CN107162426A - A kind of glass capsulation material, sealing material paste and preparation method thereof - Google Patents
A kind of glass capsulation material, sealing material paste and preparation method thereof Download PDFInfo
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- CN107162426A CN107162426A CN201710474589.2A CN201710474589A CN107162426A CN 107162426 A CN107162426 A CN 107162426A CN 201710474589 A CN201710474589 A CN 201710474589A CN 107162426 A CN107162426 A CN 107162426A
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- glass capsulation
- capsulation material
- parts
- paste
- glass
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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
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a kind of glass capsulation material, sealing material paste and preparation method thereof.Wherein, glass capsulation material, includes the raw material of following mass fraction：Bi2O35 10 parts, SiO28 15 parts, TiO236 parts, 46 parts of silane coupler, 12 parts of CaO, 68 parts of bentonite, Fe2O358 parts, 9 15 parts of ZnO, MnO246 parts.Using the raw material of specific proportioning, using the interaction between each raw material, collaboration comes into force, and makes the glass capsulation material not easy to foaming, airtight effect when for sealing good.
Description
Technical field
The invention belongs to packaging of photoelectric device technical field, and in particular to a kind of glass capsulation material, sealing material paste and its
Preparation method.
Background technology
Display of organic electroluminescence OLED (Organic Light-Emitting Diode) is put down as a kind of new
Plate shows, because it has actively luminous, high brightness, high-resolution, wide viewing angle, fast-response speed, low energy consumption and can be flexible
The features such as change, it is expected to be widely applied in Medical Devices and optoelectronic display device.
There is the organic layer material for steam and oxygen extremely sensitivity in current OLED, this causes OLED to show
The life-span of device substantially reduces.In order to solve this problem, various materials are mainly used in the prior art by the organic of OLED
Layer material is isolated from the outside, and improves its sealing property.Wherein conventional encapsulating method is：In nitrogen atmosphere, shown in OLED
The sealing area filling glass material of the upper and lower base plate of panel, then utilizes laser beam movement heated frit fusing.After fusing
Frit forms closed encapsulation connection between upper and lower base plate.
Frits all at present mostly uses inorganic oxide and filler, when using process, is scattered in organic
In solvent, then on silk screen brush to the upper and lower base plate of OLED display panel.Because of point of inorganic oxide and filler in organic solvent
Dissipate property poor, it is easy to foaming in uneven components, fusion process in frit when causing to seal, influence sealing effectiveness.
The content of the invention
Therefore, to be solved by this invention is existing glass capsulation material poor defect of easy to foaming, airtight effect in sealing,
It is the good glass capsulation material of stability, close and then it is low to provide a kind of good not easy to foaming, airtight effect, softening point and thermal coefficient of expansion
Envelope material paste and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
Glass capsulation material provided by the present invention, includes the raw material of following mass fraction：
Further, the raw material of following mass fraction is included：
Further, 7-8 parts of beta-eucryptite and/or β-spodumene is included.
Further, 2-3 parts of vanadic anhydride is included.
Further, 1-2 parts of diboron trioxide is included.
In addition, the present invention also provides a kind of glass capsulation material paste, include the raw material of following mass fraction：
55-78 parts of glass capsulation material any one of claim 1-5
6-8 parts of polymeric adhesive
20-25 parts of organic solvent.
Further, the high polymer binder is carboxymethyl cellulose and/or acrylic resin.
Further, the organic solvent be terpineol, dibutyl phthalate or triglyme at least
It is a kind of.
In addition, present invention also offers the preparation method of above-mentioned glass capsulation material paste, comprising the following steps：
1) the glass capsulation material and polymeric adhesive are ground for the first time, obtains abrasive；
2) abrasive is scattered in the organic solvent, and regrind, obtain the glass capsulation material
Paste.
Further, the particle diameter of the abrasive is less than 2 μm.
