CN114212995B - Preparation method of OLED sealing solder - Google Patents

Preparation method of OLED sealing solder Download PDF

Info

Publication number
CN114212995B
CN114212995B CN202111609266.2A CN202111609266A CN114212995B CN 114212995 B CN114212995 B CN 114212995B CN 202111609266 A CN202111609266 A CN 202111609266A CN 114212995 B CN114212995 B CN 114212995B
Authority
CN
China
Prior art keywords
glass
sealing
percent
oled
solder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202111609266.2A
Other languages
Chinese (zh)
Other versions
CN114212995A (en
Inventor
彭寿
张冲
李金威
王巍巍
倪嘉
仲召进
赵凤阳
王萍萍
高强
柯震坤
韩娜
石丽芬
杨勇
李常青
周刚
曹欣
单传丽
崔介东
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Building Materials Glass New Materials Research Institute Group Co Ltd
Original Assignee
China Building Materials Glass New Materials Research Institute Group Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Building Materials Glass New Materials Research Institute Group Co Ltd filed Critical China Building Materials Glass New Materials Research Institute Group Co Ltd
Priority to CN202111609266.2A priority Critical patent/CN114212995B/en
Publication of CN114212995A publication Critical patent/CN114212995A/en
Application granted granted Critical
Publication of CN114212995B publication Critical patent/CN114212995B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/068—Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths
    • 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
    • C03C12/00—Powdered glass; Bead compositions
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/52—Encapsulations
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/52—Encapsulations
    • H01L33/56—Materials, e.g. epoxy or silicone resin

Landscapes

  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Glass Compositions (AREA)

Abstract

The application discloses a preparation method of OLED sealing solder, which comprises the following steps of: 40 to 50 percent of Bi 2 O 3 ，5～15%SiO 2 ，10～15%B 2 O 3 ，15～25%ZnO，1～5%Li 2 O，1～5%Na 2 O, 0-3% SrO, 1-4% BaO, and MnO 2 、CuO、CeO 2 、Co 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the And uniformly mixing the glass batch, placing the mixture into a crucible, placing the crucible into a high-temperature furnace, heating to 800-1000 ℃, grinding the prepared sealing glass to obtain 50-200 mu m sealing glass powder, and uniformly mixing the organic binder and the sealing glass powder to prepare the OLED sealing solder. The application has the beneficial effects that: the prepared sealing solder has low sealing temperature, is environment-friendly, has excellent sealing performance and good chemical stability and electrical insulation performance, and can meet the requirement of heating and sealing by lasers with different wavelengths from ultraviolet to infrared.

