CN103539354B - Frit composition of sealed light-emitting device, as well as preparation method and air-tight sealing method - Google Patents
Frit composition of sealed light-emitting device, as well as preparation method and air-tight sealing method Download PDFInfo
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Abstract
The invention provides a frit composition of a sealed light-emitting device, as well as a preparation method and an air-tight sealing method. The frit composition comprises the following components in molar percentage: 20-40% of V2O5, 30-60% of TeO2, 0-10% of ZnO, 10-20% of Co2O3 and 0-5% of GeO2. The preparation method of the frit composition comprises the following steps of sintering oxide powder, and obtaining glass beads along with water quenching of the molten oxide powder; crushing the obtained glass beads to form the frit composition in glass particle morphology, wherein the oxide powder comprises the following components in molar percentage: 20-40% of V2O5, 30-60% of TeO2, 0-10% of ZnO, 10-20% of Co2O3 and 0-5% of GeO2. By adopting the frit composition provided by the invention, air-tight packaging with high sealing strength can be obtained, and environmental pollution can be avoided.
Description
Technical field
The present invention relates to encapsulant technical field, more particularly to a kind of glass frit compositions of sealing luminescent device and
Preparation method, method for hermetic sealing.
Background technology
Glass frit compositions be applied to as the class intermediate materials that substrate is sealed luminescent device envelope
Connect, so that the inside of luminescent device and ambient environment, it is to avoid luminescent device is affected by the ambient and makes performance
Decline.
Luminescent device, such as organic electroluminescence device, have obtained increasing concern and extensive application.In Organic Electricity
In electroluminescence device, display of organic electroluminescence oled as a kind of emerging flat faced display color contrast, visual angle,
The aspect such as response speed and energy consumption is respectively provided with potential advantage, and glass frit compositions are particularly heavy for the performance of luminescent device
Will.
However, traditional glass frit compositions contain the noxious substances such as vanadic anhydride, to absorb realization as absorbent
The laser of base plate seals, and in the case that glass frit compositions fusion temperature is relatively low, thermal coefficient of expansion raises, and forms sealing-in
When crackle and subside, there is the not high defect of sealing intensity.
Content of the invention
Based on this, be provided with a kind of sealing intensity higher, free of contamination sealing luminescent device glass frit compositions.
Additionally, there is a need to offer, a kind of sealing intensity is high, the preparation method of free of contamination glass frit compositions.
In addition, there is a need to offer, a kind of sealing intensity is high, the free of contamination encapsulating method based on glass frit compositions.
The glass frit compositions of above-mentioned sealing luminescent device and preparation method, method for hermetic sealing pass through to introduce co2o3, with
co2o3As absorb laser main additive is nontoxic and good absorbing effect, so that glass frit compositions is obtained relatively as a kind of glass
Obtain relatively low thermal coefficient of expansion (cte) while low fusion temperature, and then ensure that between glass frit compositions and substrate
Good wettability, applying above-mentioned glass frit compositions that substrate is carried out with sealing-in will be high for the sealing intensity that ensure that sealing-in, no dirty
Dye.
Brief description
Fig. 1 is the flow chart of the preparation method of the glass frit compositions of an embodiment；
Fig. 2 is the flow chart of the encapsulating method based on glass frit compositions of an embodiment；
Fig. 3 is the cte of the glass frit compositions of an embodiment and the relation schematic diagram of melting temperature.
Specific embodiment
With reference to embodiment and accompanying drawing, glass frit compositions to sealing luminescent device and preparation method, airtight close
Encapsulation method is described in further detail.
One embodiment sealing luminescent device glass frit compositions be a kind of glass, according to molar percentage include with
Lower component: 20-40v2o5、30-60teo2、0-10zno、10-20co2o3、0-5geo2.
In preferred embodiment, v in glass frit compositions2o5And teo2With the mixing of the molar ratio of 4:6, and zno and
geo2Molar percentage be not zero.
In the present embodiment, v2o5And teo2Between molar ratio be 4:6 when melting temperature be up to minimum, but expand
Coefficient is larger, now, adds geo2The coefficient of expansion will be significantly reduced with zno.