Compared with prior art, the present invention has the advantages that：
The glass capsulation material that the embodiment of the present invention is provided, using the raw material of specific proportioning, using mutual between each raw material
Effect, collaboration comes into force, and makes the glass capsulation material not easy to foaming, airtight effect when for sealing good.It is even especially with silane
Join agent and bentonite, first improve the dispersion effect of other raw materials in organic solvent, improve the uniform of each feed distribution
Property, enhance sealing effectiveness；Second bubble can be prevented to produce when melting sealing, while can also fill bubble, improves sealing
Effect.After tested, the sealing effectiveness of the glass capsulation material can reach that vapour quantity is not more than 10-7g/m2/ day, amount of oxygen is not more than
10-4cm3/m2/ day.
Embodiment
In order to which the object, technical solutions and advantages of the present invention are better described, below in conjunction with specific embodiment to this hair
It is bright to be described further.The present invention can be embodied in many different forms, and should not be construed as limited to set forth herein
Embodiment.Opposite there is provided these embodiments so that the disclosure will be thorough and complete, and the design of the present invention will be filled
Divide and convey to those skilled in the art, the present invention will only be defined by the appended claims.
Embodiment 1
A kind of glass capsulation material paste is present embodiments provided, by 8g Bi2O3, 11g SiO2, 5g TiO2, 5g
KH550,1.5g CaO, 7g bentonite, 7g Fe2O3, 12g ZnO, 5g MnO2, 7g carboxymethyl cellulose and 22g
Terpineol is constituted；
The preparation method of above-mentioned glass capsulation material paste, comprises the following steps：
1) ground for the first time by glass capsulation material and with polymeric adhesive-carboxymethyl cellulose, obtain particle diameter less than 2
μm abrasive；
2) abrasive is scattered in organic solvent-terpineol, and regrind, obtain the glass capsulation
Expect paste.
Embodiment 2
A kind of glass capsulation material paste is present embodiments provided, by 5g Bi2O3, 15g SiO2, 3g TiO2, 6g
KH550,1g CaO, 8g bentonite, 5g Fe2O3, 15g ZnO, 4g MnO2, 8g acrylic resin and 20g it is three sweet
Diethylene glycol dimethyl ether is constituted；
The preparation method of above-mentioned glass capsulation material paste, comprises the following steps：
1) ground for the first time by glass capsulation material and with polymeric adhesive-acrylic resin, obtain particle diameter less than 2 μm
Abrasive；
2) abrasive is scattered in organic solvent-triglyme, and regrind, obtain the glass
Glass sealing material paste.
Embodiment 3
A kind of glass capsulation material paste is present embodiments provided, by 10g Bi2O3, 8g SiO2, 6g TiO2, 4g
KH550,2g CaO, 6g bentonite, 8g Fe2O3, 9g ZnO, 6g MnO2, 6g acrylic resin and 25g it is three sweet
Diethylene glycol dimethyl ether is constituted；
The preparation method of above-mentioned glass capsulation material paste, comprises the following steps：
1) ground for the first time by glass capsulation material and with polymeric adhesive-acrylic resin, obtain particle diameter less than 2 μm
Abrasive；
2) abrasive is scattered in organic solvent-triglyme, and regrind, obtain the glass
Glass sealing material paste.
Embodiment 4
A kind of glass capsulation material paste is present embodiments provided, by 8g Bi2O3, 11g SiO2, 5g TiO2, 5g
KH550,1.5g CaO, 7g bentonite, 7g Fe2O3, 12g ZnO, 5g MnO2, 7.5g beta-eucryptite, the five of 2.5g
V 2 O, 1.5g diboron trioxide, 7g carboxymethyl cellulose and 22g terpineol composition；
The preparation method of above-mentioned glass capsulation material paste, comprises the following steps：
1) ground for the first time by glass capsulation material and with polymeric adhesive-carboxymethyl cellulose, obtain particle diameter less than 2
μm abrasive；
2) abrasive is scattered in organic solvent-terpineol, and regrind, obtain the glass capsulation
Expect paste.
