CN115734467A - Copper electrode slurry for COB (chip on board) packaging glass substrate and preparation method thereof - Google Patents
Copper electrode slurry for COB (chip on board) packaging glass substrate and preparation method thereof Download PDFInfo
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Abstract
The invention provides copper electrode paste for a COB (chip on board) packaging glass substrate and a preparation method thereof, wherein the formula of the copper electrode paste comprises the following components in percentage by mass: 65-75% of copper powder, 15-30% of organic carrier, 5-10% of glass powder and 0.2-0.5% of organic additive, wherein the copper powder is prepared by mixing several copper powders with different particle sizes and different shapes, and the glass powder is prepared by mixing two glass powders with different sintering characteristics. The copper electrode slurry prepared by the invention has good conductivity, printability and matching property with a substrate sintered by N 2 After the atmosphere high-temperature sintering, the copper layer has no obvious shrinkage, the dry film adhesive force of the copper layer is high, and the copper layer has excellent acid and alkali resistance and excellent adhesive force, and can completely replace the application of silver paste on a glass substrate.
Description
Technical Field
The invention relates to the technical field of conductive copper electrode paste, in particular to copper electrode paste for a COB (chip on board) packaging glass substrate and a preparation method thereof.
Background
The thick film electronic paste is formed by printing an electrode circuit on a ceramic substrate and sintering at high temperature. Compared with the common PCB, the PCB has remarkable advantages in the aspects of heat dissipation and stability, has remarkable value advantages in severe environments such as high temperature, high humidity, high power and high vibration, and is mainly applied to the fields of automobile electronics, communication systems, aerospace, military and the like.
The thick film circuit mainly comprises a substrate and thick film electronic paste. The substrate is a carrier of the thick film circuit, mainly comprises a ceramic substrate, a polymer substrate, a glass substrate and a composite substrate, and the material performance of the substrate has important influence on the quality of the thick film circuit. The most common being used today are ceramic substrates.
The thick film electronic paste is the core and key of a thick film circuit, and can be divided into the following parts according to the purposes: resistance paste, conductor paste and dielectric paste. The quality of the film directly influences the performance of the rear film element and the printed board.
With the development of technology, substrates for packaging COB light sources for LED lighting have been developed and updated from aluminum substrates → copper substrates → ceramic substrates → glass substrates → sapphire substrates. Since the light emitting efficiency of the COB light source packaging glass substrate for LED illumination is larger than or equal to 140Lm/W, the 4W LED lamp is equivalent to the brightness (about 600 lumens) of a 40W incandescent lamp, which means that the energy can be saved by 9 times (or 90%) and the service life can be improved by more than 10 times (at least 20000h, as high as 250000 h). In view of the above, glass substrates for COB light sources for LED lighting (particularly, high thermal conductivity type glass substrates) have a better light emission effect and lower cost than metal substrates (AI substrates, cu substrates), ceramic substrates, and the like, and therefore, glass substrates for LED lighting have a wide spread application value and a wide market.
The conventional electrode paste such as COB packaging substrate is mainly made of silver paste, and due to the fact that silver has excellent conductivity and sintering activity, a compact metal layer can be formed under high-temperature sintering, and the electrode paste has excellent weldability, solder resistance, conductivity and the like, is simple in sintering process, and is easy to realize mass production. With the wider application of products and larger usage amount, the cost becomes a main consideration factor of merchants, copper as base metal has the conductivity similar to that of silver, and the price of copper is 1/5-1/10 of the price of silver, so that the copper paste replacing silver prize as thick film paste electrode paste has the advantage of remarkably reducing cost, and becomes the development trend of future thick film paste.
The patent application publication No. CN 105934416A discloses a glass substrate provided with copper-based conductive tapes, which discloses a preparation method and application range of copper paste for glass-based use, but the design and application of the glass-based copper paste are more specific, and the formula and preparation method of the copper paste for glass substrate are not described in detail.
The patent application publication No. CN 104658633A mentions 'a formula and a preparation method of conductive copper paste for an automobile glass hot wire', and the patent mentions a preparation method of the conductive copper paste for a glass substrate, which is applied to the field of automobile rear windshield heating wires, wherein the sintering temperature is higher than 600 ℃, and the sintering process condition of the copper paste for the COB packaging glass substrate is not met.
