Light-absorbing material, glass powder, slurry for laser sealing, and preparation method therefor and use thereof
By using the light-absorbing material FexMnyOz, the problems of high sealing temperature and weak photo-thermal conversion capability of inorganic sealing materials are solved, and efficient packaging and good protection effects are achieved during laser sealing.
Patent Information
- Application Number
- PCT/CN2023/124696
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2023-10-16
- Publication Date
- 2025-04-24
AI Technical Summary
In the prior art, the sealing temperature of inorganic sealing materials is high and the photothermal conversion ability is weak, making it difficult to ensure the sealing quality during laser sealing.
Using a light absorbing material FexMnyOz, a light absorbing material with ferromagnetic and dielectric properties is prepared by mixing FeOi and MnOj and then sintering. It is applied to the slurry for laser sealing to improve its light absorbing performance, dispersion and accumulation density.
It effectively reduces the thermal impact during laser sealing, improves the packaging effect, enhances the binding force between the substrate and the packaging cover plate, reduces the penetration of water vapor and oxygen, and extends the service life of the device.
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Figure CN2023124696_24042025_PF_FP_ABST
Abstract
Description
Light-absorbing material, glass powder, laser sealing slurry, and preparation method and application thereof Technical Field
[0001] The present application belongs to the field of solder technology, and in particular to a light-absorbing material, glass powder, slurry for laser sealing, and a preparation method and application thereof. Background Art
[0002] Inorganic glass paste can be applied to glass, ceramic, or metal substrates through methods such as screen printing. The paste is heated to remove the organic carrier, and further heating melts the glass to bond to the substrate. For example, the electronics industry is currently experiencing rapid development. Organic light-emitting diode (OLED) technology, with its advantages of lightweight, low-voltage operation, high brightness, and low power consumption, has widely replaced liquid crystal displays (LCDs). When OLEDs are used in display devices and other products, the lifespan of organic materials is negatively affected by water and air. A good seal can isolate these materials and extend the product's lifespan. Resins are typically used to seal products, but after curing, the molecular gaps between these materials are large, resulting in curing defects. This weakens the bond with the substrate and package cover, allowing moisture and oxygen to easily penetrate the gaps and enter the internal seal, causing accelerated device aging. Using glass-based inorganic materials for sealing products, on the other hand, can generally improve water and oxygen barrier properties by one to two orders of magnitude compared to organic resins. Furthermore, their airtight packaging stability and weather resistance are significantly superior to those of organic resins, effectively addressing the drawbacks of organic resin sealing. Currently, developed solders for laser sealing include alloy materials such as Sn-Pb, Sn-Ag, Sn-Bi, Sn-Zn, and Sn-Cu; and polymer materials such as polyepoxy (PEP), polyethylene (PE), polycarbonate (PC), thermoplastic silicone rubber (TPSE), and polyvinyl butyral (PVB). In comparison, inorganic glass solders suitable for laser welding are relatively scarce.
[0003] The sealing operating temperature of inorganic glass solder is typically above 400°C. Therefore, for some electronic components that cannot withstand high temperatures, such as organic light-emitting diodes, it is impossible to seal them by heating the entire device. Such devices can be sealed using laser sealing, which uses a laser to heat only the area where the solder is applied, keeping other areas or core components of the device at a lower, safe temperature. This is because the solder used in laser sealing must not only have the required sealing properties but also have good light-to-heat conversion capabilities. Traditional bismuth-based glass has disadvantages such as high sealing temperatures and weak light-to-heat conversion capabilities, which poses many difficulties when used in laser sealing. For example, if the laser power is too high, the temperature between the substrate and the underlying precision circuitry will be too high, causing damage to related functional components. If the laser power is too low, the glass at the sealing point will not reach a fully molten state, and the sealing quality cannot be guaranteed. Therefore, how to improve the light-to-heat conversion function of glass solder has become a bottleneck that needs to be overcome in current laser sealing technology. Technical issues
[0004] The purpose of this application is to provide a light-absorbing material, glass powder, laser sealing slurry, and preparation method and application, aiming to solve the problems of high sealing temperature and weak light-to-heat conversion ability of inorganic sealing materials in the prior art. Technical Solutions
[0005] To achieve the above application objectives, the technical solutions adopted in this application are as follows:
[0006] In the first aspect, the present application provides a light-absorbing material having the general formula Fe x Mn y O z , where 1≤x≤10, 1≤y≤5, 1≤z≤17.
[0007] The present application is to improve the situation that the sealing effect of resin-sealed devices is poor and the service life of the devices is short. The embodiments of the present application provide a light-absorbing material. The light-absorbing material has ferrimagnetic and dielectric properties, and its relative magnetic permeability and relative electrical conductivity are both in plural form. It can generate both dielectric loss and magneto-induced loss. Therefore, the light-absorbing material can absorb incident electromagnetic waves and can better absorb the energy provided by the laser heating and melting method. The light-absorbing material of the present application is an inorganic material that is acid-resistant, alkali-resistant, and chemically resistant. When applied to laser sealing slurry, it not only gives the laser sealing slurry light-absorbing properties and reduces the thermal expansion coefficient, but also can improve the dispersibility and stacking density of the laser sealing slurry, and has a strong binding force with the substrate or the packaging cover plate. It is difficult for water vapor and oxygen to penetrate the gap into the internal sealing area, which can form a better protection for the device, improve the packaging effect and reduce the problem of internal cracks.
[0008] In some embodiments, the Fe x Mny O z Including FeO i With MnO j The composition of Fe x Mn y O z It is a crystalline compound, wherein 0≤i≤3, 0≤j≤4.
[0009] In some embodiments, the Fe x Mn y O z Including FeMnO3, Fe2MnO4, Fe3MnO5, Fe4MnO6, FeMn2O3, FeMn3O7, FeMn4O9, Fe2MnO5, Fe4MnO8, Fe6MnO 11 、Fe8MnO 16 , Fe2Mn2O7, Fe2Mn3O9, Fe2Mn4O 11 、Fe5MnO7、FeMn5O 11 、Fe 10 MnO 17 、Fe2Mn5O 13 At least one of .
[0010] In some embodiments, the Fe x Mn y O z The shape is at least one of granular, spherical, spherical, and flake.
[0011] In some embodiments, the Fe x Mn y O z The particle size is 0.1~50μm.
[0012] In a second aspect, the present application provides a method for preparing a light-absorbing material, comprising the following steps:
[0013] FeO i With MnO j After mixing, sintering is performed to obtain Fe x Mn y O z light-absorbing material, wherein 0≤i≤3, 0≤j≤4, 1≤x≤10, 1≤y≤5, 1≤z≤17.
[0014] In the preparation method of the glass material of this application, FeO i With MnO j After mixing and sintering, Fe x Mn y O zThe light-absorbing material is simple and practical, has strong operability, and is suitable for large-scale production.
[0015] In some embodiments, the sintering process is performed at a temperature of 1000-1400°C.
[0016] In some embodiments, the FeO i With MnO j The mass ratio is 0.13~11.5.
