CN104628256A - Low-melting-point frit and electrical component sealing method utilizing the same - Google Patents
Low-melting-point frit and electrical component sealing method utilizing the same Download PDFInfo
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- CN104628256A CN104628256A CN201310557006.4A CN201310557006A CN104628256A CN 104628256 A CN104628256 A CN 104628256A CN 201310557006 A CN201310557006 A CN 201310557006A CN 104628256 A CN104628256 A CN 104628256A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
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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
Abstract
The invention describes a frit paste composition and a preparation method, and more specifically relates to a low-melting-point frit paste composition suitable for protection of organic light emitting diode (OLED) components. The invention also provides a method for air hermetic sealing of electrical components by the frit paste composition. The frit and the electrical component sealing method utilizing the frit provided by the invention can achieve excellent sealing effect on water vapor and gas, and can easily process electrical components at low temperature.
Description
Technical field
The present invention relates to a kind of low melting glass material paste composition; more specifically; disclosed herein the preparation method of frit, and use frit paste composition to manufacture and sealing plane panel by typography, and the method for the element protecting thermotolerance more weak.Described electrical element, includes OLED (OLED), dye sensitization solar battery (DSSC), lighting (LED).The present invention adopts OLED display to set forth as an example.
Background technology
Organic electroluminescent LED (Organic light emitting diode, OLED) display of organic electroluminescence is also called, its structure belongs to sandwich type structure, usually being made up of anode, hole injection layer, hole transmission layer, luminescent layer, electron transfer layer and negative electrode etc., is a kind of total solids indicating meter utilizing current drives.Under the driving of impressed current, electronics and hole carrier are injected into leads organic luminous layer, then in luminescent layer, is compounded to form exciton, is sent out and luminous by exciton radiation de excitation.Due to OLED there is frivolous, power saving, wide viewing angle, image quality is even, speed of response is fast, can realize the features such as Flexible Displays, be acknowledged as " dreamlike indicating meter ".
But OLED is a kind of device to steam and oxygen extreme sensitivity, as long as OLED does not encapsulate, just easily cause stain at light-emitting zone, and stain can expand along with the time.On the one hand, penetrate into the steam of device and oxygen can with the low workfunction metal material of device cathodes, there is oxidizing reaction in such as Al, Mg, Ca etc., causes forming insulation layer at negative electrode and organic functions interlayer, causes device cannot be luminous.Meanwhile, during OLED work, the existence of steam can bring out the electrolysis venting that electrochemical reaction and water occur between anode and negative electrode, forms blackspot.On the other hand, also can there is irreversible chemical reaction with steam, oxygen in organic materials, destroys the stability of organic molecule, reduces device light emitting efficiency.Therefore, in order to protect OLED from steam and oxygen deterioration of device performance, above-mentioned OLED display being carried out gas-tight seal and will seem very important.
The prevailing method of above-mentioned OLED display being carried out to gas-tight seal is exactly by after UV treatment, uses epoxide, inorganic substance or the/organic substance that can form sealing.Such as, Vitex system company develops a kind of Barix encapsulation technology, adopts the alternating layer of inorganic materials and organic materials to seal OLED display.Although this sealing method can provide and good physical strength, their equipment costs are very expensive, and in a lot of occasion, these sealings fail anti-sealing Oxygen permeation in OLED display.
Another common method being used for sealing OLED display adopts metal solder or soft soldering exactly.But, owing to there is substantial difference between glass substrate and the CTE of metal in above-mentioned OLED display, so the OLED display adopting metal solder is non-resistant in wide temperature range.
Based on the hermetic sealing technology of frit, especially leaded frit, for the device of encapsulation provides excellent resistance to air loss.But these frits comprise toxic element mostly, as antimony (Sb) and plumbous (Pb), all environmental hazard can be caused.Such as, Chinese patent CN200810182354.7 discloses a kind of frit paste composition based on P2O5-V2O5-ZnO and carrys out hermetically sealing electrical element, but the shortcoming of this frit paste composition is, containing a certain amount of Sb2O3 oxide compound, can cause environmental pollution.Therefore, developing the frit of a kind of Environment-friendlylow-temperature low-temperature welding, is very urgent.