In patent application publication No. CN112125527A, it is also mentioned "a high thermal expansion glass powder for copper paste and its preparation method and application", and the preparation and test method of glass powder is described mainly in the aspect of glass preparation, and the application performance of copper paste prepared from the glass powder on different ceramic substrates is not described.
In view of the current few studies on copper paste for glass substrates, especially on COB-packaged glass substrates, or the results of the COB-packaged glass substrates being comparable to foreign products, it is necessary to provide a copper electrode paste to solve the above problems.
Disclosure of Invention
According to the problems of few researches on the aspect of domestic glass substrate copper paste, the copper electrode paste for COB packaging glass substrates and the preparation method thereof are provided. The invention starts from a glass substrate for packaging a COB light source of LED illumination, mainly considers mutual matching of copper powder, glass powder and polymer resin of different types, realizes conductive copper paste with excellent performance comparable to that of silver paste on the glass substrate, adopts copper paste to replace the silver paste to be printed electrode circuit paste, realizes cost reduction substitution, finally realizes high conductivity, high welding tension and high sintering compactness, and can be used as a conductive copper paste product comparable to that of foreign products.
The technical means adopted by the invention are as follows:
the copper electrode slurry for the COB packaging glass substrate comprises the following components in percentage by mass:
65-75% of copper powder, wherein the copper powder is prepared by mixing spherical powder and flaky powder, and the particle size D50 of the spherical powder is 0.2-1.5 mu m; the grain diameter D50 of the flaky powder is 3.0-7.0 mu m;
15% -30% of organic carrier;
5-10% of glass powder, wherein the glass powder is formed by mixing two kinds of glass powder with different sintering characteristics, and the glass powder A is formed by mixing 40-70% of bismuth oxide, 5-20% of boric acid, 5-20% of silicon oxide, 5-10% of basic copper carbonate, 0.5-2% of manganese dioxide, 0-5% of one or more of alkaline earth metal oxides and 0-3% of one or more of alkali metal oxides in percentage by mass; the glass powder B is prepared by mixing one or more of 40-60% of bismuth oxide, 20-40% of boric acid, 0-5% of zinc oxide, 0-1% of aluminum oxide, 5-10% of alkaline earth metal oxide and 0-3% of alkali metal oxide;
0.2 to 0.5 percent of organic additive.
Copper powder is used as a functional phase of the conductive paste, has good conductivity and heat conductivity, excellent physical and mechanical properties, and has a remarkable advantage in price compared with precious metals such as gold, platinum, palladium, silver and the like, and is widely applied to various conductive and resistance pastes. Silver powders of different types, different particle sizes and different morphologies have different effects on the application field of the slurry.
The copper powder of the present invention is relatively broad in kind, and includes spherical copper powder and flake copper powder. Wherein the grain diameter D50 of the spherical powder is 0.2-1.5 μm; the particle size D50 of the flaky powder is 3.0-7.0 mu m, and the flaky powder has good dispersibility and stacking compactness in slurry, and is favorable for improving the compactness and good conductivity of the sintered silver layer.
The glass powder is used as a sintering aid and a bonding agent in the copper paste, so that the densification degree of the sintered copper layer is improved, and the copper layer and the substrate form effective combination. The primary factor affecting the action of the glass frit in the paste is the characteristic softening temperature of the glass frit. The softening point is too high, the sintering activity is low, the wettability to copper powder is poor, the sintering compactness of the copper powder is reduced, and the conductivity of a copper layer is influenced; too low a softening point may cause excessive erosion of the substrate, resulting in a decrease in the electrical properties of the substrate itself. Therefore, the selection of a proper glass system has significant significance on the performance of the conductive copper paste.
The two kinds of glass powder provided by the invention are matched by adopting the glass powder with different sintering characteristics, wherein the glass powder A has a characteristic temperature with a wide adjustable range, has good wettability on a glass substrate and copper powder, can improve the sintering activity of the copper powder, and improves the compactness of a copper layer; the glass powder B belongs to microcrystalline glass, is microcrystalline in the sintering process, improves the acid and alkali resistance of a copper film, and improves the mechanical strength of a glass substrate. The copper layer is ensured to have excellent welding adhesion, electrical property and ageing resistance by matching the copper layer and the copper layer.