[0017] In a third aspect, the present application provides a glass powder comprising the light-absorbing material described above or the light-absorbing material prepared by the preparation method described above.
[0018] In this application, Fe x Mn y O z Since the light-absorbing material can be evenly dispersed in other components in the sealing glass paste formula, it can also be used as a glass raw material. It can be evenly dispersed in the glass after melting processing, and then the glass is applied to the packaging paste to obtain a uniformly mixed sealing glass paste, thereby realizing the conversion of electromagnetic wave energy into thermal energy, which is beneficial to the softening and sealing of the glass and improves the uniformity of heat absorption of the glass system.
[0019] In some embodiments, based on the molar percentage of the glass powder being 100%, the glass powder includes the following molar percentages of the raw material components:
[0020] In some embodiments, the other oxides include at least one of SiO2, CuO, Co3O4, BaO, Al2O3, MgO, CaO, TiO2, WO3, and SrO.
[0021] In some embodiments, the glass powder includes at least one of amorphous glass and microcrystalline glass.
[0022] In a fourth aspect, the present application provides a method for preparing glass powder, comprising the following steps:
[0023] Weigh the raw materials of each component according to the molar percentage of each component contained in the glass frit mentioned above;
[0024] The raw materials of each component are mixed, melted and processed to obtain glass powder.
[0025] In this application, in order to obtain the glass powder mentioned above, this application provides a method for preparing glass powder. First, each component is weighed according to the mass percentage of each raw material contained in the glass frit mentioned above, and the ratio of each raw material of the glass powder is adjusted. Then, the glass raw materials mentioned above are mixed to obtain a highly dispersed glass raw material mixture. The raw materials are melted to form liquid glass frit. After processing, a glass powder with a low glass transition temperature and a low expansion coefficient can be obtained. The glass powder prepared by the above-mentioned glass frit preparation method is applied to the encapsulation slurry, which can effectively improve the encapsulation effect of the encapsulation slurry.
[0026] In some embodiments, the temperature of the melt treatment is 600-1500°C.
[0027] In a fifth aspect, the present application provides a slurry for laser sealing, comprising the light-absorbing material described above or the light-absorbing material obtained by the preparation method described above or the glass powder described above or the glass powder obtained by the preparation method described above.
[0028] In the laser sealing paste of the application example, Fe x Mn y O z It can be added to the slurry as a single component and mixed evenly, or melted into the glass as a glass-forming material. On the one hand, since the sealing glass slurry contains light-absorbing materials, the light-absorbing materials can effectively absorb energy when encapsulating electronic products. While ensuring the sealing performance requirements, it can effectively reduce the laser energy provided in the sealing process. This can not only reduce the defects caused by the thermal shock generated during laser sealing to the product, but also save energy. On the other hand, the light-absorbing material is an inorganic material that is acid-resistant, alkali-resistant, and chemically resistant. When used in the laser sealing slurry, it not only gives the laser sealing slurry light-absorbing properties and reduces the thermal expansion coefficient, but also improves the dispersion and stacking density of the laser sealing slurry. It has a strong bonding force with the substrate or the packaging cover, and it is difficult for water vapor and oxygen to penetrate the gap into the internal sealing area, which can provide better protection for the device, improve the packaging effect, and reduce the problem of internal hidden cracks.
[0029] In some embodiments, the laser sealing paste further comprises an organic carrier, a functional filler and a light-absorbing filler, and the weight proportions of the glass powder, the organic carrier, the functional filler and the light-absorbing filler are as follows:
[0030] In some embodiments, the functional filler comprises at least one of β-eucryptite, zirconium phosphotungstate, zirconium tungstate, cordierite, zirconium oxide, and zirconium powder.
[0031] In some embodiments, the functional filler is in the shape of at least one of granular, spherical, quasi-spherical, and flake.
[0032] In some embodiments, the particle size of the functional filler is 0.05-5 μm.
[0033] In some embodiments, the light-absorbing filler includes at least one of copper chrome black, iron manganese black, iron chrome black, silicon carbide, and tungsten powder.
[0034] In some embodiments, the light-absorbing filler is in the shape of at least one of granules, spheres, quasi-spheres, and flakes.
[0035] In some embodiments, the particle size of the light-absorbing filler is 0.05 to 5 μm.
[0036] In a sixth aspect, the present application provides a method for preparing the above-mentioned laser sealing slurry. The method for preparing the laser sealing slurry of the present application comprises the following steps:
[0037] The glass powder, the organic carrier, the functional filler and the light-absorbing filler are mixed to obtain the slurry for laser sealing;
[0038] Wherein, the glass powder includes the light-absorbing material of the above-mentioned application embodiment or the light-absorbing material prepared by the method for preparing the light-absorbing material of the above-mentioned application embodiment or the glass powder of the above-mentioned application embodiment or the glass powder prepared by the method for preparing the glass powder of the above-mentioned application embodiment.
[0039] The method for preparing the laser sealing slurry in the embodiment of the present application mixes the glass powder containing the light-absorbing material of the embodiment of the present application with an organic carrier, a functional filler, and a light-absorbing filler component. This gives the prepared laser sealing slurry the ability to effectively reduce the laser energy provided in the sealing process while ensuring the sealing performance requirements when packaging electronic products. It also gives the laser sealing slurry the function of light absorption and reducing the thermal expansion coefficient, which can improve the dispersibility and stacking density of the laser sealing slurry and strengthen the bonding force with the substrate or packaging cover. In addition, the conditions of the preparation method of the embodiment of the present application are easy to control, which improves the quality stability of the prepared laser sealing slurry.
[0040] In a seventh aspect, the present application provides an application of the above-mentioned laser sealing slurry in packaging organic light-emitting diodes, solar photovoltaics, lasers or MEMS.
[0041] It is precisely because the laser sealing slurry has a low expansion coefficient and a low glass transition temperature that the present application applies the laser sealing slurry to the encapsulation of organic light-emitting diodes, which can improve the dispersion and stacking density of the laser sealing slurry, and has a strong bonding force with the substrate or the encapsulation cover. It is difficult for water vapor and oxygen to penetrate the gap into the internal sealing area, which can provide better protection for the organic light-emitting diodes, improve the encapsulation effect and reduce the problem of internal hidden cracks. BRIEF DESCRIPTION OF THE DRAWINGS
[0042] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following briefly introduces the drawings required for use in the embodiments or descriptions of the prior art. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained like these drawings without any creative work.