Further, in glass frit compositions, the molar percentage of each component is 32 v2o5、48 teo2、4.5 zno、13
co2o3、2.5 geo2When be up to best material result, that is, melting temperature and thermal coefficient of expansion all reach reduced levels.
The glass frit compositions of above-mentioned sealing luminescent device are by introducing co2o3, with co2o3As the master absorbing laser
Want additive nontoxic and good absorbing effect, make glass frit compositions obtain obtaining while relatively low fusion temperature as a kind of glass
To relatively low thermal coefficient of expansion (cte), and then ensure that good wettability between glass frit compositions and substrate, application is above-mentioned
Glass frit compositions carry out sealing-in to substrate will be high, pollution-free for the sealing intensity that ensure that sealing-in.
Traditional glass frit compositions are so that melting temperature maintains slightly lower temperature and makes thermal coefficient of expansion very
Height is it is impossible to obtain the glass frit compositions compared with low melting point temperature and relatively low thermel expansion coefficient simultaneously, and above-mentioned glass frit compositions
Do not need to add any fire resistant infilling and can reach and melt the low and low feature of thermal coefficient of expansion it is ensured that relatively low thermal expansion system
The material of number and substrate matches and obtains preferable sealing effectiveness.
Refer to Fig. 1, the preparation method of the glass frit compositions of an embodiment, comprise the following steps:
S110, sintered oxide powder, and obtain bead with the oxide powder water quenching of melting.
In the present embodiment, oxide powder includes following components: 420-40 v according to molar percentage2o5、30-60
teo2、0-10 zno、10-20 co2o3、0-5 geo2.
Molar percentage weighs a certain amount of v as described above2o5、teo2、zno、co2o3、geo2Mutually it is mixed to get
Oxide powder, oxide powder is placed in high temperature furnace the oxide powder that sintering obtains molten condition, and by molten
The oxide powder of state is poured into water and carries out water quenching formation bead.
S130, pulverizes the glass frit compositions that the bead obtaining forms glass particle form.
In the present embodiment, the average particle size distribution pulverizing the glass frit compositions of bead form obtaining is less than 5 microns.
Mode for pulverizing bead can be ball milling, grinding or other suitable mode.
In the preparation method of the glass frit compositions of other embodiment, after above-mentioned steps s130, also include selecting crude drugs with winnower and obtain
Step to the glass frit compositions being consistent with presetting granularity distribution.
In the present embodiment, this glass frit compositions makes melting temperature and thermal coefficient of expansion relatively low, the wettability with substrate
Well.
Refer to Fig. 2, the encapsulating method based on glass frit compositions of an embodiment, comprise the following steps:
S210, glass frit compositions are deposited on substrate.
In the present embodiment, glass frit compositions include following components: 20-40 v according to molar percentage2o5、30-60
teo2、0-10 zno、10-20 co2o3、0-5 geo2.
First substrate and second substrate are provided, by the modes such as silk screen printing make glass frit compositions be deposited on substrate it
On, this substrate is second substrate；Pre- laminating first substrate and second substrate are so that be deposited on the glass frit composition of second substrate
Thing is placed between first substrate and second substrate.
S230, the substrate that presintering deposited glass frit compositions obtains prefabricated component.
In the present embodiment, in 400 DEG C, presintering, wherein, presintering are carried out to the substrate that deposited glass frit compositions
Atmosphere can be any one in noble gases, reducibility gas or low oxygen atmosphere environment.This low oxygen atmosphere environment institute
Oxygenous will be less than 5%, aoxidized with the transition preventing oxide in glass frit compositions.
Compared with traditional glass frit compositions, due to traditional glass frit compositions need 450 DEG C environment it
Under carry out presintering, and glass frit compositions as above only need to complete presintering process at 400 DEG C, it is to avoid mistake
Pyrolytic damage caused by high temperature.
S250, forms the hermetic between substrate by radiation source sealing-in prefabricated component.
In the present embodiment, this radiation source can be any one in laser, infrared ray and microwave.By radiation source heats
Glass frit compositions form strip of paper used for sealing so that glass frit compositions are melted, and by two substrate connections, that is, first substrate is connected to the
On two substrates.
In the sealing means based on glass frit compositions of another embodiment, glass frit compositions are mixed with organic binder bond
Close, before above-mentioned s230, the method also includes:
The substrate that deposited glass frit compositions is heated to 300 DEG C -350 DEG C, and stops Preset Time, burn out organic viscous
Knot agent.