Embodiment 5
A kind of glass capsulation material paste is present embodiments provided, by 8g Bi2O3, 11g SiO2, 5g TiO2, 5g
KH550,1.5g CaO, 7g bentonite, 7g Fe2O3, 12g ZnO, 5g MnO2, 8g β-spodumene, 2g five oxidations
Two vanadium, 2g diboron trioxide, 7g carboxymethyl cellulose and 25g dibutyl phthalate composition；
The preparation method of above-mentioned glass capsulation material paste, comprises the following steps：
1) ground for the first time by glass capsulation material and with polymeric adhesive-carboxymethyl cellulose, obtain particle diameter less than 2
μm abrasive；
2) abrasive is scattered in organic solvent-terpineol, and regrind, obtain the glass capsulation
Expect paste.
Comparative example 1
This comparative example provides a kind of glass capsulation material paste, by 8g Bi2O3, 11g SiO2, 5g TiO2, 1.5g
CaO, 7g bentonite, 7g Fe2O3, 12g ZnO, 5g MnO2, 7g carboxymethyl cellulose and 22g terpineol composition；
The preparation method of above-mentioned glass capsulation material paste, comprises the following steps：
1) ground for the first time by glass capsulation material and with polymeric adhesive-carboxymethyl cellulose, obtain particle diameter less than 2
μm abrasive；
2) abrasive is scattered in organic solvent-terpineol, and regrind, obtain the glass capsulation
Expect paste.
Comparative example 2
This comparative example provides a kind of glass capsulation material paste, by 8g Bi2O3, 11g SiO2, 5g TiO2, 5g
KH550,1.5g CaO, 7g Fe2O3, 12g ZnO, 5g MnO2, 7g carboxymethyl cellulose and 22g terpineol composition；
The preparation method of above-mentioned glass capsulation material paste, comprises the following steps：
1) ground for the first time by glass capsulation material and with polymeric adhesive-carboxymethyl cellulose, obtain particle diameter less than 2
μm abrasive；
2) abrasive is scattered in organic solvent-terpineol, and regrind, obtain the glass capsulation
Expect paste.
Test example 1
Glass capsulation material paste made from the various embodiments described above and comparative example is used for sealed OLED display, OLED shows
Show what device was made up of upper substrate, infrabasal plate, position to be sealed and OLED sedimentaries.Specific sealing step is as follows：With silk screen by glass
Brush at glass sealing material paste brush to the corresponding position to be sealed of upper substrate.Pre-sintered processing is carried out below softening point temperature.It is first
Frit first is heated into 130 DEG C of insulations makes the moisture evaporation in glass capsulation material paste for 5 minutes, is then heated to macromolecule and glues
Agent burning point insulation 10 minutes is connect, polymeric adhesive is removed completely.The finally heated softening point to glass capsulation material paste with
Upper insulation 10 minutes, pre-sintered good glass capsulation material paste is placed on laser package workbench and is sintered.What is used swashs
Light device is semiconductor laser, and the wavelength for sending 6.5 watts is 810 nanometers of continuous laser, with the rate melt glass of 5 mm/seconds
Glass sealing material paste, two substrates are merged, air locking is made.
The air-tightness of above-mentioned air locking is detected using Varian947 helium leak checks instrument, detection 100 is above-mentioned close every time
Device is sealed, corresponding testing result is as shown in table 1 below and 2：
The air-tightness number up to standard of the air locking of table 1
| Number | |
| Embodiment 1 | 100 |
| Embodiment 2 | 100 |
| Embodiment 3 | 100 |
| Embodiment 4 | 100 |
| Embodiment 5 | 100 |
| Comparative example 1 | 50 |
| Comparative example 2 | 38 |
The air-tightness of the air locking of table 2
| Vapour quantity g/m2/ day | Amount of oxygen cm3/m2/ day | |
| Embodiment 1 | 10-7 | 10-4 |
| Embodiment 2 | 10-7 | 10-4 |
| Embodiment 3 | 10-7 | 10-4 |
| Embodiment 4 | 10-7 | 10-4 |
| Embodiment 5 | 10-7 | 10-4 |
| Comparative example 1 | 10-5 | 10-2 |
| Comparative example 2 | 10-4 | 10-1 |
It was found from table 1 and 2：Using the raw material of specific proportioning, using the interaction between each raw material, collaboration comes into force, and makes this
Glass capsulation material not easy to foaming, airtight effect when for sealing is good.