Above-mentioned disclosed in background information be only used to strengthen understanding to background technology of the present invention, therefore, it may comprise the information not being formed in this domestic prior art well known by persons skilled in the art.
Summary of the invention
Main purpose of the present invention is to provide a kind of environment-friendly low-melting point frit and the frit paste composition containing this frit, to solve the problem.
In the periodic table of elements, because lead and bismuth are two adjacent elements, they all belong to the P district in the 6th cycle, have very similar character.And containing the two glass in viscosity, transition temperature Tg, the aspects such as the coefficient of expansion must be similar.In addition, antimony and bismuth are again congenerss, and chemical property is comparatively close.So current bismuth glass material is the excellent substitute of lead glass material.In addition, carry out the Bi2O3 of Substitute For Partial with boron oxide and zinc oxide, the mobility of glass system can not only be increased, reduce the fusing point of frit system, and increase chemical stability and the glass formation range of frit system due to boron oxide.
To achieve these goals, the invention provides a kind of lead-less glasses material, it is characterized in that, it contains:
Bi2O3(70-80wt％)，
B2O3(5-15wt％)，
ZnO(5-10wt％)，
CuO(0-15wt％)，
MnO2(0-15wt％)，
Fe2O3(0-5wt％)，
BaO (1-5wt%), and
Wherein, CuO+Fe2O3+MnO2, in the scope of 5wt% to 15wt%, is a kind of more satisfactory combination, effectively improves the infrared Absorption of glass frit compositions to 810nm place and has very high absorption cross section, and the existence of a certain amount of Fe2O3 improves the weather resistance of material.
Second object of the present invention is just to provide a kind of preparation method of low melting glass material powder, the method comprised the following steps:
A) prepare burden; Raw material is taken according to composition and ratio;
B) batch mixing: the raw material taken is carried out in shredder mix, grind, until feedstock composition mixes, obtain admixtion;
C) high temperature melting-annealing: admixtion is put into platinum crucible, then the platinum crucible that admixtion is housed is put into resistance furnace to heat, 1000 DEG C-1500 DEG C are progressively risen to by room temperature, and be incubated 6 hours, admixtion is fully melted, obtain glass metal, then described glass metal cast is annealed in a mold, obtain the both bulk glasses of having annealed.
D) grinding and screening: both bulk glasses is smashed to pieces, and allows into grinding machine for grinding 1-6 hour, then by the glass powder after grinding, obtain the frit of low melting point through 400 object screen clothes;
3rd object of the present invention is just to provide a kind of sealing method using this low melting glass material paste composition to carry out hermetically sealing electrical element, first, first glass substrate and the second glass substrate are provided, then by coating process, described frit paste composition is fixed on the predetermined position of the first glass substrate, finally utilize source of radiation (as laser or infrared rays) to carry out heated frit, make it be welded to by the first glass substrate on the second described glass substrate and also form gas-tight seal dam betwixt.
Frit of the present invention is excellent with the sealing effectiveness utilizing the sealing method of the OLED display element of this frit to steam and oxygen, and easily carries out machining at low temperature.
See accompanying drawing; the present invention can be easier to understand by following illustrative description; more clearly understand other objects of the present invention simultaneously, method, feature and advantage are all included within this description, comprise within the scope of the present invention, and be subject to the protection of appended claims.
Accompanying drawing explanation
Be described in detail exemplary embodiment in conjunction with the drawings, feature will become obvious to those skilled in the art, in accompanying drawing:
Fig. 1 illustrates the OLED element seal process schematic diagram utilizing frit paste composition of the present invention;
Fig. 2 illustrates the material loading and sintering process that utilize frit paste composition of the present invention;
Fig. 3 illustrates the process schematic utilizing frit paste composition LASER HEATING OLED element of the present invention;
Wherein, 100 shown in Fig. 3 is the upper surface of the first glass substrate;
Wherein, 200 shown in Fig. 3 is Environment-friendlylow-temperature low-temperature glass for bonding feed composition disclosed in the present invention;
Wherein, 300 shown in Fig. 3 is the upper surface of the second glass substrate.