In the present embodiment, during the substrate that deposited glass frit compositions is heated, in heating-up temperature liter
Stop Preset Time to when 300 DEG C -350 DEG C, so that organic binder bond total number during presintering burns out.
The above-mentioned encapsulating method based on glass frit compositions, absorbs radiation source by glass frit compositions and reaches in substrate
The effect of local heating, can be used for realizing the air hermetic encapsulation in thin-film device or organic luminescent device, with by stronger close
Envelope property ensures the performance of thin-film device or organic luminescent device.
To illustrate below in conjunction with specific embodiment.
Embodiment 1
Preparation glass frit compositions, it includes following components: 20 v according to molar percentage2o5、60 teo2、15 co2o3、
5 zno.
Weigh v according to as above molar percentage2o5、teo2、co2o3, zno, and be mixed to get oxide powder, be placed in high temperature
Sintering obtains the oxide powder of molten condition in stove, and the oxide powder of molten condition is poured into water carries out water quenching and obtain
Bead；
Pulverize the bead obtaining to obtain the glass frit composition that average particle size distribution is less than 5 microns of glass particle form
Thing, and the granule of required each particle size distribution is selected by selecting crude drugs with winnower.
The melting temperature of this glass frit compositions preparing is 391 DEG C, and thermal coefficient of expansion is 92.4.
Embodiment 2
Preparation glass frit compositions, it includes following components: 30 v according to molar percentage2o5、45 teo2、20 co2o3、
5 geo2.
Weigh v according to as above molar percentage2o5、teo2、co2o3、geo2, and it is mixed to get oxide powder, it is placed in height
Sintering obtains the oxide powder of molten condition in warm stove, and the oxide powder of molten condition is poured into water carries out water quenching and obtain
To bead；
Pulverize the bead obtaining to obtain the glass frit composition that average particle size distribution is less than 5 microns of glass particle form
Thing, and the granule of required each particle size distribution is selected by selecting crude drugs with winnower.
The melting temperature of this glass frit compositions preparing is 335 DEG C, and thermal coefficient of expansion is 104.8.
Embodiment 3
Preparation glass frit compositions, it includes following components: 40 v according to molar percentage2o5、30 teo2、15 co2o3、
10 zno、5 geo2.
Weigh v according to as above molar percentage2o5、teo2、co2o3、geo2, and it is mixed to get oxide powder, it is placed in height
Sintering obtains the oxide powder of molten condition in warm stove, and the oxide powder of molten condition is poured into water carries out water quenching and obtain
To bead；
Pulverize the bead obtaining to obtain the glass frit composition that average particle size distribution is less than 5 microns of glass particle form
Thing, and the granule of required each particle size distribution is selected by selecting crude drugs with winnower.
The melting temperature of this glass frit compositions preparing is 372 DEG C, and thermal coefficient of expansion is 87.5.
Embodiment 4
Preparation glass frit compositions, it includes following components: 32 v according to molar percentage2o5、48 teo2、13 co2o3、
4.5 zno、2.5 geo2.
Weigh v according to as above molar percentage2o5、teo2、co2o3、zno、geo2, and it is mixed to get oxide powder, put
In high temperature furnace, sintering obtains the oxide powder of molten condition, and the oxide powder of molten condition is poured into water carries out water
Quench and obtain bead；
Pulverize the bead obtaining to obtain the glass frit composition that average particle size distribution is less than 5 microns of glass particle form
Thing, and the granule of required each particle size distribution is selected by selecting crude drugs with winnower.
The melting temperature of this glass frit compositions preparing is 357 DEG C, and thermal coefficient of expansion is 81.2.
Embodiment 5
Preparation glass frit compositions, it includes following components: 32 v according to molar percentage2o5、49 teo2、10 co2o3、
5.5 zno、2.5 geo2.
Weigh v according to as above molar percentage2o5、teo2、co2o3、zno、geo2, and it is mixed to get oxide powder, put
In high temperature furnace, sintering obtains the oxide powder of molten condition, and the oxide powder of molten condition is poured into water carries out water
Quench and obtain bead；
Pulverize the bead obtaining to obtain the glass frit composition that average particle size distribution is less than 5 microns of glass particle form
Thing, and the granule of required each particle size distribution is selected by selecting crude drugs with winnower.