Description

Preparation method of OLED sealing solder
Technical Field
The application relates to the technical field of electronic glass, in particular to a preparation method of OLED sealing solder.
Background
With the rapid development of electronic information display technology, flat panel display technologies such as Liquid Crystal Displays (LCDs) and organic light emitting diode displays (OLEDs) have gradually replaced CRT displays, wherein OLEDs are widely used in mobile phone screens, computer displays, full color televisions, etc. because of their advantages of self luminescence, low driving voltage, high luminous efficiency, short response time, high definition and contrast, near 180 ° viewing angle, wide use temperature range, flexible display and large-area full color display, etc., and are known as the most promising display devices in the industry. However, since the organic materials of the electrodes and the light emitting layer constituting the OLED device are very sensitive to pollutants in the atmosphere, moisture and oxygen, electrochemical corrosion is easily generated in an environment containing moisture and oxygen, and the service life of the OLED is reduced. Therefore, the OLED must be effectively sealed from external moisture and oxygen.
At present, the OLED sealing mode is mainly divided into three categories of light-cured resin sealing, metal film sealing and low-melting-point glass sealing. The light-cured resin is used for sealing an organic material, so that the light-cured resin is easy to age for a long time, poor in high temperature resistance and unstable in sealing performance; the metal film has good sealing performance, but the process is complex, and the multilayer coating sealing is required to realize electrical insulation and good wettability, so that the cost is higher; the low-melting point glass sealing has the advantages of excellent chemical stability and electrical property, low sealing temperature, easy adjustment of expansion coefficient, good sealing air tightness, simple process and the like, and becomes a hot material for OLED sealing.
The bismuthate glass is a hot material for low-temperature sealing due to the excellent performances of low sealing temperature, good chemical stability, good wettability with a glass substrate and the like. However, the bismuth oxide content of the glass system is too high, crystallization is very easy in the heating and sealing process, so that the controllability of the expansion coefficient of the sealing material is poor, the sealing air tightness is reduced, such as patents of electric nitrate (JP 2004331394A), fuzhou university (CN 106495490B) and the like, and meanwhile, in order to further reduce the influence of high temperature on the device performance in the sealing process, methods of directional infrared heating and sealing, laser sealing and the like are provided, but the sealing temperature of the sealing solder developed by the method is still too high, and only the sealing solder with specific wavelength can be met, such as patents of Shanghai silicate institute of China academy of sciences (CN 113121117A), china institute of construction materials science (CN 103910490B) and the like, and the requirement on a heating light source is higher, and the application range is narrow.
Disclosure of Invention
The application aims to solve the technical problems, and provides a preparation method suitable for OLED sealing solder, which is low in sealing temperature and realizes heating and sealing of lasers with different wavelengths from ultraviolet to infrared by introducing different coloring metal ions.
In order to achieve the above purpose, the technical scheme adopted by the application is as follows:
the preparation method of the OLED sealing solder is characterized by comprising the following steps of:
(1) Weighing raw materials of the batch according to mole percentage: 40 to 50 percent of Bi 2 O 3 5 to 15 percent of SiO 2 10 to 15 percent of B 2 O 3 15 to 25 percent of ZnO and 1 to 5 percent of Li 2 O, 1-5% Na 2 O，0～3% SrO, 1-4% BaO, 0-1.5% MnO 2 2 to 5 percent of CuO and 0 to 5 percent of CeO 2 0 to 1.5 percent of Co 2 O 3 ；
(2) Placing the mixture in the step (1) into a crucible after being completely and uniformly mixed, placing the crucible into a high-temperature furnace, heating to 800-1000 ℃ at 1-10 ℃/min, preserving heat for 30-90 min, pouring out and quenching molten glass, and preparing sealing glass;
(3) Grinding the sealing glass prepared in the step (2) to obtain 50-200 mu m sealing glass powder, and uniformly mixing the organic binder with the sealing glass powder according to the mass percentage of 10-20% to prepare the sealing solder.
Further, in the step (1), the glass batch (Li 2 O+Na 2 O value is 3-8%, srO+BaO value is 3-5%, mnO value 2 +CuO+CeO 2 +Co 2 O 3 ) The value is 4-9%.
Further, in the step (2), the glass liquid quenching method includes water quenching and roll-rolling the sheet.
Further, in the step (3), the grinding method includes a ball milling method and an air stream pulverizing method.
Further, in the step (3), the organic binder includes one or a combination of several of terpineol, dipropyl ether, triethyl orthoformate and triphenyl phosphate.