Embodiment
Illustrative embodiments of the present invention is described below with reference to the accompanying drawings, repeatability will be omitted if desired and describe.
The following detailed description of the present invention.
A kind of low melting glass material paste composition of the present invention, it is characterized in that, it contains:
A) glass frit powder composition: Bi2O3 (70-80wt%), B2O3 (5-15wt%), ZnO (5-10wt%), CuO (0-15wt%), MnO2 (0-15wt%), Fe2O3 (0-5wt%), BaO (1-5wt%), wherein, CuO+Fe2O3+MnO2 is in the scope of 5wt% to 15wt%;
B) filler;
C) organic binder bond, when described organic binder bond has the molecular weight of 10,000g/ mole-300,000g/ moles and dissolves in organic solvent with 1-5wt%, organic paste composition viscosity is 500cps-100,000cps, and
D) organic solvent.
When the content forming the composition of frit of the present invention is outside above-mentioned scope, sometimes can not form vitreum, water tolerance is obviously deteriorated sometimes, is also sometimes unfavorable for the absorption of frit to source of radiation.
Described low melting glass material powder, preferably contains:
Bi2O3(70-75wt％)，
B2O3(5-10wt％)，
ZnO(5-10wt％)，
CuO(1-15wt％)，
MnO2(1-15wt％)，
Fe2O3(1-5wt％)，
BaO (1-5wt%), and
Wherein, CuO+Fe2O3+MnO2 is in the scope of 5wt% to 15wt%.
Below more specifically will set forth, how obtain the preparation method of a low melting glass material.
Low melting glass material, first adopts the basic components system of binary (Bi2O3-B2O3) to form the Network former of frit.Bismuth oxide and boron oxide mainly define the unit of frit network body, and be highly stable vitreous structure, physical strength is good, and stable chemical nature.Adopt zinc oxide to adulterate bismuth oxide and boron oxide system, modification can be carried out to above-mentioned Bi2O3-B2O3 bis-tuple, greatly enhance the sintering mobility of glass frit compositions, reduce the glass transition temp of frit.Such as, when in above-mentioned frit, the content of ZnO component is less than 5wt%, frit paste composition often has more high softening temperature Tdsp.This is mainly because the ZnO component of high-content has part to provide the ability of free oxygen in frit Network former system, the fracture of the old key of glass network and the restructuring of new key is made to become relatively easy, thus have the benefit of fluxing, the mobility of frit is also better, can Some substitute Bi2O3.Contrary, if when the ZnO component in above-mentioned glass frit compositions is higher than 10wt%, ZnO high-content causes the network contiguity in whole glass network former greatly to reduce, the weaken of frit, is unfavorable for obtaining the good frit of welding strength.
Then, from all the other components to the water tolerance of gas-tight seal frit, sintering mobility, glass transition temp Tg, frit degree of absorption and thermal expansivity confirm that other material forms.
In order to improve the absorption of frit to corresponding wave band, all need to increase suitable extinction component, these extinction components freely comprise CuO, Fe2O3, V2O5, the transition metal oxides such as TiO2, the material of one or two or more kinds composition in the group that rare-earth oxide (lanthanide metal oxide) forms.
In the present invention, absorbancy can be expressed as:
β＝-log
10[T／(1-R)
2]／t
Wherein, β refers to specific absorbance, and T is exactly the ratio of the light of t after being transmitted through, and R is then the reflectivity of frit.Generally speaking, the specific absorbance adding the frit of transition metal or rare-earth oxide should be able to be greater than 2/mm.And include Fe2O3, the frit of V2O5 and TiO2 has the specific absorbance of more than 33/mm.
The low melting glass material that the present invention discloses, includes:
CuO(1-15wt％)，
MnO2(1-15wt％)，
Fe2O3 (1-5wt%), wherein, CuO+Fe2O3+MnO2 is in the scope of 5wt% to 15wt%.The combination of these components is very good to the receptivity of the Infrared at 810nm place.
