CN107043215A - A kind of low temperature sealing glass of lanthana modification and its preparation and application method - Google Patents
A kind of low temperature sealing glass of lanthana modification and its preparation and application method Download PDFInfo
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- CN107043215A CN107043215A CN201710273036.0A CN201710273036A CN107043215A CN 107043215 A CN107043215 A CN 107043215A CN 201710273036 A CN201710273036 A CN 201710273036A CN 107043215 A CN107043215 A CN 107043215A
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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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
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Abstract
The invention discloses a kind of La2O3Modified low temperature sealing glass and its preparation and application, raw material composition are ZnO, Na2O、P2O5、La2O3, its mol ratio is 33 ~ 45：15~25：22~40：5~25.By introducing La3+Ion, O is attracted using its high field intensity2‑Ion, promotes PO3To PO4Transformation, reinforcing glass network stabilization, so as to improve its heat endurance.High concentration La2O3Addition, as intermediate reinforcing agent, the wetting of glass and base material can be significantly improved.By the ZnO and P that introduce high concentration2O5, the coordinative role of the two is played, the transformetion range of the glass is reduced to 350 425 DEG C；Na2O can reduce the fusion temperature of glass, and can further improve its sealing property.The glass of the present invention is applied to LED fluorescent powder sealing-in, electronic material and other low-temperature sealing fields.
Description
Technical field
The invention belongs to seal glass field, and in particular to a kind of La2O3Modified low temperature sealing glass and its preparation are with making
Use method.
Background technology
Low temperature sealing glass（Sealing temperature<600 DEG C), due to its good heat resistance and chemical stability, high machinery is strong
Degree, is widely used in the various fields such as electric slurry, electrovacuum and microelectric technique, the energy, aerospace, automobile, such as luminous two
Pole pipe（LED）In fluorescent material sealing-in, the whether excellent actual use performance for directly resulting in battery of the performance of seal, sealing materials.Envelope
Connect glass and can also be used for mutual sealing-in between glass, ceramics, metal, semiconductor.But, research both at home and abroad is generally using containing at present
Pb seal, sealing materials, this will be polluted to environment.In addition, phosphate glass is because with melting temperature sealing is low, the coefficient of expansion is adjustable
Whole scope is wide, price is low, obtain extensive concern the advantages of can substantially reduce environmental pollution.
Patent application 201310259302.6, discloses a kind of low-temperature lead-free glass dust and preparation method thereof, but the body
Another poisonous material Sb is introduced in system, environmental issue is not solved.And patent application 201210366375.0 is also disclosed
Lead-free glass material and preparation method thereof, passes through P2O5、K2O、Na2O、ZrO2、TiO2Composition design Deng raw material avoids ring
Border is polluted, but the softening range of the glass is 500 ~ 600 DEG C, it is difficult to meet low-temperature sealing especially electronic component low temperature
The requirement of Fast Sintering.The previous work of this seminar is found that B-Bi-Zn system glass can solve the above problems, and has applied specially
Profit.However, B-Bi-Zn system glass is because contain transition-metal ions Bi so that glass darkens in sintering process so that glass
Glass is in the light transmission rate step-down of visible light wave range, and B-Bi-Zn system glass is easy to crystallization, is difficult to control in sealing-in process.Cause
This, B-Bi-Zn system glass is limited in terms of optical property by larger.
The content of the invention
In order to solve the above problems, the invention provides a kind of La2O3Modified low temperature sealing glass and its preparation and use
Method, passes through La2O3Introduce La3+Ion, O is attracted using its high field intensity2-Ion, promotes PO3To PO4Transformation, reinforcing glass network
Stability, so as to improve its heat endurance, the material, which is placed in 1000 hours in 80 DEG C of hot water, can keep good stability.It is highly concentrated
Spend La2O3Addition, as intermediate reinforcing agent, the wetting of glass and base material can be significantly improved.By the ZnO for introducing high concentration
With P2O5, the coordinative role of the two is played, the transformetion range of the glass is reduced to 350-425 DEG C；Na2O can reduce glass
Fusion temperature, and can further improve its sealing property.The glass of the present invention is applied to LED fluorescent powder sealing-in, electronics
Material and other low-temperature sealing fields.