The sealing glass powder provided by the application is low-melting glass powder, and Bi is used for preparing the sealing glass powder 2 O 3 、SiO 2 、B 2 O 3 ZnO is used as a main component, and also comprises one or more compounds for enhancing the network structure of glass, reducing the characteristic temperature of glass and enhancing the spectral absorption performance of glass.
According to diagonal lines and adjacent rules in the periodic table, bismuth can replace lead in the sealing glass with low melting point. Bi (Bi) 2 O 3 As a glass forming body, with SiO 2 、B 2 O 3 When the glass forming body components are mixed and melted, the glass forming range is relatively large. In addition, bi and Pb have electron configurations, ionic radii and atomic weights very similar, and in bismuthate glasses, bi-O bonds tend to be covalent bonds, so that [ BiO 6 ]And [ BiO ] 3 ]As structural units, it is possible to add [ SiO ] 4 ]Together form a glass network skeleton and Bi 3+ The polarizability of ions is large, which makes Bi 2 O 3 And PbO have similar structure and properties in glass. However, the Bi is because the Bi is excessively high, which leads to easy crystallization of the glass, loose structure of the glass and larger expansion coefficient 2 O 3 The composition range is 40-50 mol%.
SiO 2 In glass with silicon oxygen tetrahedra [ SiO ] 4 ]The glass network structure is connected, so that the glass structure is more compact, the chemical stability of the glass is enhanced, the thermal expansion coefficient of the glass is reduced, but excessive SiO is generated 2 Which can lead to glass melting and clarification difficulties and increase the characteristic temperature of the glass, thus the SiO 2 The composition range is 5-15 mol%.
B 2 O 3 As glass forming oxides, the bismuthate glass system is mainly composed of boron-oxygen triangle [ BO ] 3 ]And boron oxygen tetrahedra [ BO ] 4 ]As a structural unit, with [ BiO ] 3 ]And [ BiO ] 6 ]Together form a glass network structure. B (B) 2 O 3 The introduction of the glass can reduce the expansion coefficient of the glass and improve the thermal stability, chemical stability and mechanical strength of the glass. But when B 2 O 3 When the content is too high, it is impossible to supply sufficient free oxygen, resulting in [ BO ] 4 ]Backward [ BO ] 3 ]The transition, the "boron anomaly" occurs, which increases its expansion coefficient. Thus said B 2 O 3 The composition range is 10-15 mol%.
ZnO is mainly zinc oxide octahedron [ ZnO ] in bismuthate glass system 6 ]As an exonetwork oxide, it provides free oxygen that promotes [ BiO 3 ]、[BiO 6 ][ BO ] 3 ]The generation of the glass structure is caused to loosen, and the characteristic temperature is reduced; meanwhile, znO can improve the chemical stability, the thermal stability and the refractive index of the glass, but the content is too high, so that the crystallization tendency of the glass is increased, and the thermal expansion coefficient is increased, so that the ZnO has the composition range of 15-25 mol%.
Li 2 O、Na 2 O is an alkali metal oxide of the same genus in the glass structureAll belong to network external oxides, the free oxygen provided by the network external oxides can reduce the network connection degree of the glass, play a role of fluxing agent and reduce the characteristic temperature of the glass, but the increase of the alkali metal content also leads to the increase of the thermal expansion coefficient of the glass, and the thermal stability, chemical stability and mechanical mildness of the glass are reduced, so that the Li 2 O is 1-5 mol%, na 2 O has a composition in the range of 1 to 5mol% and (Li 2 O+Na 2 O) is 3-8 mol%.
BaO and SrO belong to alkaline earth metal oxides, are used as divalent glass network external oxides, can improve chemical stability and mechanical strength, have good fluxing effect, enable glass to be easy to fuse, but the content is too high, so that the glass tends to be crystallized, the density is increased, the corrosion to refractory materials is large, and the service life of a kiln is reduced, therefore, the BaO composition range is 1-4%, the SrO composition range is 0-3%, and the (SrO+BaO) composition range is 3-5%.
MnO 2 、CuO、CeO 2 、Co 2 O 3 As a metallic colorant into the vitreous, non-bridging oxygen can be provided to promote [ BiO ] 3 ]、[BiO 6 ][ BO ] 3 ]The generation causes the glass structure to be loose, the characteristic temperature is reduced, and meanwhile, the spectral absorptivity of the sealing glass under different wavelengths can be improved by different metal ions. MnO (MnO) 2 Mn of bismuthate glass during melting 2+ Oxidation to Mn at high temperature 3+ Mainly by [ MnO ] 6 ]The glass has a glass structure, so that the spectral absorptivity of the glass at 400-750 nm can be obviously improved; cuO in bismuthate glass [ CuO ] 6 ]O in (a) 2+ Is received B 3+ 、Bi 3+ The effect and influence of [ CuO ] 6 ]An asymmetric structure is formed, so that the spectral absorptivity of the glass at 600-1500 nm can be obviously improved; ceO (CeO) 2 In bismuthate glass, due to Ce 4+ The special 4f electron layer structure leads to glass with strong absorptivity in the ultraviolet region; co (Co) 2 O 3 Conversion to Co at high temperature during melting of bismuthate glass 2+ Mainly by [ CoO ] 4 ]The glass can be obviously improved by 500 to 650 percent when the glass is in a glass structureSpectral absorbance in