In addition, when the content of the B component aO in above-mentioned frit is less than 1wt%, there is the problem that softening point temperature increases in described glass frit compositions, because the barium ion of divalence, be free on outside glass network former, have very strong polarizability, the Network former link level in frit is died down, softening temperature reduces.Contrary, when the content of the B component aO in above-mentioned frit is higher than 5wt%, is unfavorable for the stable of frit, sometimes devitrification occurs.
According to low melting glass material paste composition of the present invention, it is characterized in that, containing b) filler, primary chemical formula is Al2O3 and SiO2.The content of filler, in order to regulate glass frit compositions at the thermal expansivity of sintering process, improves the bonding strength of glass frit compositions and the first glass substrate and the second glass substrate, prevents distortion and part cracking, and protects metal electrode.
According to low melting glass material paste composition of the present invention, it is characterized in that, it contains c) organic adhesive, described organic binder bond has 10,000g/ moles-300, the molecular weight of 000g/ mole and when dissolving in organic solvent with 1-5wt%, organic paste composition viscosity is 500cps-100,000cps.Organic binder bond, freely comprises EC cellulose-based, AC acrylic resin, or PC gathers at least one material in alkyl carbonate system.
According to low melting glass material paste composition of the present invention, it is characterized in that, it contains d) organic solvent.The selection of described organic solvent, must consider organic binder bond and can be dissolved in organic solvent.Organic solvent of the present invention can be acetate of butyl carbitol (BCA), terpinol (TPN), dibutyl phthalate (DBP), or 2,2,4-trimethylammonium-1.3 pentanediol mono isobutyrate (texanol alcohol ester), or triglyme (triglyme) or their composition group in one or two kinds.Caking agent/the organic solvent used in the present invention can be EC ethyl cellulose/BCA acetate of butyl carbitol, AC acrylic resin/2,2,4-trimethylammonium-1.3 pentanediol mono isobutyrate (texanol alcohol ester), or zinc-containing solid catalyst (Polyalkylene Carbonate)/triglyme.Meanwhile, the viscosity of frit paste composition depends on that the ratio of organic binder bond and organic solvent is how many.
The feature of above-mentioned frit paste composition is, its viscosity is 500cps-100,000cps, preferred 2000cps-100,000cps.The viscosity of frit paste composition has impact to a certain extent for the yield of its gas-tight seal on the first glass substrate and the second glass substrate.When the viscosity of frit paste composition is lower than 500cps, frit paste composition, in silk screen printing process, extremely easily penetrates half tone and cannot reach the ideal thickness of frit.When the viscosity of frit paste composition is higher than 100,000cps, caking agent just directly adheres on half tone, and returning in black technique in printing, sometimes can cause the plug-hole phenomenon of silk-screen half tone.Meanwhile, when the viscosity of frit paste composition is higher than 100,000cps, the surface topography of frit on the first glass substrate also can be uneven, and the drop of high lower is very big, has a great impact the yield of follow-up gas-tight seal.
According to low melting glass material paste composition of the present invention, it contains:
A) glass frit powder of 50wt%-90wt%;
B) filler of 1wt%-15wt%;
C) organic binder bond of 1wt%-5wt%, when described organic binder bond has the molecular weight of 10,000g/ mole-300,000g/ moles and dissolves in organic solvent with 1-5wt%, organic paste composition viscosity is 500cps-100,000cps; With
D) organic solvent of 5wt%-45wt%.
Except the number of component in glass frit compositions, outside having a great impact the gas-tight seal of OLED, in composition, the size of particle is also very important.The particle of the frit of the present invention containing such composition is preferably had to the size of 0.1um-20um.When the particle diameter of frit components is less than 20um, because it has very little particle diameter, frit has very high specific surface area, and the surface energy of its system is very high, and therefore whole frit system has and reduces surface-area, reduce the demand of energy in frit system, just obtain enough outside abilities at reduced temperatures, the particle in glass powder will overcome migration activation energy, draws close mutually and forms new network body, thus comparatively speaking, the sintering process in frit is conducive to.Generally speaking, the size of frit particles, in above-mentioned scope, is applicable to low-temperature sintering, is applicable to the gas-tight seal of heat labile element, and can be used in follow-up radiation source heats, improves the fine ratio of product of OLED display.