Further, the organic carrier is prepared from 65-75% of high molecular resin and 70-90% of organic solvent.
Furthermore, the polymer resin is formed by mixing ethyl cellulose and acrylic resin according to a preset proportion.
Further, the organic solvent is selected from one or more of alcohols or ethers, wherein the alcohols comprise one or more of terpineol, turpentine and alcohol ester dodeca, and the ethers comprise one or two of diethylene glycol butyl ether and diethylene glycol butyl ether acetate.
Further, the organic additive comprises a leveling agent, a coupling agent, a defoaming agent, a thixotropic agent and the like, wherein the coupling agent can be selected from a silane coupling agent and the like; the thixotropic agent can be selected from hydrogenated castor oil, polyamide wax, etc.
The invention also discloses a preparation method of the copper electrode slurry for the COB packaging glass substrate, which is characterized by comprising the following steps:
s1, mixing different types of polymer resins according to a preset proportion, mixing the mixed resins with an organic solvent and an organic additive according to a certain proportion, and fully dissolving the mixed resins to obtain a required organic carrier;
s2, uniformly mixing the organic carrier prepared in the step S1 with copper powder, glass powder and an organic additive according to the slurry proportion to obtain a mixture;
and S3, fully grinding the mixture by using a three-roll machine to obtain a copper electrode slurry preformed product, and filtering, testing and adjusting the viscosity of the copper slurry preformed product until the copper electrode slurry meeting the requirements is obtained.
Further, in the step S1, the organic solvent is added and then the polymer resin is added into the reaction kettle in sequence, the water bath heating temperature of the reaction kettle is stable, and the mixture is stirred and dissolved completely; and adding a preset organic additive into the completely dissolved and transparent carrier, and continuously stirring and heating to obtain the required organic carrier.
Further, in step S2, the preparation of the two kinds of glass frits includes the following steps:
s21, converting into a specific raw material mass ratio according to a preset glass oxide formula, and accurately weighing;
s22, fully mixing the weighed raw materials in a mixer to ensure that the raw materials with different components are uniformly mixed;
s23, placing the mixed raw materials into an alumina crucible, then placing the crucible into a muffle furnace to be melted at 1100-1350 ℃ and preserving heat for 30-60 min;
s24, pouring the melted glass liquid into deionized water for water quenching to obtain glass particles with the size of about 1 mm;
s25, filling the glass particles into a ball milling tank, carrying out ball milling for 8-12 h, sieving by a 500-mesh sieve, and drying in an oven at 120 ℃ to obtain required glass powder, wherein the particle size of the glass powder is controlled to be D50: 3-5 μm.
Further, in the step S3, the mixture is sufficiently ground by a three-roll mill for 5 to 8 times, and the viscosity is controlled to be 50 to 100 pas.
Compared with the prior art, the invention has the following advantages:
1. the invention starts from the formula of copper paste, the selected copper powder is compounded and matched, the copper powder is prepared by matching nano-scale copper powder with certain flake powder and balls, the sintering activity is high, and the low-temperature sintering is met.
2. The adhesive force of the copper paste on the glass substrate is very low, and the invention adopts two glass powders with different characteristics to match, thereby improving the adhesive force of the metal layer: the glass A adopts bismuth-copper-manganese-silicon-lithium glass, the wettability and the corrosivity of the glass and the glass for several shifts are improved, the glass B has excellent acid resistance and mechanical strength, copper paste prepared by matching the bismuth-copper-manganese-silicon-lithium glass and the glass is high in sintering activity, the copper layer densification degree is high, the adhesion with a glass substrate is high, and the metal layer is good in resistance.
In conclusion, the copper electrode slurry prepared by matching different types of copper powder, glass powder and polymer resin has good conductivity, printability and matching property with matrix sintering. Warp of N 2 In the atmosphere, after the conductive copper paste is sintered on the glass substrate at the temperature of below 600 ℃, the copper layer has no obvious shrinkage, the dry film adhesive force of the copper layer is high, and the conductive copper paste has excellent acid and alkali resistance and excellent adhesive force, and can completely replace the application of the silver paste on the glass substrate.