The present invention is implemented by following technical solution：
A kind of La2O3The raw material composition of modified low temperature sealing glass is ZnO, Na2O、P2O5、La2O3, its mol ratio is 33 ~ 45：
15~25：22~40：5~25.
It is preferred that, raw material ZnO, Na2O、P2O5、La2O3Mol ratio be 38 ~ 40.5：18~22：27~29.5：10~15.
The method for preparing low temperature sealing glass modified as described above comprises the following steps：
（1）Raw material is well mixed；Founded by 880-1100 DEG C, soaking time 1-4 hours；To the glass metal melted, enter
Row chilling, obtains glass frit；Then, glass frit is crushed, grinding or ball milling obtain glass powder after sieving；
（2）Glass powder and binding agent, dispersant and solvent are mixed into slurry, ball milling disperses in ball mill；Curtain coating
Shaping, is spontaneously dried, and the idiosome of shape, is made seal glass needed for being then cut into.
The step（2）Binding agent be epoxy resin, methylcellulose, polyvinyl butyral resin, in polyvinyl alcohol
One or more of mixtures.
The step（2）Dispersant be fish oil, polyacrylic acid, polyvinyl alcohol, polyacrylamide in one or more
Mixture.
The step（2）Solvent be water, ethanol, isopropanol, n-butanol, toluene, dimethylbenzene, acetone in one kind or several
The mixture planted.
Application method：Seal glass, which is placed in, treats sealing-in position, is heated up in electric furnace with 1-5 DEG C/min speed, 400-500
DEG C insulation 0.5-1 hours, is then warming up to 500-650 DEG C of isothermal holding 0.5-1 hours with 1-5 DEG C/min speed, that is, completes
Sealing-in.
The remarkable advantage of the present invention is：
（1）Pass through La2O3Introduce La3+Ion, O is attracted using its high field intensity2-Ion, promotes PO3To PO4Transformation, reinforcing glass
Network, so as to improve its heat endurance, reduces tendency towards devitrification, the material, which is placed in 1000 hours in 80 DEG C of hot water, can keep good
Stability；
（2）La2O3The thermal coefficient of expansion of adjustable glass, can further improve its sealing property；Moreover, high concentration La2O3's
Addition, as intermediate reinforcing agent, can significantly improve the wetting of glass and base material, be conducive to implementing sealing-in；
（3）Introduce the ZnO and P of high concentration2O5, the coordinative role of the two is played, the transformetion range of the glass is reduced to
350-425℃；
（4）Na2O can reduce the glass melting temperature of glass, and can improve its sealing property；
（5）Preparing raw material of the present invention is simple and easy to get, process stabilizing, has reached practical and industrialized condition.
Brief description of the drawings
Fig. 1 is thermal dilatometry of the embodiment 1-4 seal glass under the conditions of parallel laboratory test.
Fig. 2 is DSC curve of the embodiment 1-4 seal glass under the conditions of parallel laboratory test.
Embodiment
A kind of La2O3The raw material composition of modified low temperature sealing glass is ZnO, Na2O、P2O5、La2O3, its mol ratio is 33
~45：15~25：22~40：5~25.
Prepare and contain La as described above2O3The method of modified low temperature sealing glass comprises the following steps：
（1）Raw material is well mixed；Founded by 880-1100 DEG C, soaking time 1-4 hours；To the glass metal melted, enter
Row chilling, obtains glass frit；Then, glass frit is crushed, grinding or ball milling obtain glass powder after sieving；
（2）Glass powder and binding agent, dispersant and solvent are mixed into slurry, ball milling disperses in ball mill；Curtain coating
Shaping, is spontaneously dried, and the idiosome of shape, is made seal glass needed for being then cut into.