The melting temperature of this glass frit compositions preparing is 360 DEG C, and thermal coefficient of expansion is 84.1.
Refer to Fig. 3, Fig. 3 show embodiment 1～embodiment 5 preparation the melting temperature of glass frit compositions and heat swollen
The test result of swollen coefficient (cte).As can be seen from Figure 3 the fusing point of the glass frit compositions of embodiment 1～embodiment 5 preparation
Temperature and thermal coefficient of expansion are all relatively low, can effectively reduce in surrounding for example outside aqueous vapor etc. to thin-film device or organic
The erosion of optical device, thus improve performance and the life-span of thin-film device or organic luminescent device.
Embodiment described above only have expressed the several embodiments of the present invention, and its description is more concrete and detailed, but simultaneously
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, some deformation can also be made and improve, these broadly fall into the guarantor of the present invention
Shield scope.Therefore, the protection domain of patent of the present invention should be defined by claims.
Claims (10)
1. a kind of glass frit compositions of sealing luminescent device are it is characterised in that include following components according to molar percentage:
20-40v2o5、30-60teo2、0-10zno、10-20co2o3、0-5geo2, and zno and geo2Molar percentage be not zero.
2. the glass frit compositions of sealing luminescent device according to claim 1 are it is characterised in that described glass frit composition
V described in thing2o5And teo2Molar ratio mixing with 4:6.
3. the glass frit compositions of sealing luminescent device according to claim 1 are it is characterised in that described glass frit composition
In thing, the molar percentage of various components is: 32v2o5、48teo2、4.5zno、13co2o3、2.5geo2.
4. a kind of preparation method of glass frit compositions is it is characterised in that comprise the steps:
Sintered oxide powder, and obtain bead with the oxide powder water quenching of melting；
The bead obtaining described in pulverizing forms the glass frit compositions of glass particle form；
Wherein, described oxide powder includes following components according to molar percentage: 20-40v2o5、30-60teo2、0-10zno、
10-20co2o3、0-5geo2, and zno and geo2Molar percentage be not zero.
5. the preparation method of glass frit compositions according to claim 4 is it is characterised in that in described glass frit compositions
Described v2o5And teo2Molar ratio mixing with 4:6.
6. the preparation method of glass frit compositions according to claim 5 is it is characterised in that in described glass frit compositions
The molar percentage of various components is: 32v2o5、48teo2、4.5zno、13co2o3、2.5geo2.
7. the preparation method of glass frit compositions according to claim 4 is it is characterised in that obtain described in described pulverizing
After bead forms the step of glass frit compositions of glass particle form, methods described also includes:
Selecting crude drugs with winnower obtains the step being distributed the glass frit compositions being consistent with presetting granularity.
8. a kind of encapsulating method based on glass frit compositions is it is characterised in that comprise the steps:
Glass frit compositions are deposited on substrate；
The substrate that deposited glass frit compositions described in presintering obtains prefabricated component；
Hermetic between described substrate is formed by prefabricated component described in radiation source sealing-in；
Described glass frit compositions include following components according to molar percentage: 20-40v2o5、30-60teo2、0-10zno、10-
20co2o3、0-5geo2, and zno and geo2Molar percentage be not zero.
9. the encapsulating method based on glass frit compositions according to claim 8 is it is characterised in that described glass frit composition
Thing is mixed with organic binder bond, deposited described in described presintering glass frit compositions substrate obtain prefabricated component step it
Before, methods described also includes:
The described substrate that deposited glass frit compositions is heated to 300 DEG C -350 DEG C, and stops Preset Time, have described in burning-up
Machine binding agent.
10. the encapsulating method based on glass frit compositions according to claim 8 is it is characterised in that described frit group
V described in compound2o5And teo2Ratio mixing with 4:6.
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| WO2011130632A1 (en) * | 2010-04-15 | 2011-10-20 | Ferro Corporation | Low-melting lead-free bismuth sealing glasses |
| CN102452794A (en) * | 2010-10-27 | 2012-05-16 | 郑庆云 | Crystalline low-melting-point sealing glass and preparation method thereof |
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