0.4
CaF2 0.5 1.00 1.00 0 1.00 0.50 0.5
CeO2 0.5 0.50 0.50 0 0.50 0.5
ZnO 5.55
ZrO2 1
Table 4: comparison of glass Properties obtained with different formulations
Figure RE-GDA0002955474520000071
As is evident from the data obtained by the comparative tests in tables 3 and 4, the glass tube obtained in accordance with this example has a thermal expansion coefficient and a glass transition point TgGlass softening point TfThe value of the fluorescent lamp is in the required range, meets the requirements on the basic performance and the operability of the sealing process, obtains the satisfactory effects of fixing the filament and packaging the lamp tube, can replace foreign similar products, overcomes the defect of toxic components in foreign glass, and is harmless to human bodies and the environment.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. The present invention is not to be limited by the specific embodiments disclosed herein, and other embodiments that fall within the scope of the claims of the present application are intended to be within the scope of the present invention.

Claims (8)

1. A glass bead for fixing filament of incandescent lamp is characterized in that:
the glass comprises the following components in percentage by mass: (46-54)% SiO2、(20-25)%BaO、(0.2-4.0)%SrO、(1.5-4.0)%MgO、(1.0-4.0)%CaO、(0-4.0)%Bi2O3、(2.0-7.0)%B2O3、(1.0-3.0)%Na2O、(2.0-6.0)%K20、(1.5-4.5)%Al2O3、(0.5-1.0)%Cr2O3、(0.2-1.5)%MnO2、(0.2-1.0)%Co2O3、(0.17-0.80)%Fe2O3、(0-1.0)%CaF2And (0-1.0)% CeO2
2. A process for producing a glass bead for fixing an incandescent lamp filament, comprising the glass bead for fixing an incandescent lamp filament according to claim 1, characterized by further comprising the steps of:
step 1-obtaining glass fragments: weighing required materials, mixing the materials through a ball mill, putting the mixture after ball milling and uniform mixing into a ceramic crucible, melting and preserving heat of the mixture, and pouring molten glass liquid into deionized water to obtain glass fragments;
step 2-obtaining a glass preform: and (2) drying the glass fragments obtained in the step (1), crushing the glass fragments by using a ball mill, using organic matters such as polyvinyl alcohol (PVA) as a binder, preparing glass powder into slurry (such as water-based slurry), granulating by using a spray granulator, pressing into a glass tube blank by using a mould, slowly heating and discharging glue by using a glue discharging furnace, and finally sintering to form a glass preform.
3. The process according to claim 2, wherein the glass beads for fixing the filament of the incandescent lamp are prepared by:
the glass melting temperature in the step 1 is 1450-1500 ℃, and the heat preservation is usually 80-120 min.
4. The process according to claim 2, wherein the glass beads for fixing the filament of the incandescent lamp are prepared by:
in step 2, the median particle size D50 of the ground glass pieces was between 15 μm and 35 μm after ball milling.
5. The process according to claim 2, wherein the glass beads for fixing the filament of the incandescent lamp are prepared by:
the mass fraction of the binder used in step 2 is between (2-4)% and the binder may preferably be polyvinyl alcohol (PVA).
6. The process according to claim 2, wherein the glass beads for fixing the filament of the incandescent lamp are prepared by:
in the step 2, the spray granulator is used for granulating and then is pressed into a glass tube blank by a mould, and the required pressure is between 20MPa and 100 MPa.
7. The process according to claim 2, wherein the glass beads for fixing the filament of the incandescent lamp are prepared by:
in the step 2, the sintering temperature required by the glass tube blank sintered after the temperature is slowly raised and the glue is discharged through the glue discharging furnace is between 680 and 720 ℃.
8. The process according to claim 7, wherein the glass beads for fixing the filament of the incandescent lamp are prepared by:
in step 2, the temperature needs to be slowly raised to the required sintering temperature, and the heating process is as follows:
room temperature (warming up with 120 min) → 250 ℃ (holding 30min) → 250 ℃ (warming up with 150 min) → 400 ℃ (holding 30min) → 400 ℃ (warming up with 30min) → 450 ℃ (holding 30min) → 450 ℃ (warming up with 90 min) → 700 ℃ (holding 10min) → 700 ℃ (power off) → furnace cooling.
CN202011444456.9A 2020-12-08 2020-12-08 Glass bead for fixing filament of incandescent lamp and preparation process thereof Pending CN112573831A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113788605A (en) * 2021-08-30 2021-12-14 四川航天川南火工技术有限公司 Pressing and forming method for long glass tube for initiating explosive device sealing body
CN114014527A (en) * 2021-11-01 2022-02-08 西安赛尔电子材料科技有限公司 Aluminum-sealed phosphate glass powder spray granulation method

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1986492A (en) * 2006-12-15 2007-06-27 武汉理工大学 Preparing process of great size energy-storing dielectric ceramic
CN101565276A (en) * 2009-06-01 2009-10-28 贵阳晶华电子材料有限公司 Glass powder for PDP barrier
CN102030477A (en) * 2009-10-07 2011-04-27 旭硝子株式会社 Ceramic material composition
CN102276151A (en) * 2011-05-16 2011-12-14 周涛 Technological method for preparing LTCC (low temperature co-fired ceramic) amorphous glass ceramic powder with microwave plasma torch
JP2017071532A (en) * 2015-10-08 2017-04-13 日本電気硝子株式会社 Glass powder for three-dimensional molding

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1986492A (en) * 2006-12-15 2007-06-27 武汉理工大学 Preparing process of great size energy-storing dielectric ceramic
CN101565276A (en) * 2009-06-01 2009-10-28 贵阳晶华电子材料有限公司 Glass powder for PDP barrier
CN102030477A (en) * 2009-10-07 2011-04-27 旭硝子株式会社 Ceramic material composition
CN102276151A (en) * 2011-05-16 2011-12-14 周涛 Technological method for preparing LTCC (low temperature co-fired ceramic) amorphous glass ceramic powder with microwave plasma torch
JP2017071532A (en) * 2015-10-08 2017-04-13 日本電気硝子株式会社 Glass powder for three-dimensional molding

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113788605A (en) * 2021-08-30 2021-12-14 四川航天川南火工技术有限公司 Pressing and forming method for long glass tube for initiating explosive device sealing body
CN114014527A (en) * 2021-11-01 2022-02-08 西安赛尔电子材料科技有限公司 Aluminum-sealed phosphate glass powder spray granulation method

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