As the concrete example of low melting glass material paste composition of the present invention, material preparation flow will be described in detail below.
A) prepare burden: according to aforesaid method, by the frit system component confirmed, extinction component and other adjustment component take according to a certain percentage.
B) batch mixing: by each frit components above-mentioned, put into shredder and fully grind, dispersion, then grinds, in dispersion, until within the granular size of each component is roughly 20um.Shredder can be conventional three-roller, utilizes the shearing force under different rotating speeds and the gap between adjustment three roll shafts to realize abundant grinding to frit and dispersion.Undersized frit glass particles, has large specific surface area, contributes in follow-up high-temperature technology, help better fusing and fully flowing.
C) fusing and annealing: by above-mentioned b) in fully ground frit blends, proceed in High Temperature Furnaces Heating Apparatus and carry out long-time heating fusing.These inorganicss need under ultra-high temperature condition, normally carry out long period heating in the temperature range of 1000 DEG C-1600 DEG C and can form glass metal.In the present invention, frit progressively rises within 1100 DEG C-1300 DEG C from room temperature by the High Temperature Furnaces Heating Apparatus of general employing 1650 DEG C, temperature rise rate 5 DEG C/per minute.When after the temperature of fusion that frit reaches predetermined, frit slowly occurs soften and form glass metal from particulate state.This process need keeps 1-6 hour, until obtain the glass metal fully melted.Glass metal good for above-mentioned fusing is carried out anneal, glass metal is kept for some time in its softening temperature and glass transition temp region, then, slowly glass metal is continued to be cooled to room temperature, just can obtain little glass block.
D) grinding and screening: above-mentioned little glass block is carried out milled processed, first these little glass block can be positioned in agate shredder and carry out just grinding, obtain glass block particle.Then poured into from the charging opening of three-roller by ground glass block particle, the different rotating speeds and the spacing (being less than the gap of 5um) that control three roll shafts carry out fine grinding and dispersion.Frit blends after grinding, carry out screening process, screen cloth can select the specification of more than 325 orders, preferably 400 orders.Do not penetrate the further three-roller grinding of frit and the screening process of screen cloth, until meet sieve number requirement, now, just can obtain low melting glass material powder.
According to the method for the hermetically sealing electrical element of low melting glass material paste composition of the present invention, comprise the following steps:
A) the first glass substrate and the second glass substrate is prepared;
B) by the frit described in any one of 1-7 of described claim, the predetermined position of the first glass substrate is fixed on by coating process, utilize source of radiation (as laser or infrared rays) to carry out heated frit, make it be welded to by the first glass substrate on the second described glass substrate and also form gas-tight seal dam betwixt.
According to a kind of method using low melting glass material hermetically sealing electrical element of the present invention, comprise the predetermined position first low melting glass material being fixed in advance the first glass substrate.Generally speaking, comprise silk screen printing or some glue etc. by coated glass material paste composition exactly in the technique of glass substrate, preferred silk-screen printing technique realizes the fixed position described low melting glass material being coated on the first glass substrate.Then, the first glass substrate being coated with low melting glass material is carried out the process of frit paste composition sintering process.
According to a kind of method using the hermetically sealing electrical element of low melting glass material of the present invention; also comprise and utilize source of radiation (such as laser or infrared rays) to heat low melting glass material on the fixed position being fixed on the first glass substrate; make the frit after melting can form hermetically sealing dam between the first glass substrate and the second glass substrate, to protect electrical element.Use low melting glass material provided by the invention, the speed that water oxygen molecule can be penetrated into electrical element inside is down to 10
-6in the level of g/m2/day, significantly provide the obstructing capacity to water oxygen.
In order to contribute to understanding the present invention, shown below is exemplary embodiment of the present invention.But, the present invention is not limited to following illustrative embodiments.
Embodiment
Embodiment 1. [manufacture of glass frit compositions]
Manufacture frit paste composition with the composition in table 1 according to embodiment 1 ~ 4, the unit in table 1 is wt%.Filler for this frit paste composition is the eucryptite containing Al2O3 and SiO2 chemical composition, be cellulose polymer EC/Texanol for the organic adhesive/organic solvent in the project 1 and 2 of this frit paste composition, the organic binder bond/organic solvent in project 3 and 4 is AC acrylic resin/Texanol.