Therefore, the copper electrode paste provided by the invention has a wider sintering window, can be matched with different sintering curves of customers, finally realizes high conductivity, high welding tension and high sintering compactness, fills the blank of the domestic application of the technology, can be used as a conductive copper paste product comparable to foreign products, and plays a key role in promoting the development of the domestic glass substrate in the COB packaging field.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the description of the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is an SEM image of the glass frit of the present invention.
FIG. 2 is a metallographic microscope photograph of a sintered copper paste according to example 1 of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments of the present invention may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The invention provides copper electrode paste for a COB (chip on Board) packaging glass substrate, which comprises the following components in percentage by mass:
65-75% of copper powder, wherein the copper powder is prepared by mixing spherical powder and flaky powder, and the particle size D50 of the spherical powder is 0.2-1.5 mu m; the particle size D50 of the flaky powder is 3.0-7.0 mu m;
15-30% of organic carrier, which is prepared by 65-75% of macromolecular resin and 70-90% of organic solvent; the polymer resin is prepared by mixing ethyl cellulose and acrylic resin according to a certain proportion; the organic solvent is selected from one or more of alcohols or ethers, wherein the alcohols comprise one or more of terpineol, turpentine and alcohol ester dodeca, and the ethers comprise one or two of diethylene glycol butyl ether and diethylene glycol butyl ether acetate;
the glass powder A is formed by mixing 40-70% of bismuth oxide, 5-20% of boric acid, 5-20% of silicon oxide, 5-10% of basic copper carbonate, 0.5-2% of manganese dioxide, 0-5% of one or more of alkaline earth metal oxides and 0-3% of one or more of alkali metal oxides in percentage by mass; the glass powder B is one or a mixture of more of 40 to 60 percent of bismuth oxide, 20 to 40 percent of boric acid, 0 to 5 percent of zinc oxide, 0 to 1 percent of aluminum oxide, 5 to 10 percent of alkaline earth metal oxide and 0 to 3 percent of alkali metal oxide;
0.2 to 0.5 percent of organic additive, which at least comprises a flatting agent, a coupling agent, a thixotropic agent and the like, wherein the coupling agent can be selected from a silane coupling agent and the like; the thixotropic agent can be selected from hydrogenated castor oil, polyamide wax, etc.
The invention also discloses a preparation method of the copper electrode slurry for the COB packaging glass substrate, which comprises the following steps:
s1, mixing high molecular resins with different molecular weights according to a certain proportion, mixing the high molecular resins with an organic solvent and an organic additive according to a certain proportion, and fully dissolving the mixture to obtain a required organic carrier;
in order to guarantee the viscosity of the conductive silver paste and the printing stability, the preparation method of the preferable carrier is particularly proposed, and comprises the following steps:
(1) The above-mentioned preferred organic solvent and the polymer resin are precisely weighed according to the designed formulation ratio.
(2) The raw materials are added with organic solvent and then added with polymer resin in sequence, the resin is ensured not to agglomerate, sink to the bottom and the like, the water bath heating temperature of the reaction kettle is stabilized at 85 ℃, the rotating speed of a stirrer is 150, and the raw materials are stirred and dissolved for 3 to 5 hours.
(3) Adding designed organic additive into the completely transparent carrier, and stirring and heating for 0.5min. The organic resin is fully organic solvent to be transparent, undissolved particles can not exist, and the addition of the additives can ensure that the paste has good printing performance and stability.
(4) And after stirring is finished, discharging the prepared organic carrier into a stainless steel barrel prepared in advance, covering the stainless steel barrel with a cover, placing the organic carrier to room temperature, naturally cooling the organic carrier, and avoiding the instability of the viscosity of the carrier caused by the volatilization of an organic solvent so as to obtain the organic carrier required by the invention.