nm. By summarizing the law of influence of each metal colorant on spectral absorption performance after glass coloring, the complementary principle is utilized, and MnO is introduced into the patent 2 、CuO、CeO 2 、Co 2 O 3 As a metal colorant, the sealing solder can absorb the spectra of different wavelengths from ultraviolet to infrared, improve the sealing temperature and meet the requirement of heating and sealing of lasers with different wavelengths, but the excessive content of the colorant can cause the increase of cost and the increase of glass crystallization tendency, so the MnO 2 The composition range is 0-1.5%, the composition range of CuO is 2-5%, ceO 2 The composition range is 0-5%, co 2 O 3 The composition range is 0 to 1.5%, and (MnO) 2 +CuO+CeO 2 +Co 2 O 3 ) The composition range is 4-9%.
The application has the beneficial effects that:
(1) The application adopts bismuthate glass, and can realize sealing solder with low sealing temperature, matched expansion coefficient and good sealing air tightness by adjusting the mole percentage of each component;
(2) Mn in the present application 4+ 、Cu 2+ 、Ce 4+ 、Co 3+ The metal coloring ions are introduced into the glass structure in an internal doping mode, and the provided free oxygen enters the glass structure to break the connection between glass networks, so that the glass structure is loose, and the characteristic temperature of the glass is reduced; meanwhile, the metal coloring ions are introduced in an internal doping mode, so that the glass is more uniformly colored, the heat can be uniformly absorbed in the heating and sealing process, the sealing defect is reduced, and the sealing air tightness is improved.
(3) According to the characteristic that different coloring metal ions in glass cause the glass to have selective absorption on spectrum, mn is introduced 4+ 、Cu 2+ 、Ce 4+ 、Co 3+ As a colorant, the sealing solder can absorb different wavelength spectrums from ultraviolet to infrared, can meet the heating sealing of lasers with different wavelengths, and improves the application range of the sealing solder.
(4) The sealing solder of the application has no toxic elements such as Pb, cr, and the like, is environment-friendly, has low sealing temperature of 420-500 ℃ and simple preparation process.
Drawings
FIG. 1 is a graph showing the thermal expansion test of a glass sample of example 1;
FIG. 2 is a graph showing the thermal expansion test of the glass sample of example 5.
Detailed Description
The present application is described in further detail below by way of the following detailed description, which is presented herein for purposes of illustration and explanation only and is not intended to be limiting.
Example 1
(1) 402.778 g Bi is accurately weighed 2 O 3 (42%), 16.076 g SiO 2 (13%), 15.761 g B 2 O 3 (11%), 38.522 g ZnO (23%), 2.281 g Li 2 CO 3 （Li 2 O1.5%), 3.272 g Na 2 CO 3 （Na 2 O1.5%), 3.038 g SrCO 3 (SrO 1%) 8.123 g BaCO 3 (BaO 2%) 1.789 g MnO 2 (1%), 3.274 g CuO (2%), 3.542 g CeO 2 (1%), 1.542 g Co 2 O 3 (1%), putting the weighed raw materials into a mixer for mixing for 1h;
(2) Placing the raw materials mixed uniformly in the step (1) into an alumina crucible, placing the alumina crucible into a high-temperature furnace, heating to 1000 ℃ at 10 ℃/min, preserving heat for 1h, pouring the melted glass liquid into a stainless steel sheet rolling machine for sheet rolling, and preparing broken glass;
(3) Crushing the crushed glass of the rolled sheet into 50-150 mu m glass powder by an air flow crusher, mixing 88% of glass powder, 6% of terpineol and 6% of dipropyl ether into slurry according to mass percentage, and uniformly dispersing by adopting planetary ball milling for 30min to obtain the sealing solder.
The glass has a thermal expansion coefficient of 8.3X10-6/. Degree.C, a transformation point of 425.6 ℃, an expansion softening point of 451.9 ℃, a sealing temperature of 492 ℃ and good performance.
Example 2
(1) 409.079 g Bi is accurately weighed 2 O 3 (45%), 11.722 g of SiO 2 (10%) 17.657 gB 2 O 3 (13%), 26.99 g ZnO (17%), 4.325 g Li 2 CO 3 （Li 2 O3%), 6.203 g Na 2 CO 3 （Na 2 O3%), 2.88 g SrCO 3 (SrO 1%) 11.55 g BaCO 3 (BaO 3%) 0.848 g MnO 2 (0.5%), 4.656 g CuO (3%), 3.358 g CeO 2 (1%), 0.731 g Co 2 O 3 (0.5%), and then putting the weighed raw materials into a mixer for mixing for 1h;
(2) Placing the raw materials mixed uniformly in the step (1) into an alumina crucible, placing the alumina crucible into a high-temperature furnace, heating to 1000 ℃ at 10 ℃/min, preserving heat for 1h, pouring the melted glass liquid into a stainless steel sheet rolling machine for sheet rolling, and preparing broken glass;
(3) Crushing the crushed glass of the rolled sheet into 50-150 mu m glass powder by an air flow crusher, mixing 86% of glass powder, 6% of terpineol, 4% of dipropyl ether and 4% of triethyl orthoformate into slurry according to mass percentage, and uniformly dispersing by adopting planetary ball milling for 30min to obtain the sealing solder.
The glass has a thermal expansion coefficient of 8.5X10-6/. Degree.C, a transition point of 415.32 ℃, an expansion softening point of 432.8 ℃, a sealing temperature of 471 ℃ and good performance.
Example 3