[0043] FIG1 is a TG-DSC characteristic temperature diagram of the glass powder in Example 2-1 of the present application;
[0044] FIG2 is a cross-sectional morphology of the laser sealing slurry of Comparative Example 3-1 of the present application pre-sintered at 420° C.;
[0045] FIG3 is a cross-sectional morphology of the slurry for laser sealing of Example 3-1 of the present application pre-sintered at 420° C.;
[0046] FIG4 is a cross-sectional morphology of the laser sealing slurry of Comparative Example 3-2 of the present application pre-sintered at 420° C.;
[0047] FIG5 is a cross-sectional morphology diagram of the laser sintering slurry for laser sealing in Comparative Example 3-1 of the present application;
[0048] FIG6 is a cross-sectional view of the laser sintering of the slurry for laser sealing in Example 3-1 of the present application;
[0049] Figure 7 is a cross-sectional view of the laser sintering slurry for laser sealing in comparative example 3-2 of the present application. Modes for Carrying Out the Invention
[0050] In order to make the technical problems, technical solutions and beneficial effects to be solved by this application more clearly understood, the present application is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain this application and are not intended to limit this application.
[0051] In this application, the term "and / or" describes the relationship between associated objects, indicating that three possible relationships exist. For example, A and / or B can represent: A exists alone, A and B exist simultaneously, and B exists alone. A and B can be singular or plural. The character " / " generally indicates that the associated objects are in an "or" relationship.
[0052] In this application, "at least one" means one or more, and "more than one" means two or more. "At least one of the following" or similar expressions refers to any combination of these items, including any combination of single items or plural items. For example, "at least one of a, b, or c", or "at least one of a, b, and c" can all mean: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, and c can be single or multiple.
[0053] It should be understood that in the various embodiments of the present application, the size of the serial numbers of the above-mentioned processes does not mean the order of execution. Some or all of the steps can be executed in parallel or sequentially. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present application.
[0054] The terms used in the embodiments of the present application are only for the purpose of describing specific embodiments and are not intended to limit the present application. The singular forms "a", "an" and "the" used in the embodiments of the present application and the appended claims are also intended to include plural forms unless the context clearly indicates otherwise.
[0055] The weights of the relevant components mentioned in the examples of this application may not only refer to the specific content of each component, but also represent the weight ratio between the components. Therefore, as long as the content of the relevant components is proportionally enlarged or reduced according to the examples of this application, it is within the scope disclosed in the examples of this application. Specifically, the mass in the examples of this application may be μg, mg, g, kg, etc., which are mass units known in the chemical industry.
[0056] The terms "first" and "second" are used solely for descriptive purposes to distinguish objects, such as substances, from one another and should not be understood to indicate or imply relative importance or to implicitly specify the quantity of the technical features being referred to. For example, without departing from the scope of the embodiments of this application, a first XX may also be referred to as a second XX, and similarly, a second XX may also be referred to as a first XX. Thus, features defined as "first" or "second" may explicitly or implicitly include one or more of such features.
[0057] In the first aspect, the present invention provides a light absorbing material having the general formula of Fe x Mn y O z , where 1≤x≤10, 1≤y≤5, 1≤z≤17.
[0058] In order to improve the poor sealing effect of resin-sealed devices and the short service life of devices, the embodiments of the present application provide a light-absorbing material. On the one hand, the light-absorbing material has ferrimagnetic and dielectric properties, and its relative magnetic permeability and relative electrical conductivity are both in plural form. It can generate both dielectric loss and magneto-induced loss. Therefore, the light-absorbing material can absorb incident electromagnetic waves and can better absorb the energy provided by the laser heating and melting method. On the other hand, the light-absorbing material in the embodiment of the present application is an inorganic material that is acid-resistant, alkali-resistant, and chemically resistant. When used in laser sealing slurry, it not only gives the laser sealing slurry light-absorbing properties and reduces the thermal expansion coefficient, but also can improve the dispersibility and stacking density of the laser sealing slurry, and has a strong bonding force with the substrate or the packaging cover plate. It is difficult for water vapor and oxygen to penetrate the gap into the internal sealing area, which can form a better protection for the device, improve the packaging effect and reduce the problem of internal hidden cracks.
[0059] In some embodiments, Fe x Mn y O z Including FeO i With MnO j The raw materials of the compound are widely available, which can reduce production costs, and Fe x Mn y O z It is a crystalline compound, which has good light absorption properties, high temperature resistance and high oxidation resistance, wherein 0≤i≤3, 0≤j≤4. x Mn y O z Including FeMnO3, Fe2MnO4, Fe3MnO5, Fe4MnO6, FeMn2O3, FeMn3O7, FeMn4O9, Fe2MnO5, Fe4MnO8, Fe6MnO 11 、Fe8MnO 16 , Fe2Mn2O7, Fe2Mn3O9, Fe2Mn4O 11 、Fe5MnO7、FeMn5O 11 、Fe 10 MnO 17 、Fe2Mn5O 13 It is understandable that the technology in this field can be reasonably expanded according to actual applications, as long as it is suitable for Fe as a light absorbing material x Mn y O z All are within the protection scope of this application.
[0060] In some embodiments, Fe x Mn y O zThe shape of Fe is at least one of granular, spherical, quasi-spherical, and flake. x Mn y O z The shapes are diverse and can be selected according to actual needs. They can be used in any proportion and applied to packaging slurry to improve the dispersion and stacking density of the conductive slurry, which is beneficial to improving the packaging effect.
[0061] In some embodiments, Fe x Mn y O z The particle size is 0.1 to 50 μm, such as 0.1 μm, 25 μm, and 50 μm. The light-absorbing material provided in the embodiment of the present application is micro-nano-scale, which can improve the mixing uniformity with other materials and thus improve the Fe x Mn y O z It can be used in slurries to improve the dispersion and stacking density of conductive slurries, which is beneficial to improving the sintering density of slurries. It also has a strong bonding force with substrates or package covers, and it is difficult for water vapor and oxygen to penetrate the gap into the internal sealing area, which can protect the device and effectively solve the defects of resin sealing.
[0062] In addition, Fe x Mn y O z The material can be prepared by any one of the following methods: high temperature calcination, physical vapor deposition, chemical vapor deposition, and hydrothermal method. The high temperature calcination method is described below.
[0063] In a second aspect, an embodiment of the present application provides a method for preparing a light-absorbing material, comprising the following steps:
[0064] Step S01. Include FeO i With MnO j After mixing, sintering is performed to obtain Fe x Mn y O z light-absorbing material, wherein 0≤i≤3, 0≤j≤4, 1≤x≤10, 1≤y≤5, 1≤z≤17.
[0065] In the preparation method of the glass material in the embodiment of the present application, FeO i With MnO j After mixing and sintering, Fe x Mn y O z The light-absorbing material is simple and practical, has strong operability, and is suitable for large-scale production.
[0066] In step S01, under high temperature, FeO i With MnO j After mixing and sintering, Fe x Mn y O z The sintering temperature can be 1000-1400℃, such as 1000℃, 1200℃, 1300℃, 1400℃, etc., which can make FeO i With MnO j Completely melt, mix and react thoroughly.
[0067] In some embodiments, under high temperature, FeO i With MnO j After mixing and sintering, Fe x Mn y O z The light absorbing material is adjusted by FeO i With MnO j The mass ratio of is 0.13 to 11.5, such as 0.46, 0.61, 0.92, 1.64, 4.14, etc., which can be used to prepare different light-absorbing materials.