The step（2）Binding agent be epoxy resin, methylcellulose, polyvinyl butyral resin, in polyvinyl alcohol
One or more of mixtures.
The step（2）Dispersant be fish oil, polyacrylic acid, polyvinyl alcohol, polyacrylamide in one or more
Mixture.
The step（2）Solvent be water, ethanol, isopropanol, n-butanol, toluene, dimethylbenzene, acetone in one kind or several
The mixture planted.
Seal glass, which is placed in, treats sealing-in position, is heated up in electric furnace with 1-5 DEG C/min speed, 400-500 DEG C of insulation
0.5-1 hours, 500-650 DEG C of isothermal holding is then warming up to 0.5-1 hours with 1-5 DEG C/min speed, that is, completes sealing-in.
Table 1 is the sealing glass composition table in embodiment 1-4（Mole percent）
Embodiment 1：The preparation and sealing-in of material
According to the proportioning of each component of embodiment 1 in table 1, a certain amount of analysis pure raw material is weighed（ZnO、Na2O、P2O5、
La2O3）, it is well mixed within 24 hours with planetary ball mill ball milling；Then powder is put into platinum crucible, is placed in chamber type electric resistance furnace
In air atmosphere, 900 DEG C are heated to 3 DEG C/min, 1 hour is incubated；Then, crucible is taken out, melt is poured into deionized water
Chilling, dries the fragment for obtaining glass melt；Grinding, crosses 100 mesh sieves, obtains glass powder.By glass dust and polyvinyl alcohol, fish
Oil, ethanol and toluene（Weight ratio is followed successively by 80%, 2%, 1%, 10%, 7%）Slurry is mixed into, ball milling disperses in ball mill；
Flow casting molding, is spontaneously dried, the idiosome of shape needed for being then cut into；Idiosome is placed in and treats sealing-in position, with 2 in electric furnace
DEG C/heating of min speed, 1 hour is incubated at 400 DEG C, 500 DEG C of isothermal holdings 1 are then warming up to 2 DEG C/min speed small
When, that is, complete sealing-in.The example is to preferably constitute.Melt after insulation is poured into the stainless steel grinding tool after preheating, acquisition Φ=
10mm, d=25mm glass cylinder, are tested on NETZSCH DIL 402EP thermal dilatometers with the 10 DEG C/min rate of heat addition,
Obtain glass transition point and softening point.Fig. 1,2 show, add the La of 5% molar fraction2O3The glass transition point of seal glass be
359 DEG C, softening point is 374 DEG C, and linear expansion coefficient is 1.42 × 10-5/K.Weightlessness after being placed 1000 hours in 80 DEG C of hot water
Rate is less than 0.001%.
Embodiment 2：The preparation and sealing-in of material
According to the proportioning of each component of embodiment 2 in table 1, a certain amount of analysis pure raw material is weighed（ZnO、Na2O、P2O5、
La2O3）, it is well mixed within 24 hours with planetary ball mill ball milling；Then powder is put into platinum crucible, is placed in chamber type electric resistance furnace
In air atmosphere, 950 DEG C are heated to 3 DEG C/min, 1 hour is incubated；Then, crucible is taken out, melt is poured into deionized water
Chilling, dries the fragment for obtaining glass melt；Grinding, crosses 100 mesh sieves, obtains glass powder.By glass dust and methylcellulose,
Polyvinyl alcohol, n-butanol and acetone（Weight ratio is followed successively by 82%, 2%, 2%, 8%, 6%）Slurry is mixed into, ball milling is equal in ball mill
It is even scattered；Flow casting molding, is spontaneously dried, the idiosome of shape needed for being then cut into；Idiosome is placed in and treats sealing-in position, in electric furnace
In heated up with 2 DEG C/min speed, be incubated 1 hour at 400 DEG C, 500 DEG C of isothermal holdings be then warming up to 2 DEG C/min speed
1 hour, that is, complete sealing-in.The example is to preferably constitute.Melt after insulation is poured into the stainless steel grinding tool after preheating, Φ is obtained
=10mm, d=25mm glass cylinder, are tested on NETZSCH DIL 402EP thermal dilatometers with the 10 DEG C/min rate of heat addition,
Obtain glass transition point and softening point.Fig. 1,2 show, add the La of 10% molar fraction2O3Seal glass glass transition point
For 384 DEG C, softening point is 405 DEG C, and linear expansion coefficient is 1.41 × 10-5/K.Mistake after being placed 1000 hours in 80 DEG C of hot water
Rate is less than 0.001% again.