(1) 412.124 g Bi is accurately weighed 2 O 3 (46%), 9.242 g SiO 2 (8%), 14.725 g B 2 O 3 (11%), 31.295 g ZnO (20%), 4.262 g Li 2 CO 3 （Li 2 O3%), 4.076 g Na 2 CO 3 （Na 2 O2%), 5.678 g SrCO 3 (SrO 2%) 7.588 g BaCO 3 (BaO 2%) 1.672 g MnO 2 (1%), 4.589 g CuO (3%), 3.309 g CeO 2 (1%), 1.441 g Co 2 O 3 (1%), putting the weighed raw materials into a mixer for mixing for 1h;
(2) Placing the raw materials mixed uniformly in the step (1) into an alumina crucible, placing the alumina crucible into a high-temperature furnace, heating to 1000 ℃ at 10 ℃/min, preserving heat for 1h, pouring the melted glass liquid into a stainless steel sheet rolling machine for sheet rolling, and preparing broken glass;
(3) Crushing the crushed glass of the rolled sheet into 50-150 mu m glass powder by an air flow crusher, mixing 84% of glass powder, 6% of terpineol, 4% of dipropyl ether and 4% of triphenyl phosphate into slurry according to mass percentage, and uniformly dispersing by adopting planetary ball milling for 30min to obtain the sealing solder.
The glass has a thermal expansion coefficient of 8.7X10-6/. Degree.C, a transition point of 390.5 ℃, an expansion softening point of 413.4 ℃, a sealing temperature of 448 ℃ and good performance.
Example 4
(1) Accurately weighing 414.383Bi 2 O 3 (48%), 6.679 g of SiO 2 (6%), 18.058 g B 2 O 3 (14%), 24.124 g ZnO (16%), 2.738 g Li 2 CO 3 （Li 2 O2%), 1.964 g Na 2 CO 3 （Na 2 O1%) 2.735 g SrCO 3 (SrO 1%) 10.969 g BaCO 3 (BaO 3%) 0.805 g MnO 2 (0.5%), 5.895 g CuO (4%), 9.567 g CeO 2 (3%), 2.082 g Co 2 O 3 (1.5%), and then putting the weighed raw materials into a mixer for mixing for 1h;
(2) Placing the raw materials mixed uniformly in the step (1) into an alumina crucible, placing the alumina crucible into a high-temperature furnace, heating to 1000 ℃ at 10 ℃/min, preserving heat for 1h, pouring the melted glass liquid into a stainless steel sheet rolling machine for sheet rolling, and preparing broken glass;
(3) Crushing the crushed glass of the rolled sheet into 50-150 mu m glass powder by an air flow crusher, mixing 84% of glass powder, 8% of terpineol and 8% of dipropyl ether into slurry according to mass percentage, and uniformly dispersing by adopting planetary ball milling for 30min to obtain the sealing solder.
The glass has a thermal expansion coefficient of 8.7X10-6/. Degree.C, a transformation point of 384.6 ℃, an expansion softening point of 409.8 ℃, a sealing temperature of 439 ℃ and good performance.
Example 5
(1) 414.768 g Bi is accurately weighed 2 O 3 (50%), 5.348 g SiO 2 (5%), 13.634 g B 2 O 3 (11%), 23.181 g ZnO%16%), 1.315 g Li 2 CO 3 （Li 2 O1%), 5.661 g Na 2 CO 3 （Na 2 O3%) 2.628 g SrCO 3 (SrO 1%) 14.053 g BaCO 3 (BaO 4%) 2.322 g MnO 2 (1.5%), 2.832 g CuO (2%), 12.257 g CeO 2 (4%), 2.001 g Co 2 O 3 (1.5%), and then putting the weighed raw materials into a mixer for mixing for 1h;
(2) Placing the raw materials mixed uniformly in the step (1) into an alumina crucible, placing the alumina crucible into a high-temperature furnace, heating to 1000 ℃ at 10 ℃/min, preserving heat for 1h, pouring the melted glass liquid into a stainless steel sheet rolling machine for sheet rolling, and preparing broken glass;
(3) Crushing the crushed glass of the rolled sheet into 50-150 mu m glass powder by an air flow crusher, mixing 82% of glass powder, 10% of terpineol, 4% of dipropyl ether and 4% of triethyl orthoformate into slurry according to mass percentage, and uniformly dispersing by adopting planetary ball milling for 30min to obtain the sealing solder.
The glass has a thermal expansion coefficient of 9.0X10-6/. Degree.C, a transition point of 357.4 ℃, an expansion softening point of 385.0 ℃ and a sealing temperature of 420 ℃ and has good performance.
Comparative example, information data provided for patent application number 201810311625.8,
(1) 82.70 g of Bi2O3 (40%), 7.99 g of SiO2 (30%), 16.55 g of B2O3 (30%), 1.71 g of Na2CO3 (Na 2O 1 wt%), 1.47 g of K2CO3 (K2O 1 wt%) and 3.0 g of TeO2 are accurately weighed, and the weighed raw materials are put into a mortar to be stirred and ground uniformly;
(2) Putting the raw materials uniformly mixed in the step (1) into an alumina crucible, and putting the alumina crucible into a high-temperature furnace at 1100 ℃;
(3) After the heat preservation is carried out for 90 minutes, the clear and transparent glass liquid is quickly poured into a stainless steel container filled with deionized water to prepare broken glass;
compared with the prior art, the application has the advantages of low expansion coefficient, better matching with the expansion coefficient of the sealed glass, low sealing temperature and excellent performance.
The glass properties of each example are shown in Table 1 below
Table 1 example glass properties
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application in any way; any person skilled in the art can make many possible variations and modifications to the technical solution of the present application or modifications to equivalent embodiments using the methods and technical contents disclosed above, without departing from the scope of the technical solution of the present application. Therefore, any simple modification, equivalent substitution, equivalent variation and modification of the above embodiments according to the technical substance of the present application, which do not depart from the technical solution of the present application, still fall within the scope of the technical solution of the present application.