[0068] In a third aspect, an embodiment of the present application provides a glass powder comprising the light-absorbing material described above or the light-absorbing material prepared by the preparation method described above.
[0069] In the examples of this application, Fe x Mn y O z Since the light-absorbing material can be evenly dispersed in other components in the sealing glass paste formula, it can also be used as a glass raw material. It can be evenly dispersed in the glass after melting processing, and then the glass is applied to the packaging paste to obtain a uniformly mixed sealing glass paste, thereby realizing the conversion of electromagnetic wave energy into thermal energy, which is beneficial to the softening and sealing of the glass and improves the uniformity of heat absorption of the glass system.
[0070] In some embodiments, based on the molar percentage of the glass powder being 100%, the glass powder includes the following molar percentages of the raw material components:
[0071] The low melting point glass powder provided in the embodiment of the present application adopts V-Te-Zn-BO series glass, and introduces Fe x Mn y O zThe introduction of crystalline compounds into the glass system not only maintains the characteristic of a low melting point, but also imparts the function of regulating light absorption properties and reducing the thermal expansion coefficient. By reducing the content of negative expansion fillers and light-absorbing materials, the slurry increases the glass content, which can effectively improve the internal density after sintering, improve the packaging effect, and improve the problem of internal hidden cracks. Specifically, V2O5 in the glass powder exists as a glass former, which can not only effectively reduce the transition temperature of the glass powder, but also absorb infrared light; ZnO, as a glass intermediate, has high activity in its nanopowder, which can aid melting and also inhibit crystallization; TeO2 and Bi2O3, as glass formers, can effectively reduce the glass transition temperature, but excessive content will lead to a loose glass network structure and an increase in CTE (thermal expansion coefficient); B2O3, as a glass former, can form a loose triangular structure to reduce the glass transition temperature, and can also form a tight tetrahedral structure to reduce CTE. The Tg of the glass powder in the slurry of the embodiment of the present application is 200-450°C. The glass powder provided in the embodiments of this application has excellent mechanical strength and a low coefficient of expansion. Compounds based on these characteristics, such as low-melting-point glass, offer advantages such as low sealing temperature, stable performance, and good fluidity, making them suitable for use in inorganic solders in place of lead-based glass. Furthermore, the glass powder provided in the embodiments of this application is lead-free, thus harming the environment and human health.
[0072] In the embodiment of the application, the formula is added with a light-absorbing material having a weight percentage of 0.1 to 5%. The weight percentage of the light-absorbing material is set within the above range mainly because: if the weight percentage of the added light-absorbing material is lower than 0.1%, the laser power required in the laser packaging process will be higher, which will cause the temperature rise of the substrate and the sealing material to be larger in an instant, and the temperature is too high, which can easily lead to damage to the functions of related components; at the same time, the temperature rise rate is too fast, which will also cause large transient stress, thereby causing damage to the sealing material, or causing cracks, and ultimately leading to product failure; on the contrary, if the weight percentage of the added light-absorbing material is higher than 5%, the temperature rise of the substrate and the sealing material will be slower, and it will take a longer time to heat-melt the sealing material, which will lengthen the process cycle and increase the production cost. Therefore, the weight percentage of the light-absorbing material added to the formula provided in the embodiment of the present invention is set within the range of 0.1 to 5%. Furthermore, the weight percentage of the light-absorbing material is 3 to 5%. Within this preferred content ratio range, it can better ensure the good performance of the final sealing glass paste while also reasonably controlling its production cycle. It is understood that the weight percentage of the light absorbing material may be 3%, 4%, or 5%.
[0073] In some embodiments, the other oxides include at least one of SiO2, CuO, Co3O4, BaO, Al2O3, MgO, CaO, TiO2, WO3, and SrO. Other oxides can further improve the sealing effect of the encapsulation paste. For example, SiO2, as a glass former, can improve the chemical stability of the glass, reduce the CTE, and enhance soldering strength. However, if its content is too high, it can significantly increase the glass transition temperature. CuO, MnO2, Fe2O3, and Co3O4, as functional additives, can all enhance the glass powder's ability to absorb infrared light. BaO, MgO, and CaO, as alkaline earth metal oxides, act as network modifiers and can break bonds, further lowering the glass transition temperature.
[0074] In some embodiments, the glass frit comprises at least one of amorphous glass and microcrystalline glass, with microcrystalline glass being relatively preferred. These types of glass frit have low coefficients of expansion. When used in encapsulation pastes, they can further reduce the encapsulation paste's coefficient of expansion, increase the glass content, and effectively improve the internal density after sintering, enhancing the encapsulation effect and reducing internal cracking.
[0075] In a fourth aspect, an embodiment of the present application provides a method for preparing glass powder, comprising the following steps:
[0076] Step S02. Weighing the raw materials of each component according to the molar percentage of each component contained in the glass frit described above;
[0077] Step S03: Mix, melt and process the raw materials to obtain glass powder.
[0078] In the embodiment of the present application, in order to obtain the glass powder mentioned above, the embodiment of the present application provides a method for preparing glass powder. First, each component is weighed according to the mass percentage of each raw material contained in the glass material mentioned above, and the ratio of each raw material of the glass powder is adjusted. Then, the various glass raw materials mentioned above are mixed to obtain a highly dispersed glass raw material mixture, and the various raw materials are melted to form liquid glass material. After processing, a glass powder with a low glass transition temperature and a low expansion coefficient can be obtained. The glass powder prepared by the above-mentioned glass material preparation method is applied to the encapsulation slurry, which can effectively improve the encapsulation effect of the encapsulation slurry.
[0079] In the above step S02, the glass frit is provided with raw materials of various components. The type selection and addition amount of the raw materials of various components of the provided glass frit are as discussed above, and will not be described again here to save space.
[0080] In the above step S03, the temperature of the melting treatment is 700-1400° C., which can fully melt the raw materials of each component.
[0081] In some embodiments, the processing also includes water quenching the melt to solidify the melt to obtain glass particles, and grinding and grading the glass particles to obtain glass material with a preset particle size for use in laser sealing slurry.
[0082] In a fifth aspect, an embodiment of the present application provides a slurry for laser sealing, comprising the light-absorbing material described above or the light-absorbing material obtained by the preparation method described above or the glass powder described above or the glass powder obtained by the preparation method described above.
[0083] In the application examples, Fe x Mn y O z It can be added to the slurry as a single component and mixed evenly, or melted into the glass as a glass-forming material. On the one hand, since the sealing glass slurry contains light-absorbing materials, the light-absorbing materials can effectively absorb energy when encapsulating electronic products. While ensuring the sealing performance requirements, it can effectively reduce the laser energy provided in the sealing process. This can not only reduce the defects caused by the thermal shock generated during laser sealing to the product, but also save energy. On the other hand, the light-absorbing material is an inorganic material that is acid-resistant, alkali-resistant, and chemically resistant. When used in the laser sealing slurry, it not only gives the laser sealing slurry light-absorbing properties and reduces the thermal expansion coefficient, but also improves the dispersion and stacking density of the laser sealing slurry. It has a strong bonding force with the substrate or the packaging cover, and it is difficult for water vapor and oxygen to penetrate the gap into the internal sealing area, which can provide better protection for the device, improve the packaging effect, and reduce the problem of internal hidden cracks.