Claims (10)
1. a kind of glass capsulation material, includes the raw material of following mass fraction：
2. glass capsulation material according to claim 1, it is characterised in that：Include the raw material of following mass fraction：
3. glass capsulation material according to claim 1 or 2, it is characterised in that：Also include 7-8 parts beta-eucryptite and/or
β-spodumene.
4. the glass capsulation material according to any one of claim 1-3, it is characterised in that：Also include 2-3 parts of five oxidations
Two vanadium.
5. the glass capsulation material according to any one of claim 1-4, it is characterised in that：Also include 1-2 parts of three oxidations
Two boron.
6. a kind of glass capsulation material paste, it is characterised in that include the raw material of following mass fraction：
55-78 parts of glass capsulation material any one of claim 1-5
6-8 parts of polymeric adhesive
20-25 parts of organic solvent.
7. glass capsulation material paste according to claim 6, it is characterised in that the high polymer binder is that carboxymethyl is fine
Dimension element and/or acrylic resin.
8. the glass capsulation material paste according to claim 6 or 7, it is characterised in that the organic solvent is terpineol, neighbour
At least one of dibatyl phithalate or triglyme.
9. the preparation method of the glass capsulation material paste any one of claim 6-8, comprises the following steps：
1) the glass capsulation material and polymeric adhesive are ground for the first time, obtains abrasive；
2) abrasive is scattered in the organic solvent, and regrind, obtain the glass capsulation material paste.
10. preparation method according to claim 9, it is characterised in that the particle diameter of the abrasive is less than 2 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710474589.2A CN107162426A (en) | 2017-06-21 | 2017-06-21 | A kind of glass capsulation material, sealing material paste and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710474589.2A CN107162426A (en) | 2017-06-21 | 2017-06-21 | A kind of glass capsulation material, sealing material paste and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107162426A true CN107162426A (en) | 2017-09-15 |
Family
ID=59819800
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710474589.2A Pending CN107162426A (en) | 2017-06-21 | 2017-06-21 | A kind of glass capsulation material, sealing material paste and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103178214A (en) * | 2011-12-22 | 2013-06-26 | 上海大学 | Method and device for encapsulating photoelectric device |
| CN103906718A (en) * | 2011-11-02 | 2014-07-02 | 费罗公司 | Microwave sealing of inorganic substrates using low melting glass systems |
| CN103922596A (en) * | 2013-12-31 | 2014-07-16 | 上海天马有机发光显示技术有限公司 | Frit composition, frit paste composition, electrical element sealing method and electrical element |
| CN104628252A (en) * | 2013-11-08 | 2015-05-20 | 谢再锋 | Rare earth doped lead-free frit and electrical component sealing method utilizing the same |
| CN105906199A (en) * | 2015-02-19 | 2016-08-31 | 中央硝子株式会社 | Bi2O3-TeO2-SiO2-WO3 series glass |
-
2017
- 2017-06-21 CN CN201710474589.2A patent/CN107162426A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103906718A (en) * | 2011-11-02 | 2014-07-02 | 费罗公司 | Microwave sealing of inorganic substrates using low melting glass systems |
| CN103178214A (en) * | 2011-12-22 | 2013-06-26 | 上海大学 | Method and device for encapsulating photoelectric device |
| CN104628252A (en) * | 2013-11-08 | 2015-05-20 | 谢再锋 | Rare earth doped lead-free frit and electrical component sealing method utilizing the same |
| CN103922596A (en) * | 2013-12-31 | 2014-07-16 | 上海天马有机发光显示技术有限公司 | Frit composition, frit paste composition, electrical element sealing method and electrical element |
| CN105906199A (en) * | 2015-02-19 | 2016-08-31 | 中央硝子株式会社 | Bi2O3-TeO2-SiO2-WO3 series glass |
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Application publication date: 20170915 |