Claims (3)

1. The preparation method of the OLED sealing solder is characterized by comprising the following steps of:
(1) Weighing raw materials of the batch according to mole percentage: 40 to 50 percent of Bi 2 O 3 5 to 15 percent of SiO 2 10 to 15 percent of B 2 O 3 15 to 25 percent of ZnO and 1 to 5 percent of Li 2 O, 1-5% Na 2 O,0 to 3 percent of SrO,1 to 4 percent of BaO,0 to 1.5 percent of MnO 2 2 to 5 percent of CuO and 0 to 5 percent of CeO 2 0 to 1.5 percent of Co 2 O 3 ；
(2) Placing the mixture into a crucible after completely and uniformly mixing the mixture, placing the crucible into a high-temperature furnace, heating to 800-1000 ℃ at the speed of 1-10 ℃/min, preserving heat for 30-90 min, pouring out and quenching the melted glass liquid, and preparing the sealing glass;
(3) Grinding the prepared sealing glass to obtain 50-200 mu m sealing glass powder, and uniformly mixing 10-20% of organic binder with the sealing glass powder according to mass percent to prepare the OLED sealing solder;
in the step (1), li in the glass batch is 2 O+Na 2 The O value is 3-8%, the SrO+BaO value is 3-5%, the MnO value is 3-5% 2 +CuO+CeO 2 +Co 2 O 3 The value is 4-9%;
in the step (3), the organic binder comprises one or a combination of more of terpineol, dipropyl ether, triethyl orthoformate and triphenyl phosphate.
2. The method for preparing the OLED sealing solder according to claim 1, wherein the method comprises the following steps: in the step (2), the molten glass quenching method comprises water quenching and roll-pressing the sheet.
3. The method for preparing the OLED sealing solder according to claim 1, wherein the method comprises the following steps: in the step (3), the grinding method comprises a ball milling method and an airflow grinding method.
CN202111609266.2A 2021-12-27 2021-12-27 Preparation method of OLED sealing solder Active CN114212995B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111609266.2A CN114212995B (en) 2021-12-27 2021-12-27 Preparation method of OLED sealing solder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111609266.2A CN114212995B (en) 2021-12-27 2021-12-27 Preparation method of OLED sealing solder