Embodiment 3：The preparation and sealing-in of material
According to the proportioning of each component of embodiment 3 in table 1, a certain amount of analysis pure raw material is weighed（ZnO、Na2O、P2O5、
La2O3）, it is well mixed within 24 hours with planetary ball mill ball milling；Then powder is put into platinum crucible, is placed in chamber type electric resistance furnace
In air atmosphere, 1000 DEG C are heated to 3 DEG C/min, 1 hour is incubated；Then, crucible is taken out, melt is poured into deionized water
Chilling, dries the fragment for obtaining glass melt；Grinding, crosses 100 mesh sieves, obtains glass powder.By glass dust and epoxy resin, gather
Acrylamide, isopropanol and toluene（Weight ratio is followed successively by 84%, 1.5%, 0.5%, 9%, 5%）Slurry is mixed into, the ball in ball mill
Mill is dispersed；Flow casting molding, is spontaneously dried, the idiosome of shape needed for being then cut into；Idiosome is placed in and treats sealing-in position,
Heated up in electric furnace with 2 DEG C/min speed, be incubated 1 hour at 450 DEG C, 550 DEG C of insulations are then warming up to 2 DEG C/min speed
Processing 1 hour, that is, complete sealing-in.The example is to preferably constitute.Melt after insulation is poured into the stainless steel grinding tool after preheating, obtained
Obtain Φ=10mm, d=25mm glass cylinder, with the 10 DEG C/min rate of heat addition on NETZSCH DIL 402EP thermal dilatometers
Test, obtains glass transition point and softening point.Fig. 1,2 show, add the La of 15% molar fraction2O3Seal glass glass
Transition point is 400 DEG C, and softening point is 419 DEG C, and linear expansion coefficient is 1.38 × 10-5/K.Placed 1000 hours in 80 DEG C of hot water
Weight-loss ratio afterwards is less than 0.001%.
Embodiment 4：The preparation and sealing-in of material
According to the proportioning of each component of embodiment 4 in table 1, a certain amount of analysis pure raw material is weighed（ZnO、Na2O、P2O5、
La2O3）, it is well mixed within 24 hours with planetary ball mill ball milling；Then powder is put into platinum crucible, is placed in chamber type electric resistance furnace
In air atmosphere, 1050 DEG C are heated to 3 DEG C/min, 1 hour is incubated；Then, crucible is taken out, melt is poured into deionized water
Chilling, dries the fragment for obtaining glass melt；Grinding, crosses 100 mesh sieves, obtains glass powder.Glass dust and polyvinyl alcohol are contracted
Butyraldehyde, polyacrylic acid, isopropanol and acetone（Weight ratio is followed successively by 83%, 2%, 1%, 9%, 5%）Slurry is mixed into, in ball mill
Ball milling disperses；Flow casting molding, is spontaneously dried, the idiosome of shape needed for being then cut into；Idiosome is placed in and treats sealing-in position,
Heated up in electric furnace with 2 DEG C/min speed, be incubated 1 hour at 450 DEG C, 550 DEG C of guarantors are then warming up to 2 DEG C/min speed
Temperature processing 1 hour, that is, complete sealing-in.The example is to preferably constitute.Melt after insulation is poured into the stainless steel grinding tool after preheating,
Obtain Φ=10mm, d=25mm glass cylinder, with 10 DEG C/min heating speed on NETZSCH DIL 402EP thermal dilatometers
Rate is tested, and obtains glass transition point and softening point.Fig. 1,2 show, add the La of 20% molar fraction2O3Seal glass glass
Transition point is 418 DEG C, and softening temperature is 440 DEG C, and linear expansion coefficient is 1.37 × 10-5/K.1000 are placed in 80 DEG C of hot water small
When after weight-loss ratio be about 0.001%.