Table 2 shows viscosity and the molecular weight of organic binder bond used.The test condition of viscosity is room temperature 25 DEG C, and use rich strangling to fly that Brookfield viscosity apparatus DV2T measures in 0.1rpm condition, molecular weight adopts waters2695GPC mensuration.
Table 3 shows the glass transition temp Tg with the component mixture in table 1, adopts with DTA device (DTG-60H Shimatz), heats up with the speed of 10 DEG C/min, measure the glass transition temp of glass frit compositions.
Table 1 (wt%)
Table 2
| Project | Tackiness agent | Organic solvent | Viscosity | Binder molecule amount |
| 1 and 2 | EC | Texanol | 4,500 | 11,000 |
| 3 and 4 | AC | Texanol | 2,000 | 145,000 |
Table 3
| Project | 1 | 2 | 3 | 4 |
| Glass transition temp | 373.3 | 340.8 | 364.1 | 370.5 |
According to table 3, when finding higher Bi2O3 content, the content increasing B2O3 unexpectedly reduces the glass transition temp of glass frit compositions.This may be under the condition of higher Bi2O3 (75 % by weight), and the bond energy intensity of bismuth oxide is less than the bond energy intensity of boron oxide.When the content of the zinc oxide increased in frit system or bismuth oxide, contribute to equally reducing its glass transition temp.
Embodiment 2 [hermetically sealing of OLED element]
The present invention discloses the predetermined position described frit being fixed on the first glass substrate by screen printing process or some glue coating process, utilize source of radiation to carry out heated frit, make it be welded to by the first glass substrate on the second described glass substrate and also form gas-tight seal dam betwixt.
Below by detailed method for hermetically sealing of setting forth OLED element with half tone silk screen printing process and laser radiation heating technique.It is to be understood that the frit paste composition of setting forth in the embodiment of the present invention and air hermetic packing technique, be not limited to half tone silk-screen or laser radiation heating.
Hermetically sealing technique, shown in Fig. 1-3, specific as follows:
A) preparation of frit paste composition
As Figure 2-3, by above-mentioned frit paste composition uniform stirring batch mixing (S210) prepared, to reach desirable silk-screen condition.Generally speaking, first frit paste composition is carried out being stirred well to few more than 1H before silk-screen, scraper can be adopted to stir, or be positioned over the upper rotation number hour of roller machine (roller).
B) silk screen printing process
By frit paste composition good for abundant batch mixing, be applied in the upper surface of the half tone of silk-screen board, the order number of the half tone of described silk-screen board can be 325 orders, can be also 400 orders, depends on the particle diameter of particle in frit paste composition and silk-screen effect and determines.Regulate the corresponding scraper of silk-screen board or the angle of inclination of returning blade, the height of silk-screen half tone and the first glass substrate upper surface, and the pressure and other parameters pressing down half tone of returning blade or scraper, silk-screen is in the predetermined position (S220) of the first glass substrate upper surface, frit surface is now comparatively smooth, and edge is not crude.
C) sintering process of frit paste composition
Frit paste composition on above-mentioned first glass substrate predetermined position is carried out sintering process (S230).
First, at a lower temperature by complete for the organic solvent drying in frit paste composition.Generally speaking, frit paste composition, lower than 200 DEG C, therefore, can be carried out drying by these organic easy vaporization temperatures fast in low temperature environment.
Then, frit paste composition complete for drying is carried out carbonization treatment technique.Generally speaking, the polymeric adhesive (Binder) in carbonization treatment processing requirement frit paste composition as far as possible all within 300 DEG C smooth oxygenolysis become CO2, H2O, or other gases.Specifically, frit paste composition described in the present invention to the selection of polymeric adhesive based on the glass transition temp of frit blends higher than the complete decomposition temperature of polymeric adhesive, and the viscosity of polymeric adhesive will meet silk screen printing process requirement.