Publications (2)

Publication Number Publication Date
CN114212995A CN114212995A (en) 2022-03-22
CN114212995B true CN114212995B (en) 2023-10-20

Family

ID=80705981

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111609266.2A Active CN114212995B (en) 2021-12-27 2021-12-27 Preparation method of OLED sealing solder

Country Status (1)

Country Link
CN (1) CN114212995B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115925436B (en) * 2022-12-26 2023-09-22 哈尔滨工业大学 Method for connecting ferrite and microwave dielectric ceramic by using low-melting glass soldering paste
CN116189957A (en) * 2023-03-30 2023-05-30 南京汇聚新材料科技有限公司 Copper conductive paste for inductor and preparation method and application thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000128574A (en) * 1998-10-21 2000-05-09 Nippon Electric Glass Co Ltd Bismuth-based glass composition
JP2007297266A (en) * 2006-04-03 2007-11-15 Nippon Electric Glass Co Ltd Amorphous glass tablet and tablet-integrated evacuation tube
CN103910490A (en) * 2013-01-07 2014-07-09 中国建筑材料科学研究总院 Lead-free sealing glass powder having selective spectrum absorption characteristic, and manufacturing method thereof
CN107399908A (en) * 2017-08-21 2017-11-28 北京工业大学 A kind of photo-thermal heat absorbing glass sealing-in material and preparation method thereof
CN110217993A (en) * 2019-06-26 2019-09-10 鲁米星特种玻璃科技股份有限公司 A kind of Environment-friendlylow-temperature low-temperature seal glass and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000128574A (en) * 1998-10-21 2000-05-09 Nippon Electric Glass Co Ltd Bismuth-based glass composition
JP2007297266A (en) * 2006-04-03 2007-11-15 Nippon Electric Glass Co Ltd Amorphous glass tablet and tablet-integrated evacuation tube
CN103910490A (en) * 2013-01-07 2014-07-09 中国建筑材料科学研究总院 Lead-free sealing glass powder having selective spectrum absorption characteristic, and manufacturing method thereof
CN107399908A (en) * 2017-08-21 2017-11-28 北京工业大学 A kind of photo-thermal heat absorbing glass sealing-in material and preparation method thereof
CN110217993A (en) * 2019-06-26 2019-09-10 鲁米星特种玻璃科技股份有限公司 A kind of Environment-friendlylow-temperature low-temperature seal glass and preparation method thereof