[0084] In some embodiments, the laser sealing paste further includes an organic carrier, a functional filler, and a light-absorbing filler. The laser sealing paste includes the following raw material components in parts by weight:
[0085] The embodiment of the present application provides a slurry for sealing a glass substrate, which is made by mixing glass powder, functional fillers, light-absorbing fillers and organic carriers. On the one hand, since light-absorbing materials are added to the sealing glass slurry, the light-absorbing materials can effectively absorb energy when packaging electronic products, and can effectively reduce the laser energy provided in the sealing process while ensuring the sealing performance requirements. This can not only reduce the defects caused by the thermal shock generated during laser sealing to the product, but also save energy consumption. On the other hand, the light-absorbing material is an inorganic material that is acid-resistant, alkali-resistant and chemically resistant. When used in the laser sealing slurry, it not only gives the laser sealing slurry light-absorbing properties and reduces the thermal expansion coefficient, but also improves the dispersion and stacking density of the laser sealing slurry, and has a strong bonding force with the substrate or the packaging cover. It is difficult for water vapor and oxygen to penetrate the gap into the internal sealing area, which can form a better protection for the device, improve the packaging effect and reduce the problem of internal hidden cracks.
[0086] In some embodiments, an organic vehicle is mechanically mixed with the inorganic components in the laser encapsulation slurry to impart printable viscosity and rheological characteristics to the slurry composition. The organic vehicle can be any typical organic vehicle used in laser encapsulation slurries and may contain a binder resin, solvent, etc. Furthermore, varying the organic vehicle or adjusting the solids content between 50% and 90% can effectively adjust the slurry viscosity to meet specific viscosity requirements during use.
[0087] In some embodiments, the weight percentage of the functional filler is 0 to 10 parts. The weight percentage ratio of the glass powder to the ceramic filler is limited to the above range mainly because the glass powder has high mechanical strength and expansion coefficient. Therefore, in this embodiment, the ceramic filler is added to improve the mechanical properties and expansion coefficient of the glass powder, thereby obtaining a sealing glass paste with excellent performance.
[0088] In some embodiments, the functional filler includes at least one of β-eucryptite, zirconium phosphotungstate, zirconium tungstate, cordierite, zirconium oxide, and zirconium powder. By adjusting the proportion of the expansion coefficient filler in the slurry, the thermal expansion coefficient of the sealing glass can be effectively reduced to match the thermal expansion coefficient of the glass substrate, thereby reducing the impact of thermal stress on the glass substrate.
[0089] In some embodiments, the functional filler is in the form of at least one of granules, spheres, spherical shapes, and flakes. x Mn y O z The shapes are diverse and can be selected according to actual needs. They can be used in any proportion and applied to packaging slurry to improve the dispersion and stacking density of the conductive slurry, which is beneficial to improving the packaging effect.
[0090] In some embodiments, the particle size of the functional filler is 0.05 to 5 μm, such as 0.1 μm, 25 μm, and 50 μm. The functional filler provided in the embodiment of the present application is micro-nano-scale, which can improve the mixing uniformity with other materials, thereby improving the Fe x Mn y O z It can be used in slurries to improve the dispersion and stacking density of conductive slurries, which is beneficial to improving the sintering density of slurries. It also has a strong bonding force with substrates or package covers, and it is difficult for water vapor and oxygen to penetrate the gap into the internal sealing area, which can protect the device and effectively solve the defects of resin sealing.
[0091] In some embodiments, the light-absorbing filler includes at least one of copper chromium black, iron manganese black, iron chromium black, silicon carbide, and tungsten powder. The light-absorbing filler selected in the embodiment of the present application is a high-temperature resistant inorganic material, which can not only better absorb the energy provided by the laser heating and melting method, but also better mix with other components in the sealing glass slurry formula to obtain a uniformly mixed sealing glass slurry. It can be understood that the technology in this field can be reasonably expanded according to actual applications. As long as the inorganic material is suitable as a light-absorbing filler, it is within the scope of protection of this application. Introducing it into the OLED sealing glass slurry system can further promote the absorption of laser light. By adjusting the proportion of the light-absorbing filler in the slurry, the characterization temperature of the slurry under different laser heating powers and the linear expansion width can be effectively adjusted.
[0092] In some embodiments, the light absorbing filler is in the shape of at least one of granules, spheres, spherical shapes, and flakes. x Mn y O z The shapes are diverse and can be selected according to actual needs. They can be used in any proportion and applied to packaging slurry to improve the dispersion and stacking density of the conductive slurry, which is beneficial to improving the packaging effect.
[0093] In some embodiments, the particle size of the light-absorbing filler is 0.05 to 5 μm, such as 0.1 μm, 25 μm, and 50 μm. The light-absorbing filler provided in the embodiment of the present application is micro-nano-scale, which can improve the mixing uniformity with other materials, thereby improving the Fe x Mn y O z It can be used in slurries to improve the dispersion and stacking density of conductive slurries, which is beneficial to improving the sintering density of slurries. It also has a strong bonding force with substrates or package covers, and it is difficult for water vapor and oxygen to penetrate the gap into the internal sealing area, which can protect the device and effectively solve the defects of resin sealing.
[0094] In some embodiments, the provided sealing glass paste may further include wetting and leveling agents, adhesion promoters, dispersants, etc. according to actual needs. The above-mentioned additives are well known to those skilled in the art and will not be described in detail here.
[0095] In a sixth aspect, the present application provides a method for preparing the above-mentioned laser sealing slurry. The method for preparing the laser sealing slurry of the present application comprises the following steps:
[0096] Step S04: mixing the glass powder, the organic carrier, the functional filler and the light-absorbing filler to obtain the laser sealing slurry;
[0097] The glass powder in step S04 includes the light-absorbing material described in the embodiments of the preceding application, or the light-absorbing material prepared by the method for preparing the light-absorbing material described in the embodiments of the preceding application, or the glass powder described in the embodiments of the preceding application, or the glass powder prepared by the method for preparing the glass powder described in the embodiments of the preceding application. The organic vehicle, functional filler, and light-absorbing filler components are the same as those contained in the laser sealing slurry described above.
[0098] In addition, the mixing ratio of the glass powder, organic vehicle, functional filler, and light-absorbing filler in step S04 can be based on the content ratio of the glass powder, organic vehicle, functional filler, and light-absorbing filler contained in the laser sealing paste described above. The mixing method can be any mixing method that can achieve sufficient mixing of the components.