S2, uniformly mixing the organic carrier, silver powder and glass powder according to a ratio to obtain a mixture;
in order to ensure the excellent performance of the conductive copper paste, the preparation method of the glass powder matrix is provided as follows:
(1) Converting into specific raw material mass ratio according to the designed glass oxide formula, and accurately weighing.
(2) The weighed raw materials are fully mixed in a mixer, so that the raw materials with different components are uniformly mixed.
(3) Placing the mixed raw materials into an alumina crucible, then placing the crucible into a muffle furnace to be melted at 1100-1350 ℃ and preserving the temperature for 30-60 min.
(4) And pouring the melted glass liquid into deionized water for water quenching to obtain glass particles with the particle size of about 1 mm.
(5) And (2) putting the glass particles into a ball milling tank, performing ball milling for 8-12 h, sieving by using a 500-mesh sieve, and then putting into an oven to be dried at 120 ℃ to obtain the required glass powder, wherein the particle size of the glass powder is controlled to be D50: 3-5 μm.
And S3, fully grinding the mixture for 5-8 times by using a three-roller machine to obtain a hole electrode slurry preformed product, and filtering, testing and adjusting the viscosity of silver paste of the preformed product until the hole electrode conductive silver paste meeting the requirements is obtained.
In order to ensure excellent printability of the conductive copper paste, the viscosity of the conductive copper paste of the present invention is preferably controlled to 50 to 100 pas. Unless otherwise specified, the viscosity of the present invention is measured using a Broodfield (DV 2T) viscometer, 14#/10 rpm.
Table 1 shows an example of the preparation of the conductive copper paste according to the present invention. The organic solvent in the example is three mixed solvents of terpineol, alcohol ester twelve and diethylene glycol butyl ether acetate, the solvent ratio is 1; the comparison sample is silver paste sold in the market at present.
TABLE 1
The composition of the glass frit A in the above case is given in Table 2 below
TABLE 2
| Mass ratio of | Example 1 | Example 2 | Example 3 | Example 4 |
| Bismuth oxide | 45 | 55 | 60 | 70 |
| |
20 | 20 | 15 | 10 |
| |
20 | 10 | 10 | 5 |
| Basic copper carbonate | 8 | 8 | 8 | 8 |
| Manganese dioxide | 1 | 1 | 1 | 1 |
| Mixed alkaline earth metal oxides | 4 | 2 | 2 | 2 |
| Mixed alkali metal oxides | 2 | 4 | 4 | 4 |
| Is totaled | 100 | 100 | 100 | 100 |
The composition of the glass frit B in the above case is given in Table 3 below
TABLE 3
| Mass ratio of | Example 1 | Example 2 | Example 3 | Example 4 |
| Bismuth oxide | 50 | 55 | 60 | 60 |
| Boric acid | 35 | 30 | 25 | 30 |
| Zinc oxide | 0.5 | 0.5 | 0.5 | 0.5 |
| Aluminum oxide | 1 | 1 | 1 | 1 |
| Mixed alkaline earth metal oxides | 10 | 10 | 10 | 5 |
| Mixed alkali metal oxides | 3.5 | 3.5 | 3.5 | 3.5 |
| Is totaled | 100 | 100 | 100 | 100 |
Conductive copper pastes A1, A2, A3 and A4 and comparative silver paste AD1 are prepared according to the method, and the prepared copper pastes are verified by comparative tests.