Also Published As

Publication number Publication date
CN114212995A (en) 2022-03-22

Similar Documents

Publication Publication Date Title
CN114212995B (en) Preparation method of OLED sealing solder
US9469562B2 (en) Glass substrate with sealing material layer, organic EL device using same, and manufacturing method for electronic device
CN113121117B (en) Glass powder suitable for OLED packaging and preparation method and application thereof
JP6357937B2 (en) Sealing material and sealing package
CN107265872B (en) Double-component lead-free glass powder suitable for front silver paste of crystalline silicon battery
CN110217993B (en) Environment-friendly low-temperature sealing glass and preparation method thereof
CN103601369A (en) Preparation method of lead-free electronic glass powder for back aluminum slurry of solar cell
CN111268904B (en) Preparation method of energy-saving glass
CN110240404B (en) Tellurate infrared-transmitting glass and preparation method thereof
CN110204192B (en) Deep ultraviolet transparent phosphate glass and preparation method and application thereof
CN102951841A (en) Preparation method of high borosilicate glass for solar photovoltaic batteries
CN103910491A (en) Lead-containing sealing glass powder having selective spectrum absorption characteristic, and manufacturing method thereof
CN113149432A (en) Anti-radiation boron tellurate luminescent glass and preparation method thereof
CN110255898B (en) Deep ultraviolet transparent glass, preparation method, application and melting device thereof
CN112551902A (en) Low-melting-point glass powder containing alkaline earth metal and preparation method and application thereof
JP2008308393A (en) Lead-free low softening point glass, lead-free low softening point glass composition, lead-free low softening point glass paste, and fluorescent display tube
Yanık et al. Effect of V2O5 and TeO2 substitution on thermal, structural and wettability properties in lead free bismuth zinc borate-based low temperature sealing glass and preparation of glasses in paste form as an engineering practice
JP6108285B2 (en) Manufacturing method of electronic device
CN101503276B (en) Bismuth doped strontium-aluminum-boron based optical glass and preparation thereof
CN108911515A (en) Glass powder with low melting point, glass powder slurry and preparation method thereof and panel encapsulating structure
CN110128006A (en) A kind of environment-friendly type high refractive index holvi glass and preparation method thereof
CN103910490B (en) There is barium crown sealed glass powder and the manufacture method thereof of spectral selection absorption characteristic
CN114230187B (en) Low-temperature lead-free electronic glass powder for photoelectric sealing
US7291572B2 (en) Synergistic composition for preparing high concentration fullerene (C60) glass and a method for preparing the glass in bulk monolith
CN115477472B (en) Vanadium-phosphorus sealing glass and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
CB02 Change of applicant information

Address after: 233010 Tushan Road 1047, Yuhui District, Bengbu City, Anhui Province

Applicant after: China Building Materials Glass New Materials Research Institute Group Co.,Ltd.

Address before: 233010 Tushan Road 1047, Yuhui District, Bengbu City, Anhui Province

Applicant before: CHINA BUILDING MATERIALS BENGBU GLASS INDUSTRY DESIGN & RESEARCH INSTITUTE Co.,Ltd.

CB02 Change of applicant information
GR01 Patent grant
GR01 Patent grant