[0099] The preparation method of the laser sealing slurry in the embodiment of the present application is to mix the glass powder containing the light-absorbing material of the embodiment of the present application with the organic carrier, functional filler and light-absorbing filler component, so that the prepared laser sealing slurry can effectively reduce the laser energy provided in the sealing process while ensuring the sealing performance requirements when packaging electronic products; the laser sealing slurry is also given the function of light absorption and reducing the thermal expansion coefficient, which can improve the dispersibility and stacking density of the laser sealing slurry, and has a strong bonding force with the substrate or packaging cover. In addition, the conditions of the preparation method of the embodiment of the present application are easy to control, which improves the quality stability of the prepared laser sealing slurry.
[0100] In a seventh aspect, an embodiment of the present application provides an application of the above-mentioned laser sealing slurry in the packaging of organic light-emitting diodes, solar photovoltaics, lasers or MEMS.
[0101] Precisely because the laser sealing slurry has a low expansion coefficient and a low glass transition temperature, the embodiment of the present application applies the laser sealing slurry to the packaging of organic light-emitting diodes, solar photovoltaics, lasers or MEMS, which can improve the dispersion and stacking density of the laser sealing slurry, and has a strong bonding force with the substrate or packaging cover. It is difficult for water vapor and oxygen to penetrate the gap into the internal sealing area, which can provide better protection for organic light-emitting diodes, solar photovoltaics, lasers or MEMS, improve the packaging effect and reduce the problem of internal hidden cracks.
[0102] The following describes the details in conjunction with specific embodiments.
[0103] The above embodiments merely illustrate several implementation methods of the present application. While the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that a person skilled in the art could make various modifications and improvements without departing from the spirit of the present invention, all of which fall within the scope of protection of the present invention. Therefore, the scope of protection of the present invention shall be determined by the appended claims.
[0104] 1. Light-absorbing materials and preparation methods
[0105] Example 1-1
[0106] This embodiment provides a light-absorbing material and a preparation method.
[0107] This embodiment provides a light-absorbing material and a preparation method.
[0108] Light-absorbing material, its general formula is FeMnO3.
[0109] The light-absorbing material and preparation method include the following steps:
[0110] Step S01: FeOi and MnOj are mixed and sintered to obtain a light-absorbing material containing FeMnO3.
[0111] Example 1-2
[0112] This embodiment provides a light-absorbing material and a preparation method.
[0113] Light-absorbing material, its general formula is Fe2MnO4.
[0114] The light-absorbing material and preparation method include the following steps:
[0115] Step S01: FeOi and MnOj are mixed and sintered to obtain a light-absorbing material containing Fe2MnO4.
[0116] Examples 1-3
[0117] This embodiment provides a light absorbing material and a preparation method
[0118] Light-absorbing material, its general formula is Fe3MnO5.
[0119] The light-absorbing material and preparation method include the following steps:
[0120] Step S01: FeOi and MnOj are mixed and sintered to obtain a light-absorbing material containing Fe3MnO5.
[0121] 2 Glass frit and preparation method
[0122] Example 2-1
[0123] This embodiment provides a glass powder and a preparation method.
[0124] The glass frit, based on the molar percentage of the glass powder as 100%, includes the following molar percentages of the raw material components:
[0125] Glass powder and preparation method, comprising the following steps:
[0126] Step S02. Weighing the raw materials of each component according to the molar percentage of each component contained in the glass frit described above;
[0127] Step S03: Mix the raw materials of various components, perform melting treatment, and process them to obtain glass powder.
[0128] Example 2-2
[0129] This embodiment provides a glass powder and a preparation method.
[0130] The glass frit, based on the molar percentage of the glass powder as 100%, includes the following molar percentages of the raw material components:
[0131] Glass powder and preparation method, comprising the following steps:
[0132] Step S02. Weighing the raw materials of each component according to the molar percentage of each component contained in the glass frit described above;
[0133] Step S03: Mix the raw materials of various components, perform melting treatment, and process them to obtain glass powder.
[0134] Example 2-3
[0135] This embodiment provides a glass powder and a preparation method.
[0136] The glass frit, based on the molar percentage of the glass powder as 100%, includes the following molar percentages of the raw material components:
[0137] Glass powder and preparation method, comprising the following steps:
[0138] Step S02. Weighing the raw materials of each component according to the molar percentage of each component contained in the glass frit described above;
[0139] Step S03: Mix the raw materials of various components, perform melting treatment, and process them to obtain glass powder.
[0140] Examples 2-4
[0141] This embodiment provides a glass powder and a preparation method.
[0142] The glass frit, based on the molar percentage of the glass powder as 100%, includes the following molar percentages of the raw material components:
[0143] Glass powder and preparation method, comprising the following steps:
[0144] Step S02. Weighing the raw materials of each component according to the molar percentage of each component contained in the glass frit described above;
[0145] Step S03: Mix the raw materials of various components, perform melting treatment, and process them to obtain glass powder.
[0146] Comparative Example 2-1
[0147] This comparative example provides a glass powder and a preparation method.
[0148] The glass frit, based on the molar percentage of the glass powder as 100%, includes the following molar percentages of the raw material components:
[0149] Glass powder and preparation method, comprising the following steps:
[0150] Step S02. Weighing the raw materials of each component according to the molar percentage of each component contained in the glass frit described above;
[0151] Step S03: Mix the raw materials of various components, perform melting treatment, and process them to obtain glass powder.
[0152] Comparative Example 2-2
[0153] This comparative example provides a glass powder and a preparation method.
[0154] The glass frit, based on the molar percentage of the glass powder as 100%, includes the following molar percentages of the raw material components:
[0155] Glass powder and preparation method, comprising the following steps:
[0156] Step S02. Weighing the raw materials of each component according to the molar percentage of each component contained in the glass frit described above;
[0157] Step S03: Mix the raw materials of various components, perform melting treatment, and process them to obtain glass powder.
[0158] Comparative Examples 2-3
[0159] This comparative example provides a glass powder and a preparation method.
[0160] The glass frit, based on the molar percentage of the glass powder as 100%, includes the following molar percentages of the raw material components:
[0161] Glass powder and preparation method, comprising the following steps:
[0162] Step S02. Weighing the raw materials of each component according to the molar percentage of each component contained in the glass frit described above;
[0163] Step S03: Mix the raw materials of various components, perform melting treatment, and process them to obtain glass powder.
[0164] Comparative Examples 2-4
[0165] This comparative example provides a glass powder and a preparation method.
[0166] The glass frit, based on the molar percentage of the glass powder as 100%, includes the following molar percentages of the raw material components:
[0167] Glass powder and preparation method, comprising the following steps:
[0168] Step S02. Weighing the raw materials of each component according to the molar percentage of each component contained in the glass frit described above;
[0169] Step S03: Mix the raw materials of various components, perform melting treatment, and process them to obtain glass powder.
[0170] Comparative Examples 2-5
[0171] This comparative example provides a glass powder and a preparation method.
[0172] The glass frit, based on the molar percentage of the glass powder as 100%, includes the following molar percentages of the raw material components:
[0173] Glass powder and preparation method, comprising the following steps:
[0174] Step S02. Weighing the raw materials of each component according to the molar percentage of each component contained in the glass frit described above;
[0175] Step S03: Mix the raw materials of various components, perform melting treatment, and process them to obtain glass powder.