And (3) testing results:
the copper pastes A1, A2, A3, A4 prepared according to the examples and the comparative silver paste AD1 were each subjected to a surface printing test and then N on a chain furnace 2 Sintering is carried out in the atmosphere, the sintering peak temperature is 580 ℃, and the peak temperature heat preservation time is 150min. Then, the conductivity, sintering compactness and interlayer continuity of each sample are tested, and the test results are shown in the following table 4:
TABLE 4
In conclusion, the invention provides a preparation method of copper electrode paste for a COB (chip on Board) packaging glass substrate, the conductive copper paste has good bonding property with a glass substrate, phenomena such as bubbling and falling of a metal layer can not occur after printing and sintering, and each index is equivalent to that of a comparative silver paste in performance test, so that the conductive copper paste can be used as electrode electronic paste for the glass substrate instead of the silver paste. The morphology of the glass frit can be seen in fig. 1; figure 2 is a photomicrograph of the copper layer.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. The copper electrode paste for the COB (chip on Board) packaging glass substrate is characterized by comprising the following components in percentage by mass:
65-75% of copper powder, wherein the copper powder is prepared by mixing spherical powder and flaky powder, and the particle size D50 of the spherical powder is 0.2-1.5 mu m; the grain diameter D50 of the flaky powder is 3.0-7.0 mu m;
15% -30% of organic carrier;
the glass powder A is formed by mixing 40-70% of bismuth oxide, 5-20% of boric acid, 5-20% of silicon oxide, 5-10% of basic copper carbonate, 0.5-2% of manganese dioxide, 0-5% of one or more of alkaline earth metal oxides and 0-3% of one or more of alkali metal oxides in percentage by mass; the glass powder B is one or a mixture of more of 40 to 60 percent of bismuth oxide, 20 to 40 percent of boric acid, 0 to 5 percent of zinc oxide, 0 to 1 percent of aluminum oxide, 5 to 10 percent of alkaline earth metal oxide and 0 to 3 percent of alkali metal oxide;
0.2 to 0.5 percent of organic additive.
2. The copper electrode paste for COB package glass substrates according to claim 1, wherein the organic vehicle is prepared from 65-75% of a polymeric resin and 70-90% of an organic solvent.
3. The copper electrode paste for COB package glass substrates of claim 2, wherein the polymeric resin is formed by mixing ethyl cellulose and acrylic resin according to a preset ratio.
4. The copper electrode paste for COB packaging glass substrates according to claim 2, wherein the organic solvent is selected from one or more of alcohols or ethers, wherein the alcohols include one or more of terpineol, turpentine, and alcohol ester twelve, and the ethers include one or two of diethylene glycol butyl ether and diethylene glycol butyl ether acetate.
5. The copper electrode paste for COB (chip on board) packaging glass substrates according to claim 1, wherein the organic additive comprises at least one or more of a leveling agent, a coupling agent, an antifoaming agent and a thixotropic agent.
6. The method for preparing copper electrode paste for COB package glass substrates according to any one of claims 1 to 5, comprising the steps of,
s1, mixing different types of polymer resins according to a preset proportion, mixing the mixed resins with an organic solvent and an organic additive according to a certain proportion, and fully dissolving the mixed resins to obtain a required organic carrier;
s2, uniformly mixing the organic carrier prepared in the step S1 with copper powder, glass powder and an organic additive according to a slurry ratio to obtain a mixture;
and S3, fully grinding the mixture by using a three-roller machine to obtain a copper electrode slurry preform, and filtering, testing and adjusting viscosity of the copper electrode slurry preform until the copper electrode slurry meeting the requirements is obtained.
7. The preparation method according to claim 6, wherein in the step S1, the organic solvent is added first and then the polymer resin is added, and the water bath heating temperature of the reaction kettle is stable and the mixture is completely stirred and dissolved; and adding a preset organic additive into the completely dissolved and transparent carrier, and continuously stirring and heating to obtain the required organic carrier.
8. The method according to claim 6, wherein in the step S2, the preparation of the two kinds of glass frits comprises the following steps:
s21, converting into a specific raw material mass ratio according to a preset glass oxide formula, and accurately weighing;
s22, fully mixing the weighed raw materials in a mixer to ensure that the raw materials with different components are uniformly mixed;
s23, placing the mixed raw materials into an alumina crucible, then placing the crucible into a muffle furnace, melting at 1100-1350 ℃, and preserving heat for 30-60 min;
s24, pouring the melted glass liquid into deionized water for water quenching to obtain glass particles with the size of about 1 mm;
s25, filling the glass particles into a ball milling tank, carrying out ball milling for 8-12 h, sieving by a 500-mesh sieve, and drying in an oven at 120 ℃ to obtain required glass powder, wherein the particle size of the glass powder is controlled to be D50: 3-5 μm.
9. The method of claim 6, wherein in the step S3, the mixture is sufficiently ground by a three-roll mill for 5 to 8 times, and the viscosity is controlled to be 50 to 100 Pa-S.
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