Finally, the frit paste composition after carbonization treatment is carried out sintering processes.Generally speaking, the grain fraction that in the frit paste composition that carbonization treatment is later, structure is comparatively loose, at 600 DEG C, preferably can complete sintering, shape on the predetermined position of the first glass substrate within 500 DEG C.Meanwhile, sintering temperature lower than near the glass transition temp of frit paste composition time, need slowly to heat up, to keep glass frit compositions, there is good surface topography.
D) air hermetic glass capsulation
The first glass substrate after sintering and the second glass substrate carry out air hermetic glass capsulation.
First, TFT (thin film transistor will be prepared, thin film transistor) upper surface of the second glass substrate of technique, carry out vacuum thermal evaporation art breading, form OLED unit, the upper surface of the second described glass substrate is defined as the one side (S300) of carrying out TFT technique.Described evaporation process forms OLED unit, namely on the upper surface of the second glass substrate, conventional hole input horizon HIL/ hole transmission layer HTL/ organic luminous layer EML/ electron transfer layer ETL/ electron injecting layer EIL/ negative electrode (S400) is completed, but, OLED unit described in the present invention is not limited to said structure, and theory is can by electroluminescent device architecture.Then, the upper surface of the upper surface of the second described glass substrate and the first described glass substrate is carried out exactitude position, contraposition and laminating (S500) are carried out in the predetermined position of the frit blends on the first glass substrate upper surface and the second glass substrate upper surface.Then, as shown in Figure 3, Ti: sapphire laser (λ=810nm) is passed into its upper surface by the lower surface 100 of the first glass substrate, frit blends 200 on its upper surface being heated, sealing forming hermetically sealing dam between the upper surface 100 and the upper surface 300 of the second glass substrate of the first glass substrate (S600).
Think the illustrative embodiments that can put into practice at present although combined the present invention is described in detail, but be understood that, the invention is not restricted to the embodiment announced, on the contrary, the present invention is intended to cover the various amendment and equivalents that comprise within the scope of the appended claims.
Claims (9)
1. a low melting glass material paste composition, is characterized in that, it contains
A) frit compositions, the weight percent of its chemical constitution is as follows:
Bi2O3(70-80wt％)，
B2O3(5-15wt％)，
ZnO(5-10wt％)，
CuO(0-15wt％)，
MnO2(0-15wt％)，
Fe2O3(0-5wt％)，
BaO (1-5wt%), and
Wherein, CuO+Fe2O3+MnO2 is in the scope of 5wt% to 15wt%;
B) filler
C) organic binder bond, when described organic binder bond has the molecular weight of 10,000g/ mole-300,000g/ moles and dissolves in organic solvent with 1-5wt%, organic paste composition viscosity is 500cps-100,000cps; With
D) organic solvent.
2. a kind of low melting glass material paste composition according to claim 1, it is characterized in that, it contains:
A) glass frit powder of 50wt%-90wt%;
B) filler of 1wt%-15wt%;
C) organic binder bond of 1wt%-5wt%, when described organic binder bond has the molecular weight of 10,000g/ mole-300,000g/ moles and dissolves in organic solvent with 1-5wt%, organic paste composition viscosity is 500cps-100,000cps; With
D) organic solvent of 5wt%-45wt%.
3. a kind of low melting glass material paste composition according to claim 1, it is characterized in that, described glass frit powder composition contains:
Bi2O3(70-75wt％)，
B2O3(5-10wt％)，
ZnO(5-10wt％)，
CuO(1-15wt％)，
MnO2(1-15wt％)，
Fe2O3(1-5wt％)，
BaO (1-5wt%), and
Wherein, CuO+Fe2O3+MnO2 is in the scope of 5wt% to 15wt%.
4. a kind of low melting glass material paste composition according to claim 1, is characterized in that, the main chemical compositions of described filler is SiO2 and Al2O3.
5. a kind of low melting glass material paste composition according to claim 4, is characterized in that, described organic binder bond freely comprises and is selected from cellulose-based EC, at least one material in acrylic resin AC or poly-alkyl carbonate PC.