[0176] Comparative Examples 2-6
[0177] This comparative example provides a glass powder and a preparation method.
[0178] The glass frit, based on the molar percentage of the glass powder as 100%, includes the following molar percentages of the raw material components:
[0179] Glass powder and preparation method, comprising the following steps:
[0180] Step S02. Weighing the raw materials of each component according to the molar percentage of each component contained in the glass frit described above;
[0181] Step S03: Mix the raw materials of various components, perform melting treatment, and process them to obtain glass powder.
[0182] Comparative Examples 2-7
[0183] This comparative example provides a glass powder and a preparation method.
[0184] The glass frit, based on the molar percentage of the glass powder as 100%, includes the following molar percentages of the raw material components:
[0185] Glass powder and preparation method, comprising the following steps:
[0186] Step S02. Weighing the raw materials of each component according to the molar percentage of each component contained in the glass frit described above;
[0187] Step S03: Mix the raw materials of various components, perform melting treatment, and process them to obtain glass powder.
[0188] 3 Laser sealing slurry and preparation method
[0189] Example 3-1
[0190] This embodiment provides a slurry for laser sealing and a preparation method.
[0191] The slurry for laser sealing includes a mixture of the glass powder, β-eucryptite, copper chromium black, and an organic carrier in Example 2-1, and the mass ratio of the glass powder, β-eucryptite, copper chromium black, and the organic carrier in Example 2-1 is 74:3:3:20.
[0192] A method for preparing a slurry for laser sealing comprises the following steps:
[0193] The glass powder, β-eucryptite, copper chrome black and organic carrier in Example 2-1 are mixed to obtain a slurry for laser sealing.
[0194] Comparative Example 3-1
[0195] This comparative example provides a slurry for laser sealing and a preparation method.
[0196] The slurry for laser sealing includes a mixture of the glass powder, β-eucryptite, copper chromium black and an organic carrier in Comparative Example 2-3, and the mass ratio of the glass powder, β-eucryptite, copper chromium black and the organic carrier in Comparative Example 2-3 is 74:3:3:20.
[0197] A method for preparing a slurry for laser sealing comprises the following steps:
[0198] The glass powder, β-eucryptite, copper chromium black and organic carrier in Comparative Example 2-3 are mixed to obtain a slurry for laser sealing.
[0199] Comparative Example 3-2
[0200] This embodiment provides a slurry for laser sealing and a preparation method.
[0201] The slurry for laser sealing includes a mixture of the glass powder, β-eucryptite and an organic carrier in Comparative Example 2-3, and the mass ratio of the glass powder, β-eucryptite and the organic carrier in Comparative Example 2-3 is 77:3:20.
[0202] A method for preparing a slurry for laser sealing comprises the following steps:
[0203] The mixture of the glass powder, β-eucryptite and the organic carrier in Comparative Example 2-3 is mixed, and the glass powder, β-eucryptite and the organic carrier in Comparative Example 2-3 are mixed to obtain a slurry for laser sealing.
[0204] Performance Testing
[0205] 1. Performance test of glass powder
[0206] The glass transition temperature, crystallization temperature and thermal expansion coefficient of the glass powders in Examples 2-1 to 2-4 and Comparative Examples 2-1 to 2-7 were measured. The results are shown in Table 1.
[0207] Table 1
[0208] As can be seen from Table 1, the glass transition temperatures of the glass frits in Examples 2-1 to 2-4 range from 365°C to 396°C, which is lower than the glass transition temperature of the glass frit in Comparative Example 2-6. Figure 1 shows the TG-DSC characteristic temperature graph of the glass frit in Example 2-1, which shows a relatively low glass transition temperature.
[0209] The crystallization temperature of the glass powder in Examples 2-1 to 2-4 is 495-532° C., which is lower than the crystallization temperature of the glass powder in Comparative Example 2-1, Comparative Example 2-2, Comparative Example 2-3, Comparative Example 2-6, and Comparative Example 2-7.
[0210] The thermal expansion coefficient of the glass powder in Examples 2-1 to 2-4 is 52 to 55×10 -6 / °C, which is lower than the thermal expansion coefficient of the glass powder in Comparative Example 2-1, Comparative Example 2-2, Comparative Example 2-3, Comparative Example 2-6 and Comparative Example 2-7.
[0211] In summary, the glass powders provided by Examples 2-1 to 2-4 exhibit excellent mechanical strength and thermal expansion coefficient. Compounds based on these characteristics, such as low-melting-point glass, offer advantages such as low sealing temperature, stable performance, and excellent fluidity, making them suitable for use in inorganic solders in place of lead-based glass. Furthermore, the glass powders provided by the present examples are lead-free, thus preventing environmental damage and harming human health.
[0212] Moreover, it can be seen from Table 1 that the glass powder of the embodiment of the present application contains Fe x Mn y O z It can improve the absorption of sealing laser, convert light energy into heat energy, promote better melting and sealing of slurry, and also reduce the thermal expansion coefficient. x Mn y O z It does not cause Tg to be too high, but mainly improves the light absorption performance and reduces the thermal expansion coefficient, which does not cause the thermal expansion coefficient to be too large and the stress to be large, which is beneficial to glass sealing. x Mn y O zThe presence of will not significantly change the crystallization temperature of the glass powder (because lowering the crystallization temperature of the glass will easily cause crystallization during pre-firing, which is not conducive to sealing stability), thereby improving the sealing stability of the glass powder containing the embodiment of the present application. For example, the crystallization temperature (crystallization temperature) data of the glass powder of the embodiment of the present application can show that when pre-sintering is performed at a temperature below 500°C, the glass does not crystallize and will not affect the sealing.
[0213] When the glass powder does not contain Fe x Mn y O z However, when it contains higher TeO2 and B2O3 (such as Comparative Example 2-1 and Comparative Example 2-2) or Bi2O3 (such as Comparative Example 2-4), although the Tg temperature can be lowered, the thermal expansion coefficient of the glass powder increases.
[0214] Similarly, when the glass powder does not contain Fe x Mn y O z However, when the glass powder contains a higher amount of CuO (such as Comparative Examples 2-5 and 2-7), CuO has a bond-breaking effect, which greatly reduces the Tg of the glass powder (such as Comparative Example 2-5), but still increases the thermal expansion coefficient of the glass powder.
[0215] 2 Performance test of laser sealing slurry
[0216] The density, bonding ratio, and tensile properties of the laser sealing slurries in Example 3-1, Comparative Examples 3-1, and Comparative Examples 3-2 were measured. The results are shown in Table 2. (The bonding ratio is defined as the bonding width of the glass film after laser sintering / the width of the glass film after pre-sintering * 100%).