The present invention is obtained by above-mentioned implementation can implement the La of sealing-in in low temperature2O3Modified seal glass.Its significant effect
Embodying a concentrated reflection of has good stability in use environment, it is adaptable to LED fluorescent powder sealing-in, electronic material and other low temperature
Sealing-in field.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, should all belong to the covering scope of the present invention.
Claims (7)
1. a kind of La2O3Modified low temperature sealing glass, it is characterised in that：Raw material composition is ZnO, Na2O、P2O5、La2O3, it rubs
You are than being 33 ~ 45：15~25：22~40：5~25.
2. La according to claim 12O3Modified low temperature sealing glass, it is characterised in that：Raw material ZnO, Na2O、P2O5、
La2O3Mol ratio be 38 ~ 40.5：18~22：27~29.5：10~15.
3. one kind prepares La as claimed in claim 12O3The method of modified low temperature sealing glass, it is characterised in that：Including with
Lower step：
（1）Raw material is well mixed；Founded by 880-1100 DEG C, soaking time 1-4 hours；To the glass metal melted, enter
Row chilling, obtains glass frit；Then, glass frit is crushed, grinding or ball milling obtain glass powder after sieving；
（2）Glass powder and binding agent, dispersant and solvent are mixed into slurry, ball milling disperses in ball mill；Curtain coating
Shaping, is spontaneously dried, and the idiosome of shape, is made seal glass needed for being then cut into.
4. La according to claim 32O3The preparation method of modified low temperature sealing glass, it is characterised in that：The step
（2）Binding agent be epoxy resin, methylcellulose, polyvinyl butyral resin, one or more of mixing in polyvinyl alcohol
Thing.
5. La according to claim 32O3The preparation method of modified low temperature sealing glass, it is characterised in that：The step
（2）Dispersant be fish oil, polyacrylic acid, polyvinyl alcohol, polyacrylamide in one or more of mixtures.
6. La according to claim 32O3The preparation method of modified low temperature sealing glass, it is characterised in that：The step
（2）Solvent be water, ethanol, isopropanol, n-butanol, toluene, dimethylbenzene, acetone in one or more of mixtures.
7. a kind of La as claimed in claim 12O3The application method of modified low temperature sealing glass, it is characterised in that：By sealing-in
Glass, which is placed in, treats sealing-in position, is heated up in electric furnace with 1-5 DEG C/min speed, and 400-500 DEG C is incubated 0.5-1 hours, then
500-650 DEG C of isothermal holding is warming up to 0.5-1 hours with 1-5 DEG C/min speed, that is, completes sealing-in.
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| CN201710273036.0A CN107043215A (en) | 2017-04-25 | 2017-04-25 | A kind of low temperature sealing glass of lanthana modification and its preparation and application method |
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| CN201710273036.0A CN107043215A (en) | 2017-04-25 | 2017-04-25 | A kind of low temperature sealing glass of lanthana modification and its preparation and application method |
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Cited By (2)
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| CN111003945A (en) * | 2019-12-30 | 2020-04-14 | 西安赛尔电子材料科技有限公司 | Preparation method of sealing glass material and sealing process thereof |
| CN111170639A (en) * | 2019-12-30 | 2020-05-19 | 西安赛尔电子材料科技有限公司 | Glass material for sensor sealing and preparation method thereof |
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