6. a kind of low melting glass material paste composition as claimed in claim 1, it is characterized in that, described organic solvent comprises and is selected from acetate of butyl carbitol, a-terpinol, dibutyl phthalate, ethyl acetate, β-terpinol, pimelinketone, ethylene glycol, triglyme, or at least one material of the mixture of high-boiling point alcohol and alcohol ester.
7. a kind of low melting glass material paste composition according to claim arbitrary in claim 1 to 6, it is characterized in that, described glass frit powder adopts the preparation method comprised the following steps:
A) prepare burden; Raw material is taken according to composition and ratio;
B) batch mixing: the raw material taken is carried out in shredder mix, grind, until feedstock composition mixes, obtain admixtion;
C) high temperature melting-annealing: admixtion is put into platinum crucible, then the platinum crucible that admixtion is housed is put into resistance furnace to heat, 1000 DEG C-1500 DEG C are progressively risen to by room temperature, and be incubated 6 hours, admixtion is fully melted, obtain glass metal, then described glass metal cast is annealed in a mold, obtain the both bulk glasses of having annealed.
D) grinding and screening: smashed to pieces by both bulk glasses, and allow into grinding machine for grinding 1-6 hour, then by the glass powder after grinding, carries out, after screening process, just can obtaining the frit of low melting point through 400 object screen clothes.
8. a sealing method for electrical element, it comprises:
First glass substrate;
Second glass substrate; With
The frit described in any one of 1-7 of described claim, the predetermined position of the first glass substrate is fixed on by coating process, utilize source of radiation (as laser or infrared rays) to carry out heated frit, make it be welded to by the first glass substrate on the second described glass substrate and also form gas-tight seal dam betwixt.
9. electrical element sealing method according to claim 8, is characterized in that, described electrical element includes OLED (OLED) element, dye sensitization solar battery (DSSC) or lighting (LED).
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Cited By (5)
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| WO2017016461A1 (en) * | 2015-07-27 | 2017-02-02 | 京东方科技集团股份有限公司 | Encapsulation material, organic light-emitting diode device and encapsulation method therefor |
| CN107275516A (en) * | 2017-06-21 | 2017-10-20 | 苏州卡睿知光电科技有限公司 | A kind of glass capsulation material for photoelectric device, paste and preparation method thereof |
| CN107759092A (en) * | 2017-09-28 | 2018-03-06 | 浙江光达电子科技有限公司 | It is a kind of to be used to carry on the back lead-free glass powder of passivation crystal silicon solar battery back face silver paste and preparation method thereof |
| JP2018062445A (en) * | 2016-10-13 | 2018-04-19 | 日本電気硝子株式会社 | Bismuth glass and sealing material prepared therewith |
| WO2018103163A1 (en) * | 2016-12-09 | 2018-06-14 | 东莞珂洛赫慕电子材料科技有限公司 | Low-melting-point inorganic binder slurry for aluminum substrate and preparation method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017016461A1 (en) * | 2015-07-27 | 2017-02-02 | 京东方科技集团股份有限公司 | Encapsulation material, organic light-emitting diode device and encapsulation method therefor |
| US10217959B2 (en) | 2015-07-27 | 2019-02-26 | Boe Technology Group Co., Ltd. | Packaging material including rare earth metal oxide, organic light-emitting diode device and method for packaging the same |
| JP2018062445A (en) * | 2016-10-13 | 2018-04-19 | 日本電気硝子株式会社 | Bismuth glass and sealing material prepared therewith |
| WO2018103163A1 (en) * | 2016-12-09 | 2018-06-14 | 东莞珂洛赫慕电子材料科技有限公司 | Low-melting-point inorganic binder slurry for aluminum substrate and preparation method therefor |
| CN107275516A (en) * | 2017-06-21 | 2017-10-20 | 苏州卡睿知光电科技有限公司 | A kind of glass capsulation material for photoelectric device, paste and preparation method thereof |
| CN107759092A (en) * | 2017-09-28 | 2018-03-06 | 浙江光达电子科技有限公司 | It is a kind of to be used to carry on the back lead-free glass powder of passivation crystal silicon solar battery back face silver paste and preparation method thereof |
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