[0217] Table 2 Performance comparison of slurry after laser sintering
[0218] It can be seen from Table 2 that the light-absorbing material in Example 3-1 is an inorganic material that is resistant to acid, alkali and chemical corrosion. When used in the laser sealing slurry, it not only gives the laser sealing slurry light-absorbing properties and reduces the thermal expansion coefficient, but also improves the dispersion and stacking density of the laser sealing slurry. It also has a strong bonding force with the substrate or the packaging cover, and it is difficult for water vapor and oxygen to penetrate into the internal sealing area through the gap, which can provide better protection for the device, improve the packaging effect and reduce the problem of internal hidden cracks.
[0219] It can be clearly seen from Figures 2 to 4 that after pre-sintering, the cross-sectional structure of the laser sealing slurry in Comparative Example 3-1 is loose and porous, while the laser sealing slurry in Example 3-1 and the laser sealing slurry in Comparative Example 3-2 have denser structures. The pre-sintering state and light absorption properties will affect the sealing performance of the product after laser sintering. The cross-sectional morphologies of pre-sintered samples A, B, and C are sintered at a laser power of 11.5W, as shown in Figures 5 to 7. It can be seen that the cross-sectional structure of the laser sealing slurry in Comparative Example 3-1 is relatively porous, while the cross-sectional structure of the laser sealing slurry in Example 3-1 is denser. Due to the lack of light-absorbing fillers, the laser sealing slurry in Comparative Example 3-2 is in an under-molten state, resulting in lower tensile strength after sealing.
[0220] Therefore, compared with Comparative Example 3-1 (containing the same content of β-eucryptite with low thermal expansion coefficient and copper chromium black to further increase the light absorption performance, the difference is that glass powder with different components is used), under the same laser power, due to the use of the glass powder of the present application embodiment with low thermal expansion coefficient in Example 3-1, its expansion degree after light absorption and melting is lower, which is manifested as a lower bonding ratio during sealing, and the interior of the cross section is denser when observed under an electron microscope. Compared with Comparative Example 3-2, Example 3-1 does not contain the light absorbing material copper chromium black, resulting in less heat energy converted by laser, a lack of glass powder molten flow state, inability to effectively seal, and a tensile force of NG. Therefore, there is a synergistic effect between the glass powder of the present application embodiment and components such as β-eucryptite and copper chromium black, which improves the overall effect.
[0221] The above description is only a preferred embodiment of the present application and is not intended to limit the present application. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present application should be included in the scope of protection of the present application.
Claims
1. A light absorbing material, characterized in that: Its general formula is Fe x Mn y O z , where 1≤x≤10, 1≤y≤5, 1≤z≤17.
2. The light absorbing material according to claim 1, characterized in that: The Fe x Mn y O z Including FeO i With MnO j The composition of Fe x Mn y O z It is a crystalline compound, wherein 0≤i≤3, 0≤j≤4.
3. The light absorbing material according to claim 2, characterized in that: The Fe x Mn y O z Including FeMnO3, Fe2MnO4, Fe3MnO5, Fe4MnO6, FeMn2O3, FeMn3O7, FeMn4O9, Fe2MnO5, Fe4MnO8, Fe6MnO 11 、Fe8MnO 16 , Fe2Mn2O7, Fe2Mn3O9, Fe2Mn4O 11 、Fe5MnO7、FeMn5O 11 , Fe 10 MnO 17 、Fe2Mn5O 13 At least one of .
4. The light absorbing material according to any one of claims 1 to 3, characterized in that: The Fe x Mn y O z The shape is at least one of granular, spherical, quasi-spherical, and flake.
5. The light absorbing material according to any one of claims 1 to 4, characterized in that: The Fe x Mn y O z The particle size is 0.1~50μm.
6. A method for preparing a light-absorbing material, characterized in that: The steps include: Will include FeO i With MnO j After mixing, sintering is performed to obtain Fe x Mn y O z light-absorbing material, wherein 0≤i≤3, 0≤j≤4, 1≤x≤10, 1≤y≤5, 1≤z≤17.
7. The preparation method according to claim 6, characterized in that: The sintering temperature is 1000-1400°C.
8. The preparation method according to claim 6 or 7, characterized in that: The FeO i With MnO j The mass ratio is 0.13~11.
5.
9. A glass powder, characterized in that: The light-absorbing material comprises the light-absorbing material according to any one of claims 1 to 5 or the light-absorbing material prepared by the preparation method according to any one of claims 6 to 8.
10. The glass powder according to claim 9, characterized in that: Taking the molar percentage of the glass powder as 100%, it includes the following molar percentages of the raw material components:
11. The glass powder according to claim 10, characterized in that: The other oxides include at least one of SiO2, CuO, Co3O4, BaO, Al2O3, MgO, CaO, TiO2, WO3, and SrO.
12. The glass powder according to any one of claims 9 to 11, characterized in that: The glass powder includes at least one of amorphous glass and microcrystalline glass.
13. A method for preparing glass powder, characterized in that: The steps include: Weigh the raw materials of each component according to the molar percentage of each component contained in the glass frit according to any one of claims 9 to 12; The component raw materials are mixed, melted and processed to obtain the glass material.
14. The preparation method according to claim 13, characterized in that: The temperature of the melting treatment is 600-1500°C.
15. A slurry for laser sealing, characterized in that: The invention comprises the light-absorbing material according to any one of claims 1 to 5 or the light-absorbing material obtained by the preparation method according to any one of claims 6 to 8 or the glass powder according to any one of claims 9 to 12 or the glass powder obtained by the preparation method according to claim 13 or 14.
16. The laser sealing slurry according to claim 15, characterized in that: The laser sealing slurry further comprises an organic carrier, a functional filler and a light-absorbing filler, and the weight proportions of the glass powder, the organic carrier, the functional filler and the light-absorbing filler are as follows:
17. The laser sealing slurry according to claim 16, characterized in that: The functional filler comprises at least one of β-eucryptite, zirconium phosphotungstate, zirconium tungstate, cordierite, zirconium oxide, and zirconium powder; and / or, The functional filler is in the shape of at least one of granular, spherical, quasi-spherical, and flake; and / or, The particle size of the functional filler is 0.05-5 μm.
18. The laser sealing slurry according to claim 16 or 17, characterized in that: The light-absorbing filler includes at least one of copper chrome black, iron manganese black, iron chrome black, silicon carbide, and tungsten powder; and / or, The light-absorbing filler is in the shape of at least one of granules, spheres, quasi-spheres, and flakes; and / or, The particle size of the light absorbing filler is 0.05-5 μm.
19. A method for preparing a slurry for laser sealing, characterized in that: The steps include: The glass powder, the organic carrier, the functional filler and the light-absorbing filler are mixed to obtain the slurry for laser sealing; Wherein, the glass powder comprises the light-absorbing material according to any one of claims 1-5 or the light-absorbing material obtained by the preparation method according to any one of claims 6-8 or the glass powder according to any one of claims 9-12 or the glass powder obtained by the preparation method according to claim 13 or 14.
20. Use of the laser sealing slurry according to any one of claims 15 to 18 or the laser sealing slurry prepared by the preparation method according to claim 19 in packaging organic light emitting diodes, solar photovoltaics, lasers or MEMS.
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